#------------------------------------------------------------------------------
#$Date: 2025-02-22 04:53:29 +0200 (Sat, 22 Feb 2025) $
#$Revision: 297834 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312763.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312763
loop_
_publ_author_name
'Vlahakis, Niko'
'Qu, Songrong'
'Richards, Logan S.'
'Moraes, Lygia Silva de'
'Cascio, Duilio'
'Nelson, Hosea M.'
'Rodriguez, Jose A.'
_publ_section_title
;
Fast event-based electron counting for small-molecule structure
determination by MicroED.
;
_journal_coeditor_code YP3239
_journal_issue 3
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624012300
_journal_volume 81
_journal_year 2025
_chemical_absolute_configuration rm
_chemical_formula_iupac 'C10 H16 N2 O3 S1'
_chemical_formula_moiety 'C10 H16 N2 O3 S1'
_chemical_formula_sum 'C10 H16 N2 O3 S'
_chemical_formula_weight 244.31
_chemical_name_common biotin
_chemical_name_systematic
;
5-[(3aS,4S,6aR)-2-Oxohexahydro-1H-\
thieno[3,4-d]imidazol-4-yl]pentanoic acid
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.170(2)
_cell_length_b 10.1100(19)
_cell_length_c 20.710(3)
_cell_measurement_reflns_used 4422
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 0.900
_cell_measurement_theta_min 0.099
_cell_volume 1082.5(5)
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type TEM
_diffrn_measurement_method 'continuous rotation 3D ED'
_diffrn_radiation_type electron
_diffrn_radiation_wavelength 0.0251
_diffrn_reflns_av_R_equivalents 0.1409
_diffrn_reflns_av_unetI/netI 0.1667
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 4422
_diffrn_reflns_theta_full 0.863
_diffrn_reflns_theta_max 0.900
_diffrn_reflns_theta_min 0.099
_diffrn_source FEG
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.000
_exptl_absorpt_correction_type none
_exptl_crystal_colour white
_exptl_crystal_density_diffrn 1.499
_exptl_crystal_description needle
_exptl_crystal_F_000 196
_exptl_crystal_size_max 0.010
_exptl_crystal_size_mid 0.0005
_exptl_crystal_size_min 0.00015
_refine_diff_density_max 0.232
_refine_diff_density_min -0.205
_refine_ls_abs_structure_details
;
All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_coef 1047E1(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.325
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 148
_refine_ls_number_reflns 1926
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.325
_refine_ls_R_factor_all 0.1856
_refine_ls_R_factor_gt 0.1586
_refine_ls_shift/su_max 0.018
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3832
_refine_ls_wR_factor_ref 0.4094
_reflns_number_gt 1397
_reflns_number_total 1926
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yp3239.cif
_cod_data_source_block a
_cod_original_formula_sum 'C10 H16 N2 O3 S1'
_cod_database_code 2312763
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 1 2 3210.95 577.92
0 1 3 508.12 91.93
0 -1 -3 596.88 107.81
0 1 4 128.55 27.53
0 -1 -4 67.99 16.99
0 1 5 2260.32 408.02
0 -1 -5 1917.35 346.39
0 2 3 5471.00 984.36
0 -2 -3 6366.59 1145.04
0 2 4 4201.37 756.25
0 -2 -4 4778.24 860.03
0 2 5 159.86 29.24
0 -2 -5 233.59 42.46
0 2 6 430.15 78.18
0 -2 -6 361.92 65.98
0 2 7 5086.43 915.61
0 -2 -7 4725.55 850.29
0 2 8 1528.30 277.10
0 -2 -8 1287.01 233.12
0 2 9 33.51 26.79
0 -2 -9 32.27 23.63
0 2 10 948.01 176.35
0 -2 -10 1064.17 196.13
0 2 11 -9.59 33.53
0 -2 -11 5.60 24.43
0 3 4 2332.49 420.40
0 -3 -4 2498.96 450.70
0 3 5 102.33 21.07
0 -3 -5 114.51 22.94
0 3 6 3903.72 703.04
0 -3 -6 3563.92 641.93
0 3 7 539.99 97.57
0 -3 -7 751.25 135.79
0 3 8 366.92 66.85
0 -3 -8 217.08 40.22
0 3 9 203.35 38.12
0 -3 -9 292.65 54.26
0 3 10 460.43 85.05
0 -3 -10 512.07 93.93
0 3 11 323.47 62.11
0 -3 -11 473.61 88.43
0 3 12 46.91 29.58
0 -3 -12 -1.81 16.81
0 3 13 111.71 43.41
0 -3 -13 96.93 33.82
0 3 14 119.77 59.64
0 -3 -14 62.80 45.41
0 3 15 1459.82 281.06
0 -3 -15 1436.63 271.83
0 3 16 76.78 78.31
0 -3 -16 255.92 81.81
0 -3 -17 -5.44 95.09
0 -3 -18 26.87 93.09
0 4 7 1025.45 185.70
0 -4 -7 1012.28 183.09
0 4 8 254.37 47.89
0 -4 -8 225.80 42.46
0 4 9 30.21 8.09
0 4 10 2955.45 532.09
0 -4 -10 2942.28 529.72
0 4 11 136.95 26.89
0 -4 -11 80.66 17.55
0 4 12 95.43 20.56
0 -4 -12 164.52 32.87
0 4 13 848.71 155.93
0 -4 -13 939.58 171.79
0 4 14 285.53 61.69
0 -4 -14 130.57 31.29
0 4 15 472.03 94.33
0 -4 -15 552.11 105.42
0 4 16 25.72 60.43
0 -4 -16 28.21 32.14
0 4 17 118.83 101.10
0 -4 -17 161.62 66.64
0 4 18 94.96 85.90
0 -4 -18 -31.24 57.05
0 4 19 -20.80 79.44
0 -4 -19 25.17 61.08
0 4 20 6.25 49.71
0 -4 -20 0.50 33.72
0 4 21 -8.78 45.99
0 -4 -21 29.37 28.26
0 -4 -22 1.45 22.94
0 -4 -23 16.11 19.73
0 -4 -24 10.16 14.63
0 5 6 1359.46 247.66
0 -5 -6 1177.43 214.02
0 5 7 729.38 133.39
0 -5 -7 574.23 104.65
0 5 8 350.87 65.27
0 -5 -8 368.51 67.78
0 5 9 981.20 178.11
0 -5 -9 835.54 151.31
0 5 10 138.32 27.34
0 -5 -10 153.56 29.45
0 -5 -11 129.07 25.03
0 5 12 72.96 15.79
0 -5 -12 38.17 8.73
0 5 13 51.02 13.47
0 -5 -13 68.88 15.91
0 5 14 828.16 151.43
0 -5 -14 968.29 176.03
0 5 15 520.23 96.91
0 -5 -15 566.06 105.44
0 5 16 73.20 28.37
0 -5 -16 37.67 21.53
0 5 17 67.22 49.73
0 -5 -17 49.49 23.02
0 5 18 105.28 48.31
0 -5 -18 158.83 40.64
0 5 19 54.45 35.32
0 -5 -19 48.44 22.19
0 5 20 -0.27 30.71
0 -5 -20 59.06 22.66
0 5 21 3.19 25.21
0 5 22 4.31 22.16
0 -5 -22 19.59 15.83
0 5 23 2.12 16.81
0 -5 -23 6.56 12.14
0 6 7 947.49 174.19
0 -6 -7 693.29 127.49
0 6 8 525.50 96.99
0 -6 -8 616.11 113.03
0 6 9 143.77 28.79
0 -6 -9 164.60 32.29
0 6 10 1042.05 188.97
0 -6 -10 801.03 145.22
0 6 11 300.81 56.11
0 -6 -11 239.89 45.12
0 6 12 180.49 34.77
0 -6 -12 156.78 30.27
0 -6 -13 23.87 8.80
0 6 14 100.10 20.02
0 -6 -14 118.85 23.28
0 6 15 196.21 37.96
0 -6 -15 233.04 43.65
0 6 16 48.65 17.37
0 -6 -16 57.53 15.78
0 6 17 114.24 28.05
0 -6 -17 90.59 22.46
0 6 18 50.63 20.42
0 -6 -18 27.79 17.54
0 6 19 18.81 19.53
0 -6 -19 27.05 16.68
0 6 20 26.28 23.60
0 -6 -20 8.42 14.65
0 6 21 8.00 19.33
0 -6 -21 17.08 13.48
0 6 22 -0.46 13.50
0 -6 -22 9.74 9.85
0 7 7 54.95 21.62
0 7 8 411.71 79.63
0 -7 -8 271.31 52.00
0 7 9 296.86 58.79
0 -7 -9 255.69 49.36
0 7 10 47.02 19.88
0 -7 -10 54.16 14.51
0 7 11 24.25 13.20
0 -7 -11 38.48 10.58
0 7 12 104.44 23.35
0 -7 -12 109.34 23.33
0 7 13 222.06 42.20
0 -7 -13 230.09 43.59
0 7 14 58.77 15.04
0 -7 -14 56.08 13.59
0 -7 -15 32.37 10.25
0 7 16 27.42 9.89
0 7 17 13.04 8.18
0 -7 -17 18.03 7.03
0 7 18 62.43 16.29
0 -7 -18 63.93 14.63
0 7 19 89.85 22.55
0 -7 -19 93.04 21.18
0 7 20 97.62 23.34
0 -7 -20 69.25 19.02
0 -7 -21 -6.56 11.85
0 8 8 -10.95 23.68
0 8 9 221.71 51.21
0 -8 -9 187.31 39.09
0 8 10 482.56 92.75
0 -8 -10 391.42 73.44
0 8 11 12.00 16.44
0 -8 -11 32.11 13.05
0 8 12 720.69 131.47
0 -8 -12 714.10 129.86
0 8 13 86.53 21.52
0 -8 -13 90.06 19.06
0 8 14 39.33 13.95
0 -8 -14 39.14 10.94
0 8 15 16.85 9.42
0 -8 -15 58.98 15.32
0 8 16 34.66 11.65
0 -8 -16 22.13 8.41
0 -8 -17 21.49 8.94
0 8 18 29.95 11.29
0 8 19 30.77 11.68
0 -8 -19 43.01 11.65
0 -8 -20 10.76 8.96
0 9 9 15.97 18.16
0 9 10 76.60 25.79
0 -9 -10 69.38 17.47
0 9 11 20.75 18.15
0 -9 -11 31.00 12.66
0 9 12 -8.16 11.47
0 -9 -12 4.84 9.83
0 9 13 215.79 42.25
0 -9 -13 194.97 36.90
0 9 14 4.88 10.79
0 -9 -14 35.03 9.17
0 9 15 13.08 10.74
0 -9 -15 21.71 8.88
0 9 16 23.35 11.23
0 -9 -16 44.33 11.73
0 9 17 1.29 8.41
0 -9 -17 9.70 9.63
0 -9 -18 89.14 18.73
0 10 10 13.79 17.16
0 10 11 12.68 16.92
0 -10 -11 13.14 8.68
0 10 12 3.71 15.64
0 -10 -12 20.94 9.37
0 10 13 17.27 13.51
0 -10 -13 43.41 12.35
0 10 14 5.54 14.10
0 -10 -14 8.88 8.43
0 -10 -15 20.79 9.16
0 11 11 -1.14 15.57
0 -11 -12 3.91 8.18
1 0 1 1391.06 251.85
-1 0 1 1067.59 193.00
1 0 -1 1270.42 229.48
-1 0 -1 1156.11 209.57
1 0 2 5233.93 942.48
-1 0 2 5950.41 1070.75
1 0 -2 6221.71 1119.49
-1 0 -2 7449.20 1340.23
1 0 3 534.72 99.23
-1 0 3 848.18 154.14
1 0 -3 817.10 148.59
-1 0 -3 521.55 96.91
1 0 4 3342.66 604.00
-1 0 4 3916.89 705.67
1 0 -4 3347.93 603.47
-1 0 -4 4246.15 765.99
-1 0 5 5802.90 1044.95
1 0 -5 7659.93 1378.68
-1 0 6 2050.64 370.88
1 0 -6 1628.92 295.02
-1 0 7 1786.44 324.26
1 0 -7 1339.70 243.97
-1 0 8 281.32 59.50
1 0 -8 345.60 70.22
-1 0 9 1167.42 216.76
1 0 -9 1596.52 293.70
-1 0 10 675.90 131.34
1 0 -10 1159.00 215.47
-1 0 11 511.80 106.23
1 0 -11 448.06 92.61
-1 0 12 116.82 52.55
1 0 -12 0.13 33.82
1 0 -13 26.27 41.20
1 1 0 9675.00 1740.34
-1 -1 0 9087.60 1634.45
1 -1 0 9725.06 1749.56
-1 1 0 9361.55 1684.50
1 -1 1 4506.92 812.09
-1 1 1 5489.44 988.57
1 1 -1 4630.73 833.69
-1 -1 -1 6340.25 1140.56
-1 -1 1 5615.87 1010.70
1 -1 -1 5434.12 978.56
-1 1 -1 5428.85 977.77
1 -1 2 9327.31 1678.70
-1 1 2 7241.11 1303.35
1 1 -2 8579.23 1543.84
-1 -1 -2 6221.71 1119.49
1 1 2 6329.71 1138.98
-1 -1 2 7267.45 1308.09
1 -1 -2 6925.01 1245.93
-1 1 -2 6366.59 1146.36
1 -1 3 8847.90 1593.62
-1 1 3 6635.27 1193.77
1 1 -3 7504.52 1351.55
-1 -1 -3 7162.09 1288.59
1 1 3 6780.15 1220.11
-1 -1 3 9999.00 1800.13
1 -1 -3 6732.73 1211.68
-1 1 -3 7328.03 1320.73
-1 1 4 2789.50 502.32
1 1 -4 3650.85 660.36
-1 -1 -4 2522.14 454.64
1 1 4 2926.47 527.08
-1 -1 4 3274.18 592.93
1 -1 -4 3205.68 577.65
-1 1 5 6977.70 1255.67
1 1 -5 6777.51 1221.95
-1 -1 -5 7275.35 1309.14
1 1 5 7825.88 1408.18
-1 -1 5 9171.89 1652.37
1 -1 -5 7011.95 1261.99
-1 1 6 2734.18 492.84
1 1 -6 2042.47 373.25
-1 -1 6 2505.02 455.96
1 -1 -6 2300.35 415.13
1 1 -7 14.16 32.50
-1 -1 7 131.15 48.34
-1 1 8 1539.89 279.21
1 -1 -8 1887.06 341.38
-1 1 9 334.80 65.33
1 -1 -9 516.55 97.12
-1 1 10 1343.12 245.05
1 -1 -10 1685.55 306.08
-1 1 11 452.01 89.43
-1 1 12 143.11 49.60
1 -1 -12 20.32 30.79
-1 1 13 258.11 72.54
1 -1 -13 226.38 61.08
-1 1 14 801.29 161.10
1 -1 -14 939.58 181.01
-1 1 15 86.21 75.97
1 -1 -15 296.60 85.98
-1 1 16 174.69 90.85
1 -1 -16 169.45 66.22
-1 1 17 125.96 125.52
1 -1 -17 20.92 92.38
1 -1 -18 4.85 114.82
1 -1 -19 -57.08 83.26
1 2 0 2277.43 413.29
-1 -2 0 1866.52 339.27
1 -2 0 2829.01 510.75
-1 2 0 2382.00 430.68
1 -2 1 1415.03 258.35
-1 2 1 1307.56 237.05
1 2 -1 1391.59 256.19
-1 -2 -1 1606.79 291.86
1 2 1 2150.74 389.05
-1 -2 1 1095.52 203.40
1 -2 -1 1547.27 280.00
-1 2 -1 1294.13 237.12
1 -2 2 6806.49 1226.96
-1 2 2 7314.87 1316.52
-1 -2 -2 5784.46 1040.73
1 2 2 6882.88 1238.29
1 -2 -2 6498.30 1169.79
-1 2 -2 5926.70 1069.17
-1 2 3 7159.45 1288.86
-1 -2 -3 6477.22 1165.05
1 2 3 6864.43 1234.86
1 -2 -3 6616.83 1191.13
-1 -2 -4 1823.05 328.21
-1 2 5 964.60 174.61
1 2 5 1103.42 199.22
1 -2 -5 833.69 150.96
-1 2 6 299.76 55.34
1 2 6 264.99 50.31
1 -2 -6 236.62 43.67
-1 2 7 266.83 49.52
1 -2 -7 303.71 56.26
-1 2 8 1509.60 272.89
1 -2 -8 1542.26 278.95
-1 2 9 117.24 24.34
1 -2 -9 151.53 30.56
-1 2 10 94.01 21.63
-1 2 11 303.18 60.16
1 -2 -11 168.84 35.64
-1 2 12 2516.34 456.22
1 -2 -12 2580.09 467.28
-1 2 13 62.24 28.92
1 -2 -13 46.60 23.07
-1 2 14 26.18 36.38
1 -2 -14 42.44 24.99
-1 2 15 211.60 64.22
-1 2 16 354.28 102.60
1 -2 -16 248.32 67.88
-1 2 17 -14.59 116.22
1 -2 -17 83.61 81.63
-1 2 18 91.90 137.61
1 -2 -18 186.54 106.37
-1 2 19 16.84 104.26
1 -2 -19 113.29 80.97
-1 2 20 114.06 97.80
1 -2 -20 105.92 72.46
-1 2 21 67.27 63.03
1 -2 -21 40.56 40.85
-1 2 22 4.43 55.50
1 -2 -22 41.99 34.59
-1 2 23 -36.80 46.57
1 -2 -23 -8.73 25.45
1 -2 -24 -12.95 19.78
1 -2 -25 -1.58 17.62
1 -3 0 896.64 165.89
-1 3 0 873.99 163.05
1 -3 1 2520.03 457.01
-1 3 1 3482.27 628.50
1 -3 -1 3266.27 589.51
-1 3 -1 3073.99 557.10
-1 3 3 1500.11 271.57
1 -3 -3 1269.63 229.85
-1 3 4 432.52 80.18
1 -3 -4 503.11 93.09
-1 3 5 2931.74 528.66
1 3 5 2036.42 367.98
1 -3 -5 2331.70 421.19
1 3 6 3155.64 568.17
1 -3 -6 3916.89 705.41
-1 3 7 283.16 52.76
1 3 7 342.96 62.16
1 -3 -7 313.46 57.82
-1 3 8 498.11 91.09
1 -3 -8 542.10 98.75
-1 3 9 1092.09 197.66
1 -3 -9 1110.27 201.03
-1 3 10 723.85 131.87
1 -3 -10 759.67 138.35
-1 3 11 835.54 152.32
1 -3 -11 672.48 123.30
-1 3 12 66.46 17.18
1 -3 -12 72.28 19.37
-1 3 13 652.20 120.46
1 -3 -13 783.11 143.96
-1 3 14 320.31 66.25
1 -3 -14 168.79 37.22
-1 3 15 339.27 75.20
1 -3 -15 377.46 74.49
-1 3 16 199.69 55.53
1 -3 -16 165.21 47.91
-1 3 17 376.41 88.08
1 -3 -17 499.69 101.04
1 -3 -18 97.30 46.89
-1 3 19 58.35 73.28
1 -3 -19 66.04 54.34
-1 3 20 -25.37 58.19
1 -3 -20 12.11 38.51
-1 3 21 10.31 46.99
1 -3 -21 -7.63 35.14
-1 3 22 7.78 31.98
1 -3 -22 10.50 24.15
-1 3 23 31.74 28.03
1 -3 -23 -7.03 21.69
-1 3 24 1.89 18.88
1 -3 -24 10.89 14.16
1 -4 0 571.59 108.24
-1 4 0 423.30 84.84
-1 4 1 997.53 183.12
1 -4 -1 1149.52 210.23
-1 4 2 2697.30 487.30
1 -4 -2 2522.93 455.96
-1 4 3 1867.84 338.22
1 -4 -3 1210.63 219.71
-1 4 4 858.97 156.99
1 -4 -4 906.65 164.94
-1 4 5 4591.22 827.37
1 -4 -5 5083.79 915.35
-1 4 6 1437.16 260.48
1 -4 -6 1400.54 253.39
-1 4 7 1825.16 330.32
-1 4 8 386.42 71.52
1 -4 -8 444.37 81.68
-1 4 9 1192.98 215.81
1 -4 -9 902.70 163.55
-1 4 10 833.16 151.28
-1 -4 -10 821.05 149.54
1 -4 -10 909.02 164.57
-1 4 11 612.69 112.06
1 -4 -11 398.27 72.96
-1 4 12 821.57 149.30
1 -4 -12 942.48 171.37
-1 4 13 283.43 54.42
1 -4 -13 349.02 65.59
-1 4 14 143.69 32.24
1 -4 -14 117.14 27.71
-1 4 15 394.32 75.55
1 -4 -15 385.37 74.02
-1 4 16 133.47 36.14
1 -4 -16 118.27 29.90
-1 4 17 129.65 44.28
1 -4 -17 49.18 22.00
-1 4 18 146.30 57.84
1 -4 -18 76.36 31.45
-1 4 19 163.89 52.92
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6 3 0 39.06 20.84
-6 -3 0 13.05 23.95
6 -3 0 91.06 26.95
6 -3 1 35.01 17.40
6 3 -1 39.80 22.75
-6 -3 -1 52.29 28.34
6 3 1 51.10 22.88
-6 -3 1 36.82 31.69
6 -3 -1 25.48 17.60
6 -3 2 28.76 17.00
6 3 -2 7.84 18.30
-6 -3 -2 1.14 21.06
6 3 2 17.00 17.53
-6 -3 2 6.03 25.25
6 -3 -2 24.97 18.05
6 -3 3 16.78 16.53
6 3 -3 29.63 23.72
-6 -3 -3 13.03 27.03
6 3 3 26.55 19.42
-6 -3 3 32.27 27.71
6 -3 -3 16.82 18.74
-6 3 -3 25.50 23.26
6 -3 4 29.90 16.54
6 3 -4 41.25 23.15
-6 -3 -4 17.77 19.29
6 3 4 15.32 18.35
-6 -3 4 41.49 27.76
6 -3 -4 7.00 16.65
-6 3 -4 30.40 21.38
6 -3 5 37.33 17.79
6 3 -5 1.32 23.34
-6 -3 -5 16.67 20.50
-6 -3 5 -2.62 27.90
6 -3 -5 13.84 20.65
-6 3 -5 30.40 23.02
6 3 -6 2.06 24.50
6 3 6 11.22 17.72
-6 3 -6 8.70 21.51
6 4 0 -4.62 21.75
-6 -4 0 0.74 26.45
6 -4 0 25.77 17.51
6 -4 1 62.48 20.78
6 4 -1 33.58 23.83
-6 -4 -1 21.56 25.99
6 4 1 49.81 24.18
-6 -4 1 42.80 29.58
6 -4 2 15.80 16.94
6 4 -2 7.17 20.18
-6 -4 -2 11.60 21.58
6 4 2 17.92 19.88
-6 -4 2 1.82 26.30
6 4 -3 -6.63 24.17
-6 -4 -3 11.59 24.54
6 4 3 3.20 22.08
-6 -4 3 5.49 30.58
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 95204
_shelx_res_file
;
TITL biotin_spot11_0p3dps_0p3fps_mov05_a.res in P2(1)2(1)2(1)
a.res
created by SHELXL-2019/3 at 16:34:19 on 11-Jul-2024
REM Old TITL GGYMLG in space group P 1 21 1 .
REM SHELXT solution in P2(1)2(1)2(1): R1 0.298, Rweak 0.282, Alpha 0.038
REM 0.000 for 0 systematic absences, Orientation as input
REM Flack x = 0.121 ( 0.138 ) from 461 Parsons' quotients
REM Formula found by SHELXT: C12 N O2 S
CELL 0.02510 5.1700 10.1100 20.7100 90.000 90.000 90.000
ZERR 1.000 0.0020 0.0019 0.0033 0.000 0.000 0.000
LATT -1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC C 0.600 40.938 0.136 0.374 0.547 3.278 1.225 13.013 0 0 0 0 0.76 12.011
SFAC N 0.482 31.526 0.135 0.324 0.519 2.607 1.075 10.017 0 0 0 0 0.71 14.007
SFAC O 0.392 25.675 0.144 0.306 0.511 2.272 0.937 8.270 0 0 0 0 0.66 15.999
SFAC S 1.390 40.169 0.348 0.365 0.915 2.890 2.506 13.043 0 0 0 0 1.05 32.065
SFAC H 0.129 37.737 0.036 0.553 0.127 3.772 0.236 13.518 0 0 0 0 0.31 1.008
UNIT 40 8 12 4 64
L.S. 1000
BOND
LIST 4
FMAP 2
PLAN 20
DFIX 1 O7 H11
ACTA
TEMP -173
WGHT 0.200000
EXTI10468.270508
FVAR 5.74610
S1 4 0.447151 0.629131 0.548162 11.00000 0.04103 0.06294 =
0.06455 0.00511 0.00656 0.00103
C2 1 0.272907 0.682789 0.664210 11.00000 0.04637 0.04258 =
0.06369 0.01483 0.00367 0.01432
AFIX 13
H3 5 0.156699 0.744934 0.688076 11.00000 -1.20000
AFIX 0
O1 3 0.581853 0.424239 0.746089 11.00000 0.06581 0.04263 =
0.05607 -0.00307 -0.02006 0.00045
C4 1 0.394937 0.750979 0.608197 11.00000 0.05078 0.02946 =
0.08348 0.00104 -0.02565 -0.00932
AFIX 23
H5A 5 0.561126 0.791672 0.621210 11.00000 -1.20000
H5B 5 0.279576 0.821350 0.591594 11.00000 -1.20000
AFIX 0
C5 1 0.142985 0.555961 0.568406 11.00000 0.04177 0.03005 =
0.03150 0.01580 -0.00145 0.01225
AFIX 13
H6 5 0.006644 0.616251 0.550889 11.00000 -1.20000
AFIX 0
C3 1 0.122586 0.563237 0.641236 11.00000 0.02710 0.04628 =
0.06731 0.01275 0.00750 -0.00326
AFIX 13
H4 5 -0.061673 0.566286 0.655848 11.00000 -1.20000
AFIX 0
O7 3 0.524065 0.517278 0.310914 11.00000 0.05533 0.04890 =
0.06641 0.01129 0.01771 0.00462
AFIX 88
H11 5 0.703990 0.527528 0.291153 11.00000 -1.50000
AFIX 0
N2 2 0.259503 0.461450 0.671520 11.00000 0.04852 0.02752 =
0.04619 0.00655 -0.01542 0.00170
AFIX 43
H2 5 0.222096 0.377591 0.665004 11.00000 -1.20000
AFIX 0
C6 1 0.084540 0.423110 0.543198 11.00000 0.05246 0.03205 =
0.04221 -0.01875 -0.00723 -0.00581
AFIX 23
H7A 5 -0.077660 0.392651 0.563801 11.00000 -1.20000
H7B 5 0.223863 0.362837 0.557680 11.00000 -1.20000
AFIX 0
C9 1 0.252261 0.374367 0.365956 11.00000 0.04463 0.03968 =
0.06825 -0.00014 -0.00073 0.00548
AFIX 23
H10A 5 0.103149 0.423018 0.347641 11.00000 -1.20000
H10B 5 0.209890 0.278886 0.365124 11.00000 -1.20000
AFIX 0
C1 1 0.442050 0.497255 0.709197 11.00000 0.03910 0.03084 =
0.03118 0.00425 -0.01463 0.00332
C10 1 0.485288 0.398373 0.324455 11.00000 0.04749 0.04305 =
0.05374 -0.02403 0.01886 -0.00898
N1 2 0.463433 0.626933 0.707444 11.00000 0.04964 0.04350 =
0.04539 -0.01514 -0.03089 -0.00561
AFIX 43
H1 5 0.577570 0.673122 0.729473 11.00000 -1.20000
AFIX 0
C8 1 0.289703 0.415245 0.432021 11.00000 0.05428 0.02199 =
0.05581 0.00403 -0.00859 -0.00114
AFIX 23
H9A 5 0.352328 0.507775 0.432597 11.00000 -1.20000
H9B 5 0.424798 0.359130 0.451955 11.00000 -1.20000
AFIX 0
O00F 3 0.622083 0.307723 0.302014 11.00000 0.05115 0.03884 =
0.11954 0.00876 0.01892 0.00268
C7 1 0.054424 0.406205 0.470369 11.00000 0.05195 0.03635 =
0.06816 0.01339 -0.00568 0.00708
AFIX 23
H8A 5 -0.025508 0.318811 0.462195 11.00000 -1.20000
H8B 5 -0.067987 0.474312 0.454688 11.00000 -1.20000
REM #####
REM #####
AFIX 0
HKLF 4
REM biotin_spot11_0p3dps_0p3fps_mov05_a.res in P2(1)2(1)2(1)
REM wR2 = 0.4094, GooF = S = 1.325, Restrained GooF = 1.325 for all data
REM R1 = 0.1586 for 1397 Fo > 4sig(Fo) and 0.1856 for all 1926 data
REM 148 parameters refined using 1 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 0.232, deepest hole -0.205, 1-sigma level 0.065
Q1 1 0.4656 0.5657 0.5007 11.00000 0.05 0.23
Q2 1 0.4701 0.5617 0.6621 11.00000 0.05 0.23
Q3 1 0.0196 0.4316 0.5919 11.00000 0.05 0.21
Q4 1 0.4699 0.6954 0.5793 11.00000 0.05 0.21
Q5 1 0.5253 0.5800 0.3590 11.00000 0.05 0.20
Q6 1 0.5470 0.4639 0.7712 11.00000 0.05 0.19
Q7 1 0.5034 0.4493 0.3530 11.00000 0.05 0.19
Q8 1 0.0911 0.5838 0.5974 11.00000 0.05 0.18
Q9 1 0.3729 0.6776 0.6619 11.00000 0.05 0.18
Q10 1 0.1023 0.3558 0.4177 11.00000 0.05 0.18
Q11 1 0.0692 0.4773 0.4271 11.00000 0.05 0.17
Q12 1 0.0223 0.5613 0.4268 11.00000 0.05 0.16
Q13 1 0.4315 0.8126 0.5767 11.00000 0.05 0.15
Q14 1 0.2023 0.5646 0.6263 11.00000 0.05 0.14
Q15 1 0.4579 0.6619 0.5239 11.00000 0.05 0.14
Q16 1 -0.1587 0.3163 0.5520 11.00000 0.05 0.13
Q17 1 0.3611 0.2542 0.3112 11.00000 0.05 0.12
Q18 1 0.3175 0.3615 0.4790 11.00000 0.05 0.12
Q19 1 0.5897 0.3813 0.7130 11.00000 0.05 0.12
Q20 1 0.2893 0.2796 0.3190 11.00000 0.05 0.11
;
_shelx_res_checksum 5829
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S1 0.4472(12) 0.6291(8) 0.5482(4) 0.056(2) Uani d 1 . .
C C2 0.273(3) 0.6828(15) 0.6642(7) 0.051(4) Uani d 1 . .
H H3 0.156699 0.744934 0.688076 0.061 Uiso calc 1 . .
O O1 0.582(2) 0.4242(13) 0.7461(6) 0.055(3) Uani d 1 . .
C C4 0.395(3) 0.7510(15) 0.6082(8) 0.055(4) Uani d 1 . .
H H5A 0.561126 0.791672 0.621210 0.065 Uiso calc 1 . .
H H5B 0.279576 0.821350 0.591594 0.065 Uiso calc 1 . .
C C5 0.143(2) 0.5560(11) 0.5684(6) 0.034(3) Uani d 1 . .
H H6 0.006644 0.616251 0.550889 0.041 Uiso calc 1 . .
C C3 0.123(2) 0.5632(15) 0.6412(7) 0.047(3) Uani d 1 . .
H H4 -0.061673 0.566286 0.655848 0.056 Uiso calc 1 . .
O O7 0.524(2) 0.5173(13) 0.3109(7) 0.057(3) Uani d 1 . .
H H11 0.704(10) 0.528(2) 0.291(5) 0.085 Uiso calc 1 . .
N N2 0.260(2) 0.4614(12) 0.6715(6) 0.041(3) Uani d 1 . .
H H2 0.222096 0.377591 0.665004 0.049 Uiso calc 1 . .
C C6 0.085(2) 0.4231(13) 0.5432(6) 0.042(3) Uani d 1 . .
H H7A -0.077660 0.392651 0.563801 0.051 Uiso calc 1 . .
H H7B 0.223863 0.362837 0.557680 0.051 Uiso calc 1 . .
C C9 0.252(3) 0.3744(14) 0.3660(8) 0.051(3) Uani d 1 . .
H H10A 0.103149 0.423018 0.347641 0.061 Uiso calc 1 . .
H H10B 0.209890 0.278886 0.365124 0.061 Uiso calc 1 . .
C C1 0.442(2) 0.4973(11) 0.7092(6) 0.034(3) Uani d 1 . .
C C10 0.485(2) 0.3984(14) 0.3245(7) 0.048(4) Uani d 1 . .
N N1 0.463(2) 0.6269(11) 0.7074(6) 0.046(3) Uani d 1 . .
H H1 0.577570 0.673122 0.729473 0.055 Uiso calc 1 . .
C C8 0.290(2) 0.4152(13) 0.4320(7) 0.044(3) Uani d 1 . .
H H9A 0.352328 0.507775 0.432597 0.053 Uiso calc 1 . .
H H9B 0.424798 0.359130 0.451955 0.053 Uiso calc 1 . .
O O00F 0.622(2) 0.3077(14) 0.3020(9) 0.070(4) Uani d 1 . .
C C7 0.054(3) 0.4062(15) 0.4704(7) 0.052(3) Uani d 1 . .
H H8A -0.025508 0.318811 0.462195 0.063 Uiso calc 1 . .
H H8B -0.067987 0.474312 0.454688 0.063 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 0.041(3) 0.063(5) 0.065(5) 0.001(3) 0.007(3) 0.005(3)
C2 0.046(7) 0.043(9) 0.064(11) 0.014(6) 0.004(6) 0.015(6)
O1 0.066(6) 0.043(8) 0.056(8) 0.000(5) -0.020(6) -0.003(5)
C4 0.051(8) 0.029(9) 0.083(12) -0.009(5) -0.026(7) 0.001(6)
C5 0.042(5) 0.030(7) 0.031(7) 0.012(4) -0.001(4) 0.016(4)
C3 0.027(5) 0.046(9) 0.067(10) -0.003(5) 0.007(5) 0.013(6)
O7 0.055(6) 0.049(8) 0.066(9) 0.005(5) 0.018(6) 0.011(5)
N2 0.049(5) 0.028(7) 0.046(7) 0.002(4) -0.015(5) 0.007(4)
C6 0.052(6) 0.032(7) 0.042(8) -0.006(5) -0.007(6) -0.019(5)
C9 0.045(6) 0.040(9) 0.068(11) 0.005(6) -0.001(6) 0.000(6)
C1 0.039(5) 0.031(8) 0.031(7) 0.003(5) -0.015(5) 0.004(4)
C10 0.047(6) 0.043(9) 0.054(9) -0.009(6) 0.019(6) -0.024(6)
N1 0.050(5) 0.043(8) 0.045(8) -0.006(5) -0.031(5) -0.015(4)
C8 0.054(7) 0.022(7) 0.056(9) -0.001(5) -0.009(6) 0.004(5)
O00F 0.051(6) 0.039(8) 0.120(14) 0.003(5) 0.019(7) 0.009(7)
C7 0.052(6) 0.036(9) 0.068(10) 0.007(6) -0.006(6) 0.013(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C4 S1 C5 . . 89.4(7) ?
N1 C2 C4 . . 112.0(12) ?
N1 C2 C3 . . 103.4(11) ?
C4 C2 C3 . . 110.0(13) ?
C2 C4 S1 . . 106.8(11) ?
C6 C5 C3 . . 112.5(10) ?
C6 C5 S1 . . 118.3(9) ?
C3 C5 S1 . . 106.0(9) ?
N2 C3 C5 . . 112.1(12) ?
N2 C3 C2 . . 100.8(10) ?
C5 C3 C2 . . 108.4(10) ?
C1 N2 C3 . . 116.1(12) ?
C5 C6 C7 . . 118.3(12) ?
C8 C9 C10 . . 112.9(11) ?
O1 C1 N2 . . 128.0(13) ?
O1 C1 N1 . . 122.8(11) ?
N2 C1 N1 . . 109.1(11) ?
O00F C10 O7 . . 122.1(13) ?
O00F C10 C9 . . 123.4(13) ?
O7 C10 C9 . . 114.4(11) ?
C1 N1 C2 . . 110.4(11) ?
C9 C8 C7 . . 112.8(11) ?
C8 C7 C6 . . 116.6(12) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 C4 . 1.771(19) ?
S1 C5 . 1.788(13) ?
C2 N1 . 1.446(17) ?
C2 C4 . 1.49(2) ?
C2 C3 . 1.51(2) ?
O1 C1 . 1.285(17) ?
C5 C6 . 1.472(17) ?
C5 C3 . 1.514(19) ?
C3 N2 . 1.398(17) ?
O7 C10 . 1.251(19) ?
N2 C1 . 1.277(16) ?
C6 C7 . 1.53(2) ?
C9 C8 . 1.44(2) ?
C9 C10 . 1.500(18) ?
C1 N1 . 1.316(17) ?
C10 O00F . 1.247(19) ?
C8 C7 . 1.46(2) ?