#------------------------------------------------------------------------------
#$Date: 2021-02-05 16:53:45 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261801 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022297.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_2022297
loop_
_publ_author_name
'Shishkina, Svitlana V.'
'Konovalova, Irina S.'
'Kovalenko, Sergiy M.'
'Kravchenko, Dmitriy V.'
'Bunyatyan, Natalya D.'
_publ_section_title
;
Polymorphism of methyl 4-amino-3-phenylisothiazole-5-carboxylate: an
experimental and theoretical study
;
_journal_coeditor_code VP3011
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 40
_journal_page_last 48
_journal_paper_doi 10.1107/S2053229620016356
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C11 H10 N2 O2 S'
_chemical_formula_moiety 'C11 H10 N2 O2 S'
_chemical_formula_sum 'C11 H10 N2 O2 S'
_chemical_formula_weight 234.27
_chemical_name_systematic
;
Methyl 4-amino-3-phenylisothiazole-5-carboxylate
;
_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 mixed
_audit_creation_method SHELXL-2016/6
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 3.9876(5)
_cell_length_b 10.6511(13)
_cell_length_c 25.107(2)
_cell_measurement_reflns_used 1316
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 21.69
_cell_measurement_theta_min 3.75
_cell_volume 1066.4(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Rigaku Xcalibur Sapphire3'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0694
_diffrn_reflns_av_unetI/netI 0.0558
_diffrn_reflns_limit_h_max 4
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 7448
_diffrn_reflns_theta_full 24.998
_diffrn_reflns_theta_max 24.998
_diffrn_reflns_theta_min 3.246
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 0.288
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.10802
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2018)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.459
_exptl_crystal_description plate
_exptl_crystal_F_000 488
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_min 0.080
_refine_diff_density_max 0.324
_refine_diff_density_min -0.274
_refine_ls_abs_structure_details
;
Flack x determined using 447 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.05(12)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.075
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 154
_refine_ls_number_reflns 1884
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.075
_refine_ls_R_factor_all 0.0708
_refine_ls_R_factor_gt 0.0551
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0835P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1409
_refine_ls_wR_factor_ref 0.1609
_reflns_number_gt 1448
_reflns_number_total 1884
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vp3011sup1.cif
_cod_data_source_block 1a
_cod_depositor_comments
'Adding full bibliography for 2022297--2022298.cif.'
_cod_original_cell_volume 1066.3(2)
_cod_database_code 2022297
_cod_database_fobs_code 2022297
_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_estimated_absorpt_t_min 0.945
_shelx_estimated_absorpt_t_max 0.977
_shelx_hkl_file
;
0 0 -4 324.77 20.02
0 0 -4 396.01 20.80
0 0 -5 0.79 1.17
0 0 -5 -0.47 0.38
0 0 -5 0.29 0.37
0 0 5 2.01 1.21
0 0 5 1.26 0.72
0 0 5 0.08 0.51
0 0 -6 2286.21 116.02
0 0 6 2634.54 117.48
0 0 6 2464.48 114.61
0 0 -7 5.44 2.40
0 0 7 13.34 2.57
0 0 -7 6.94 2.25
0 0 7 12.81 3.40
0 0 8 1550.58 79.25
0 0 -8 1593.48 82.00
0 0 8 1574.20 82.36
0 0 -8 1382.45 81.07
0 0 9 13.82 3.04
0 0 9 22.50 5.00
0 0 10 4580.12 232.54
0 0 10 4703.55 236.30
0 0 11 68.84 7.78
0 0 11 66.48 9.36
0 0 12 1450.04 78.83
0 0 12 1515.71 83.01
0 0 13 29.37 5.27
0 0 13 31.71 6.76
0 0 14 312.19 22.51
0 0 14 353.11 26.50
0 0 15 11.77 4.26
0 0 15 6.72 2.91
0 0 16 270.58 23.19
0 0 16 234.82 18.94
0 0 17 8.45 3.30
0 0 17 13.25 5.18
0 0 18 214.70 18.73
0 0 18 272.03 24.02
0 0 19 16.77 6.24
0 0 19 7.39 3.09
0 0 20 644.50 43.67
0 0 20 800.89 51.35
0 0 21 41.83 9.60
0 0 21 37.88 7.23
0 0 22 26.52 5.75
0 0 22 36.89 8.68
0 0 23 2.95 2.06
0 0 23 0.33 2.31
0 0 24 12.43 3.88
0 0 24 23.11 7.52
0 0 25 -0.32 1.51
0 0 26 5.05 3.75
0 0 27 1.20 0.47
0 0 28 1.29 2.36
0 0 29 2.45 3.48
0 0 30 5.07 4.38
0 0 31 3.17 4.06
0 0 32 0.27 2.72
0 0 33 5.88 4.71
0 0 34 19.87 8.06
0 0 35 6.92 5.34
0 -1 4 118.06 9.69
0 -1 4 128.43 10.07
0 1 -4 114.68 10.06
0 -1 -4 126.64 10.40
0 1 -4 122.37 10.56
0 1 4 118.79 9.99
0 -1 5 2205.11 112.43
0 1 5 2110.39 112.91
0 -1 -5 2178.10 113.79
0 -1 5 2286.66 113.22
0 1 -5 2140.72 113.36
0 -1 -6 351.23 24.05
0 1 6 345.39 22.85
0 -1 6 346.71 22.32
0 -1 6 363.81 23.27
0 1 6 361.21 22.00
0 1 6 373.26 20.78
0 1 -6 329.72 23.18
0 1 7 14.57 2.38
0 1 7 12.65 3.14
0 -1 -7 6.88 2.67
0 -1 7 11.55 2.73
0 1 7 13.37 2.84
0 -1 7 12.30 3.00
0 1 8 396.46 23.78
0 -1 8 358.82 23.71
0 -1 8 343.39 24.56
0 1 8 376.20 21.92
0 -1 -8 349.30 25.86
0 1 8 370.01 25.06
0 1 9 7.50 1.80
0 1 9 4.08 1.82
0 -1 9 5.49 2.23
0 -1 -9 9.57 3.06
0 1 9 4.95 2.13
0 -1 9 7.86 3.16
0 -1 10 697.80 40.83
0 1 -10 695.10 34.67
0 -1 -10 672.42 42.95
0 1 10 722.22 41.60
0 1 10 723.72 38.96
0 1 10 686.43 36.62
0 -1 10 647.70 38.64
0 1 10 559.72 33.35
0 -1 11 43.46 6.61
0 1 11 42.75 6.17
0 1 11 48.80 7.86
0 -1 11 56.11 8.18
0 1 11 42.11 5.28
0 1 12 1212.30 68.06
0 -1 12 1179.26 67.86
0 -1 12 1217.78 70.28
0 1 12 1298.87 71.63
0 -1 13 403.48 26.65
0 1 13 319.08 20.01
0 1 13 417.94 26.51
0 1 13 384.15 23.56
0 -1 13 435.27 29.12
0 1 13 433.40 29.33
0 1 14 84.48 8.30
0 1 14 102.91 12.25
0 1 14 83.48 9.94
0 -1 14 87.25 10.06
0 1 14 62.72 5.40
0 -1 14 90.15 11.46
0 -1 15 28.25 5.80
0 -1 15 42.22 7.78
0 1 15 35.73 7.64
0 1 15 33.57 5.11
0 1 16 623.57 41.37
0 -1 16 556.64 37.27
0 1 16 545.10 34.60
0 -1 16 596.06 40.57
0 1 17 216.21 21.11
0 -1 17 203.51 20.39
0 -1 17 199.95 18.18
0 1 17 197.21 16.15
0 1 18 446.07 31.00
0 -1 18 484.06 34.05
0 -1 18 566.52 38.83
0 1 18 516.57 37.79
0 1 19 14.00 4.54
0 -1 19 22.53 6.87
0 1 19 24.55 7.25
0 -1 19 16.41 5.23
0 1 20 8.59 3.07
0 -1 20 14.68 5.53
0 1 20 8.98 4.57
0 -1 20 9.82 3.75
0 1 21 7.75 2.82
0 -1 21 27.71 7.52
0 1 21 25.91 7.19
0 -1 21 14.08 4.70
0 1 22 334.88 29.44
0 -1 22 328.52 28.96
0 -1 22 253.86 23.39
0 1 22 240.40 20.81
0 -1 23 66.77 10.44
0 1 23 65.13 12.37
0 -1 23 83.10 13.66
0 1 23 49.16 7.88
0 1 24 7.98 4.91
0 -1 24 12.53 5.44
0 -1 24 4.85 2.62
0 1 25 15.13 6.35
0 -1 25 9.76 3.64
0 -1 25 25.48 7.81
0 1 26 35.50 9.63
0 -1 26 45.44 10.73
0 -1 27 0.78 2.38
0 1 27 0.67 3.15
0 1 28 19.88 7.07
0 -1 28 23.13 7.86
0 1 29 9.06 4.46
0 -1 29 3.22 3.92
0 1 30 5.97 4.39
0 -1 30 4.72 4.01
0 -1 31 1.98 3.31
0 1 31 0.90 1.84
0 1 32 -0.24 2.83
0 -1 32 0.49 2.74
0 -1 33 -2.23 4.68
0 1 33 2.06 1.70
0 1 34 3.41 1.85
0 -1 34 2.98 3.54
0 -1 35 3.44 3.74
0 1 35 -5.46 4.27
0 -2 0 3494.80 189.45
0 2 0 4106.99 192.88
0 2 -1 1989.43 97.80
0 -2 1 1752.68 96.31
0 -2 1 1751.42 97.58
0 -2 -1 1778.47 98.25
0 2 -1 2022.20 100.67
0 2 1 2115.65 101.59
0 2 -2 2785.76 142.11
0 -2 2 2579.74 139.78
0 -2 -2 2753.41 140.95
0 -2 2 2641.19 138.76
0 2 -2 2747.84 140.04
0 2 2 3015.67 143.17
0 -2 -3 506.80 33.28
0 2 -3 646.05 34.86
0 -2 3 535.95 32.97
0 -2 3 554.16 32.47
0 -2 -4 434.09 29.55
0 -2 4 533.36 31.98
0 -2 4 457.69 28.73
0 -2 -5 609.45 40.93
0 -2 5 723.24 41.06
0 -2 5 719.86 42.34
0 -2 6 258.80 19.16
0 -2 6 242.25 19.23
0 -2 -6 236.60 19.50
0 -2 7 376.83 26.63
0 -2 -7 364.11 27.71
0 -2 7 411.19 27.03
0 -2 8 20.85 4.62
0 -2 8 21.93 4.62
0 -2 -8 18.38 2.79
0 -2 -8 20.66 5.20
0 -2 9 856.17 50.79
0 2 9 809.26 48.45
0 -2 9 833.52 50.18
0 -2 -9 842.07 44.73
0 -2 -9 871.74 53.86
0 2 10 417.11 29.18
0 2 10 459.23 31.23
0 -2 10 431.16 30.81
0 2 10 440.16 27.28
0 -2 10 445.19 31.37
0 -2 -10 462.80 34.55
0 -2 -10 483.80 25.64
0 -2 -11 530.73 39.55
0 2 11 517.86 31.09
0 -2 11 527.26 35.89
0 2 11 539.68 36.02
0 -2 11 514.35 35.04
0 2 11 551.76 34.35
0 -2 -12 -1.41 1.58
0 -2 12 -0.06 1.70
0 2 12 2.27 0.35
0 2 12 0.63 0.49
0 -2 12 0.67 2.13
0 2 12 1.48 1.09
0 2 13 103.67 11.25
0 -2 13 89.77 11.27
0 -2 -13 115.26 15.82
0 -2 13 86.17 11.47
0 2 -13 92.69 9.46
0 2 13 99.34 9.23
0 2 13 99.78 12.41
0 2 14 0.23 0.15
0 2 14 -1.44 0.86
0 2 14 -0.27 0.77
0 -2 14 0.76 2.00
0 2 14 1.14 0.74
0 -2 -14 -2.91 2.50
0 2 -14 0.74 0.28
0 -2 14 -0.27 1.29
0 2 15 44.93 4.75
0 2 15 70.28 7.51
0 -2 -15 76.87 13.80
0 2 -15 56.46 6.45
0 2 15 65.53 8.90
0 -2 15 60.77 9.30
0 -2 15 66.82 10.09
0 2 15 81.29 11.54
0 2 16 119.55 12.46
0 2 16 74.27 6.10
0 2 16 109.57 13.89
0 2 -16 100.41 8.83
0 -2 16 106.96 12.75
0 -2 16 109.38 13.44
0 2 17 231.86 17.32
0 -2 17 254.51 21.92
0 2 17 271.41 24.11
0 2 -17 198.72 15.44
0 -2 17 254.94 23.08
0 2 17 275.17 21.72
0 2 18 20.27 6.51
0 2 18 10.91 3.25
0 2 18 8.76 3.47
0 -2 18 13.87 5.53
0 -2 18 17.67 5.20
0 2 19 0.74 1.49
0 -2 19 2.96 2.38
0 -2 19 2.90 2.58
0 2 19 0.57 1.14
0 2 19 0.89 0.41
0 -2 20 -0.52 1.56
0 2 20 -0.14 0.34
0 -2 20 1.21 1.58
0 2 20 -1.33 1.71
0 -2 21 2.06 2.02
0 2 21 0.21 1.47
0 -2 21 0.52 1.46
0 2 21 -0.69 1.31
0 -2 22 2.67 2.02
0 -2 22 1.74 1.97
0 2 22 0.57 1.18
0 2 22 -0.19 0.81
0 -2 23 70.15 11.59
0 -2 23 90.10 14.24
0 2 23 67.27 12.73
0 -2 24 104.54 14.84
0 -2 24 143.57 18.82
0 2 24 127.78 18.19
0 -2 25 11.10 4.69
0 2 25 14.57 6.03
0 -2 26 3.26 2.91
0 2 26 2.60 3.25
0 -2 27 2.85 3.34
0 2 27 4.00 2.31
0 -2 28 2.97 1.30
0 2 28 1.77 1.22
0 2 29 11.10 5.22
0 -2 29 7.97 4.80
0 -2 30 -0.85 2.50
0 2 30 2.23 3.44
0 -2 31 1.44 2.27
0 2 31 12.25 6.07
0 -2 32 4.52 3.55
0 2 32 1.45 1.82
0 2 33 4.87 2.71
0 -2 33 11.21 5.87
0 -2 34 3.44 4.11
0 2 34 -1.04 3.09
0 2 35 6.29 4.54
0 -2 35 2.23 2.68
0 -3 0 0.24 1.41
0 -3 1 1480.53 82.71
0 -3 -1 1545.08 83.65
0 -3 2 54.73 6.75
0 -3 2 48.96 7.14
0 -3 -2 50.31 7.56
0 -3 -3 10.46 3.28
0 -3 3 18.75 3.74
0 -3 3 13.96 3.68
0 -3 4 2680.62 140.90
0 -3 -4 2601.81 141.61
0 -3 4 2754.96 139.93
0 -3 -5 83.88 10.29
0 -3 5 76.56 8.87
0 -3 5 67.86 8.83
0 -3 6 1696.20 86.37
0 -3 -6 1667.10 95.23
0 -3 6 1845.50 93.97
0 -3 7 52.88 8.54
0 -3 7 50.04 7.65
0 -3 -7 47.57 8.22
0 -3 8 3297.22 172.35
0 -3 8 3448.08 174.80
0 -3 -8 3110.90 174.55
0 -3 9 117.03 13.62
0 -3 -9 108.78 14.24
0 -3 9 115.20 13.14
0 -3 10 14.95 4.48
0 -3 10 8.47 3.30
0 -3 -10 8.39 4.09
0 -3 -11 21.30 6.57
0 -3 11 43.49 7.76
0 -3 11 36.49 7.22
0 -3 -11 24.21 3.85
0 -3 -12 768.18 55.97
0 -3 12 800.24 51.49
0 3 12 763.93 49.04
0 -3 -12 841.31 44.75
0 -3 12 763.65 51.44
0 -3 -13 318.89 31.76
0 -3 13 352.29 28.55
0 -3 13 356.77 28.56
0 3 13 367.72 26.95
0 3 13 320.30 23.21
0 3 13 344.43 27.95
0 -3 -13 383.13 22.17
0 3 14 87.74 9.04
0 -3 14 90.84 12.54
0 3 14 77.61 10.68
0 -3 -14 101.19 16.07
0 -3 14 93.10 12.53
0 3 14 90.21 12.25
0 3 15 -0.61 0.80
0 3 15 -0.45 0.96
0 -3 -15 0.85 2.49
0 -3 15 3.36 2.65
0 -3 15 -0.54 1.69
0 3 15 -0.36 1.66
0 -3 16 916.61 62.32
0 -3 16 997.39 63.05
0 -3 -16 1160.90 75.71
0 3 16 1015.30 60.82
0 3 16 956.79 55.61
0 3 16 1029.25 64.15
0 3 17 7.84 2.33
0 -3 17 15.08 5.93
0 3 17 7.93 3.06
0 3 17 6.60 6.36
0 -3 17 18.30 7.50
0 -3 -17 7.75 5.08
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0 -3 18 421.37 34.43
0 3 18 457.24 33.18
0 -3 18 458.45 35.73
0 3 18 479.61 37.22
0 3 19 18.48 5.18
0 -3 19 34.70 8.59
0 -3 19 19.10 6.55
0 3 19 21.99 7.23
0 3 20 183.64 17.61
0 -3 20 168.42 18.87
0 -3 20 150.70 17.62
0 3 20 146.98 18.30
0 -3 21 15.83 5.89
0 3 21 16.99 6.67
0 3 21 11.83 3.28
0 3 21 16.33 5.12
0 -3 21 28.08 7.95
0 -3 22 29.84 7.94
0 3 22 29.41 8.06
0 -3 22 26.40 7.25
0 3 22 28.26 7.18
0 -3 23 40.10 9.56
0 3 23 31.35 8.50
0 3 24 9.17 4.66
0 -3 24 6.56 4.17
0 -3 25 1.02 0.81
0 3 25 3.22 3.58
0 3 26 36.25 10.02
0 -3 26 50.79 11.31
0 -3 27 2.70 2.15
0 3 27 0.07 3.04
0 3 28 32.64 9.70
0 -3 28 35.83 9.97
0 -3 29 3.80 3.62
0 3 29 -2.01 2.22
0 3 30 0.59 2.06
0 -3 30 10.60 5.98
0 3 31 2.79 2.80
0 -3 31 -0.37 1.74
0 3 32 -1.68 2.40
0 -3 32 -1.08 3.09
0 3 33 -1.25 2.52
0 -3 33 4.61 3.94
0 3 34 -0.08 2.51
0 -3 34 4.32 3.50
0 -3 35 -0.08 3.35
0 -4 0 528.75 36.24
0 -4 1 266.81 22.57
0 -4 -1 301.25 23.72
0 -4 2 1462.35 83.04
0 -4 -2 1473.50 83.92
0 -4 3 29.10 5.87
0 -4 3 29.34 5.65
0 -4 -3 28.78 6.09
0 -4 4 279.18 23.15
0 -4 -4 296.77 24.39
0 -4 4 305.54 22.62
0 -4 5 9.17 3.41
0 -4 5 11.54 3.53
0 -4 -5 7.20 3.14
0 -4 6 1034.17 58.36
0 -4 -6 858.41 58.94
0 -4 6 1017.27 59.51
0 -4 7 65.78 9.68
0 -4 -7 76.59 11.14
0 -4 7 64.67 9.18
0 -4 -8 411.29 34.07
0 -4 8 441.78 32.68
0 -4 8 495.45 33.12
0 -4 9 9.91 1.92
0 -4 9 10.97 3.81
0 -4 -9 12.67 4.69
0 -4 -10 1647.25 99.86
0 -4 10 1717.75 95.96
0 -4 -11 2.17 2.10
0 -4 11 1.61 0.85
0 -4 12 185.26 18.82
0 -4 -12 168.75 21.27
0 -4 13 463.73 33.62
0 -4 -13 409.75 37.21
0 -4 -13 379.44 26.36
0 -4 -14 0.96 0.61
0 -4 -14 -0.70 1.93
0 -4 14 -1.13 1.46
0 -4 -15 39.89 5.75
0 4 15 55.30 9.12
0 -4 15 50.26 9.46
0 4 15 48.55 9.16
0 -4 -15 46.15 11.66
0 4 16 131.10 15.36
0 4 16 144.47 17.28
0 -4 -16 128.24 20.44
0 -4 16 143.44 17.15
0 4 16 127.18 12.33
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-5 1 5 -3.00 6.02
-5 1 -5 7.42 5.26
-5 -1 -6 -0.20 3.66
-5 -1 6 4.44 6.34
-5 1 6 8.85 8.41
-5 1 -6 -3.56 2.53
-5 -1 6 2.63 4.66
-5 1 6 -0.74 1.18
-5 1 -6 -5.75 5.19
-5 -1 -7 4.28 4.92
-5 -1 7 10.41 10.59
-5 1 7 1.93 6.45
-5 1 -7 7.30 6.89
-5 -1 7 -0.59 3.07
-5 1 7 6.41 7.01
-5 -1 -8 -2.34 7.78
-5 -1 8 1.58 4.35
-5 -1 8 2.84 2.45
-5 1 -8 2.86 4.61
-5 1 8 6.30 5.75
-5 1 8 2.60 7.07
-5 -1 -9 -11.96 9.04
-5 -1 9 -10.01 7.08
-5 -1 9 2.03 3.27
-5 1 -9 9.11 9.21
-5 1 9 2.04 3.29
-5 1 9 0.16 4.52
-5 -1 -10 7.25 7.37
-5 -1 10 1.54 2.13
-5 -1 10 2.38 3.72
-5 1 -10 4.13 5.81
-5 1 10 -3.77 2.96
-5 -1 -11 2.73 9.24
-5 -1 11 2.96 0.95
-5 -1 11 4.56 3.66
-5 1 -11 1.53 3.27
-5 1 11 -2.62 3.81
-5 1 11 -0.07 0.98
-5 -1 -12 6.32 10.33
-5 -1 12 -3.81 4.32
-5 1 -12 0.45 6.75
-5 1 12 3.85 4.96
-5 1 12 1.35 1.49
-5 -1 -13 8.35 8.28
-5 -1 13 -1.81 2.60
-5 1 -13 -8.04 7.20
-5 1 13 -1.38 3.12
-5 1 13 -0.95 3.27
-5 -1 -14 -2.61 12.85
-5 -1 14 2.86 3.44
-5 1 -14 6.95 7.03
-5 1 14 2.66 4.34
-5 1 14 -2.44 5.68
-5 -1 -15 1.03 3.24
-5 -1 15 -1.79 2.93
-5 1 -15 3.13 7.18
-5 1 15 3.72 4.75
-5 1 15 -5.75 6.78
-5 -1 16 -0.23 3.81
-5 -1 -16 2.26 7.52
-5 -1 16 1.52 3.16
-5 1 16 0.25 1.13
-5 -1 -17 -10.47 11.42
-5 -1 17 1.68 3.56
-5 1 -17 -10.81 9.88
-5 1 17 -1.47 3.27
-5 -1 18 -9.19 6.50
-5 1 -18 10.51 10.19
-5 1 18 2.10 1.52
-5 2 0 -5.22 5.24
-5 2 0 -4.53 4.66
-5 -2 -1 13.21 9.08
-5 -2 1 10.49 4.65
-5 2 1 1.91 3.44
-5 2 -1 1.76 4.66
-5 2 1 12.39 8.57
-5 2 -1 16.67 10.52
-5 -2 -2 -2.60 1.43
-5 -2 2 0.42 3.08
-5 2 2 4.22 4.74
-5 2 -2 -0.12 3.56
-5 2 -2 -5.62 5.57
-5 -2 -3 5.46 6.21
-5 -2 3 -0.99 4.93
-5 2 3 -2.38 5.23
-5 2 -3 1.76 4.10
-5 2 3 8.37 7.90
-5 2 -3 -5.31 5.32
-5 -2 -4 5.70 6.28
-5 -2 4 10.67 8.43
-5 2 4 5.91 6.78
-5 2 -4 1.92 2.99
-5 2 4 -9.50 7.71
-5 2 -4 -1.17 2.03
-5 -2 -5 1.78 5.98
-5 -2 5 -4.66 6.58
-5 2 5 -5.39 6.77
-5 2 -5 -0.27 4.38
-5 2 5 -1.46 1.63
-5 2 -5 -4.64 4.80
-5 -2 -6 1.95 6.12
-5 -2 6 13.14 8.56
-5 2 6 4.15 3.58
-5 2 -6 -1.16 3.95
-5 2 6 6.83 7.21
-5 2 -6 -4.68 4.72
-5 -2 -7 5.44 5.74
-5 -2 7 3.98 1.59
-5 2 7 3.87 6.02
-5 2 -7 -6.75 5.50
-5 2 7 -4.47 5.99
-5 2 -7 -1.56 2.67
-5 -2 -8 4.08 1.59
-5 -2 8 10.28 8.32
-5 2 8 6.34 6.09
-5 2 -8 -4.19 1.50
-5 2 8 4.60 3.30
-5 -2 9 8.18 7.53
-5 -2 -9 25.87 14.96
-5 -2 9 11.88 7.60
-5 2 9 19.21 9.94
-5 2 -9 13.27 9.36
-5 2 9 22.48 13.47
-5 -2 10 1.47 1.41
-5 -2 -10 5.04 3.88
-5 -2 10 -5.87 5.39
-5 2 10 -6.78 7.85
-5 2 -10 2.37 3.94
-5 2 10 4.86 9.00
-5 -2 11 3.51 5.21
-5 -2 -11 17.10 14.11
-5 -2 11 -3.12 3.91
-5 2 11 5.91 7.45
-5 2 -11 -0.39 1.38
-5 2 11 3.99 7.85
-5 -2 12 8.90 6.46
-5 -2 -12 2.96 10.16
-5 -2 12 -11.78 7.59
-5 2 12 0.84 4.17
-5 2 -12 0.35 2.24
-5 2 12 13.84 11.71
-5 -2 -13 -3.13 10.28
-5 -2 13 7.02 7.20
-5 2 13 9.59 6.87
-5 2 -13 -3.86 4.52
-5 2 13 4.86 4.41
-5 -2 14 -4.41 5.58
-5 -2 -14 8.68 10.33
-5 -2 14 5.41 4.83
-5 2 14 5.13 6.78
-5 2 -14 2.27 0.77
-5 2 14 4.56 8.96
-5 -2 15 -0.88 4.12
-5 -2 -15 0.66 2.51
-5 -2 15 1.15 1.01
-5 2 -15 6.01 7.41
-5 2 15 -2.98 1.28
-5 2 15 7.28 6.60
-5 -2 -16 1.50 3.27
-5 -2 16 4.95 4.34
-5 2 -16 13.92 10.57
-5 2 16 2.05 3.32
-5 -2 -17 10.28 4.18
-5 -2 17 1.28 1.13
-5 2 -17 -13.85 10.00
-5 2 17 -12.10 8.00
-5 -2 18 -4.91 4.74
-5 2 18 5.96 6.04
-5 -3 0 -6.29 5.33
-5 -3 0 4.51 1.75
-5 3 0 3.44 5.85
-5 -3 -1 0.77 4.47
-5 -3 1 -2.39 5.06
-5 -3 -1 1.94 3.38
-5 -3 1 -0.20 4.93
-5 3 1 -13.74 9.58
-5 3 -1 -7.69 6.98
-5 -3 -2 -2.43 4.72
-5 -3 2 1.24 2.36
-5 -3 -2 8.42 8.66
-5 -3 2 -10.41 7.50
-5 3 2 9.67 7.71
-5 3 -2 -2.03 6.50
-5 -3 3 -4.15 4.74
-5 -3 -3 -1.39 5.92
-5 -3 3 -1.80 6.59
-5 3 3 2.45 1.06
-5 3 -3 -6.16 6.06
-5 -3 4 -1.68 0.92
-5 -3 -4 4.02 4.18
-5 -3 4 -4.02 4.59
-5 3 4 3.36 4.44
-5 3 -4 2.35 4.24
-5 -3 5 -0.85 3.37
-5 -3 -5 -2.90 6.04
-5 -3 5 -3.13 4.76
-5 3 5 2.03 3.56
-5 3 -5 -0.83 3.54
-5 -3 6 2.97 3.06
-5 -3 -6 -6.31 10.29
-5 -3 6 2.99 5.98
-5 3 6 4.21 8.73
-5 3 -6 0.40 1.57
-5 -3 7 2.21 3.19
-5 -3 -7 -2.36 4.67
-5 -3 7 -1.14 3.09
-5 3 7 -0.92 3.85
-5 3 -7 4.41 4.19
-5 3 7 6.99 3.73
-5 3 -7 -10.71 7.28
-5 -3 8 3.97 4.47
-5 -3 -8 4.10 5.42
-5 -3 8 6.42 4.19
-5 3 8 4.09 7.51
-5 3 -8 0.53 2.30
-5 3 8 7.10 8.81
-5 3 -8 -1.18 4.17
-5 -3 9 -0.65 1.22
-5 3 9 3.72 0.33
-5 3 -9 -0.72 3.11
-5 3 9 1.64 0.61
-5 -3 10 12.47 8.28
-5 -3 -10 5.59 10.57
-5 -3 10 0.08 5.05
-5 3 10 9.10 7.68
-5 3 -10 -8.02 5.67
-5 3 10 -14.60 10.27
-5 -3 11 -0.70 2.87
-5 -3 -11 -3.09 5.12
-5 -3 11 -0.49 3.34
-5 3 11 3.19 3.79
-5 3 -11 0.62 2.13
-5 3 11 2.21 3.23
-5 -3 12 4.76 4.81
-5 -3 -12 -6.67 6.69
-5 -3 12 -6.95 5.84
-5 3 12 3.74 6.08
-5 3 -12 1.44 2.46
-5 3 12 4.79 4.72
-5 -3 13 0.19 1.75
-5 -3 -13 -10.99 10.21
-5 -3 13 -2.08 2.86
-5 3 13 9.89 7.82
-5 3 -13 3.53 4.78
-5 3 13 1.62 5.21
-5 -3 14 6.27 5.39
-5 -3 14 0.48 0.99
-5 3 14 2.12 7.34
-5 3 -14 4.38 4.31
-5 -3 15 -2.23 5.28
-5 -3 -15 3.83 10.13
-5 -3 15 5.06 5.78
-5 3 15 -13.82 8.85
-5 3 -15 3.20 6.31
-5 -3 -16 -17.70 14.57
-5 -3 16 7.41 7.51
-5 3 16 7.40 6.74
-5 3 -16 -9.03 6.83
-5 -3 -17 -17.35 15.01
-5 -3 17 -9.94 6.82
-5 3 17 1.29 2.38
-5 3 -17 -3.37 4.35
-5 -3 18 -7.42 5.90
-5 3 18 -11.08 7.83
-5 4 0 -3.38 6.09
-5 -4 0 0.02 1.01
-5 -4 0 -0.34 3.82
5 -4 0 2.45 3.60
-5 4 -1 -1.57 9.21
-5 -4 -1 10.57 7.59
-5 -4 1 -0.73 1.37
-5 -4 -1 -4.02 1.77
-5 -4 1 -5.54 5.13
5 -4 -1 1.26 2.94
5 -4 1 4.43 4.48
-5 4 1 -2.82 7.37
-5 4 -2 -1.63 6.72
-5 -4 2 -1.73 4.07
-5 -4 -2 0.42 4.65
-5 -4 2 6.52 3.94
5 -4 2 3.11 4.89
-5 4 2 -0.10 5.80
-5 -4 3 -1.19 4.14
-5 -4 -3 2.97 3.96
5 -4 3 0.57 0.85
-5 4 3 0.57 3.97
-5 -4 4 5.59 6.81
-5 -4 -4 8.52 8.02
-5 -4 4 1.33 4.83
5 -4 4 0.84 0.87
-5 4 4 -0.04 3.88
-5 -4 5 -3.55 4.05
-5 -4 -5 -4.87 6.63
-5 -4 5 1.44 0.39
5 -4 5 -0.08 1.36
-5 4 5 -1.37 4.87
-5 -4 6 -0.33 1.51
-5 -4 -6 7.21 9.34
-5 -4 6 5.04 6.75
5 -4 6 3.17 2.97
-5 4 6 13.63 10.59
-5 -4 7 -1.97 4.15
-5 -4 -7 1.79 7.50
-5 -4 7 -4.04 4.24
5 -4 7 1.76 1.28
-5 4 7 0.75 1.44
-5 -4 8 -2.04 1.73
-5 -4 -8 2.51 3.04
-5 -4 8 2.40 4.84
5 -4 8 -0.85 2.81
-5 4 8 4.79 9.22
-5 -4 9 -5.94 5.34
-5 -4 -9 -0.58 5.11
-5 -4 9 4.06 7.46
5 -4 9 0.56 2.27
-5 4 9 -6.49 10.27
-5 -4 10 -1.31 6.42
-5 -4 -10 4.82 6.61
-5 -4 10 4.56 3.93
5 -4 10 1.70 3.25
-5 4 10 -1.96 7.84
-5 -4 11 0.10 1.96
-5 -4 -11 1.12 1.99
-5 -4 11 -3.12 4.95
5 -4 11 0.26 3.14
-5 4 11 11.04 12.15
-5 -4 12 -5.76 5.33
-5 -4 -12 -4.20 10.29
-5 -4 12 17.77 12.26
5 -4 12 -4.31 3.48
-5 4 12 0.95 6.15
-5 -4 13 0.46 5.69
-5 -4 -13 -7.99 8.81
-5 -4 13 -8.91 6.59
-5 4 13 -2.44 6.98
5 -4 13 2.73 3.16
-5 4 13 -2.60 2.63
-5 -4 14 -5.10 6.32
-5 -4 -14 3.15 9.77
-5 -4 14 5.88 7.50
-5 4 14 3.21 5.19
-5 4 -14 -0.87 1.82
5 -4 14 0.08 0.66
-5 -4 -15 -5.48 7.77
-5 -4 15 0.44 6.26
-5 4 15 0.58 4.82
-5 4 -15 -6.36 5.03
5 -4 15 7.59 4.78
-5 -4 -16 12.52 11.26
-5 -4 16 -3.50 4.12
-5 4 16 7.90 8.62
-5 4 -16 2.95 1.50
-5 -4 -17 2.58 11.37
-5 -4 17 2.54 7.10
-5 4 17 0.52 5.48
-5 4 -17 3.13 1.93
-5 -5 0 -3.05 6.24
5 -5 0 2.24 4.05
-5 -5 0 -2.23 1.42
-5 -5 -1 -3.31 4.42
-5 -5 1 -0.17 1.72
5 -5 -1 -1.73 3.58
5 -5 1 -10.78 6.10
-5 -5 1 -9.93 6.89
-5 -5 2 -11.47 7.97
5 -5 -2 -1.04 1.93
5 -5 2 -1.66 2.62
-5 -5 2 -10.04 6.91
-5 5 3 9.26 11.80
-5 -5 -3 5.12 6.51
-5 -5 3 6.57 7.00
5 -5 -3 6.57 5.61
5 -5 3 2.90 3.35
-5 -5 3 2.26 2.29
-5 5 4 5.59 7.31
-5 -5 -4 6.78 6.48
-5 -5 4 2.85 3.32
5 -5 -4 -4.05 3.84
5 -5 4 -1.34 2.29
-5 -5 4 -1.17 4.19
-5 -5 -5 10.76 9.55
-5 -5 5 4.74 3.79
5 -5 -5 4.58 4.07
5 -5 5 -1.01 1.76
-5 -5 5 -1.07 5.22
-5 5 5 3.88 0.45
-5 -5 -6 -1.31 6.26
-5 -5 6 -1.90 5.97
5 -5 6 -2.35 2.73
-5 5 6 -6.64 8.86
-5 -5 6 1.64 3.13
-5 -5 -7 -9.97 8.46
-5 -5 7 5.01 4.01
5 -5 7 -1.02 4.04
-5 5 7 -8.94 9.37
-5 -5 7 -3.82 6.89
-5 -5 -8 -19.46 12.06
-5 -5 8 -1.62 3.94
5 -5 8 0.23 1.51
-5 5 8 7.85 8.48
-5 -5 8 -13.49 8.08
-5 -5 -9 -15.69 11.16
-5 -5 9 -0.65 3.97
5 -5 9 -0.85 0.59
-5 5 9 -4.21 5.37
-5 -5 9 -7.71 6.13
-5 -5 -10 -19.87 12.85
-5 -5 10 -1.65 5.31
5 -5 10 -0.75 3.11
-5 5 10 14.39 13.29
-5 -5 10 -13.01 8.00
-5 -5 -11 7.95 6.14
-5 -5 11 -4.39 4.74
5 -5 11 -1.73 2.22
-5 -5 11 -1.52 2.75
-5 -5 -12 9.78 9.07
-5 -5 12 4.66 4.70
5 -5 12 1.29 1.47
-5 -5 12 -3.34 4.09
-5 -5 -13 4.87 2.86
-5 -5 13 -7.88 6.31
5 -5 13 2.31 1.77
-5 -5 13 -3.20 5.59
-5 -5 14 5.88 6.47
5 -5 14 0.32 1.25
-5 -5 -15 2.63 11.44
5 -5 15 0.71 2.39
-5 5 -17 -0.02 1.48
-5 -6 0 -4.30 4.08
5 -6 0 -5.01 4.27
-5 -6 -1 9.95 6.87
-5 -6 1 12.11 8.77
5 -6 -1 -1.33 3.67
5 -6 1 1.24 2.46
-5 -6 -2 -1.99 8.85
-5 -6 2 9.51 10.00
5 -6 -2 4.82 3.55
5 -6 2 2.25 3.38
-5 -6 2 4.89 6.85
-5 -6 3 1.48 2.29
5 -6 -3 4.16 2.79
5 -6 3 -0.08 0.52
-5 -6 3 1.40 0.87
-5 -6 -4 -3.79 8.68
-5 -6 4 2.81 4.39
5 -6 -4 0.23 0.84
5 -6 4 -2.47 3.02
-5 -6 4 -0.96 4.88
-5 -6 -5 4.14 5.17
-5 -6 5 1.38 4.37
5 -6 -5 0.03 2.02
5 -6 5 -1.49 0.63
-5 -6 5 -2.03 5.45
-5 -6 -6 -4.30 1.69
-5 -6 6 -0.38 1.55
5 -6 -6 -4.59 4.19
5 -6 6 -2.47 2.86
-5 -6 6 -2.60 6.50
-5 6 7 10.22 15.19
-5 -6 -7 -7.62 11.19
-5 -6 7 -5.98 7.39
5 -6 -7 -3.06 3.43
5 -6 7 -0.29 2.42
-5 -6 7 -12.37 7.84
-5 -6 -8 2.53 3.86
-5 -6 8 -9.43 7.10
5 -6 -8 -6.29 4.94
5 -6 8 1.27 0.55
-5 -6 8 2.31 0.91
-5 6 8 -13.44 13.18
-5 -6 9 -10.80 7.58
5 -6 9 -1.05 4.61
-5 -6 9 -5.90 5.44
-5 -6 -10 -8.57 8.50
5 -6 10 -0.19 0.77
-5 -6 10 -6.48 5.72
-5 -6 11 -3.56 6.55
-5 -7 3 4.01 4.35
-5 -7 4 -3.93 4.56
-5 -7 5 1.81 3.04
-5 -7 6 3.48 2.22
-5 -7 7 -1.37 4.43
-5 -7 8 3.04 5.04
-5 -7 9 -5.19 5.19
-5 -8 4 2.26 2.55
-5 -8 5 -5.61 5.63
-5 -8 6 1.53 4.68
-5 -8 7 0.67 5.08
-6 0 1 1.88 3.73
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 58935
_shelx_res_file
;
TITL 1a.res in P2(1)2(1)2(1)
1a.res
created by SHELXL-2016/6 at 17:44:51 on 21-Sep-2020
CELL 0.71073 3.9876 10.6511 25.1065 90 90 90
ZERR 4 0.0005 0.0013 0.0024 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O S
UNIT 44 40 8 8 4
L.S. 4 0 0
PLAN 20
BOND $H
list 4
fmap 2 53
acta
conf
size 0.2 0.15 0.08
temp 20
htab n2 o1
eqiv $1 0.5+x,1.5-y,1-z
htab n2 n2_$1
htab n2 o1_$1
OMIT 0 50
WGHT 0.083500
FVAR 0.90953
S1 5 0.239366 0.358154 0.547631 11.00000 0.07905 0.05410 =
0.06733 0.00144 0.00227 -0.00415
O1 4 0.565091 0.578186 0.433128 11.00000 0.10141 0.06185 =
0.06609 0.00474 0.01292 -0.00591
O2 4 0.269967 0.398072 0.433302 11.00000 0.09156 0.06413 =
0.05942 -0.00466 -0.00541 -0.00403
N1 3 0.318133 0.413337 0.607203 11.00000 0.08602 0.05396 =
0.06275 0.00631 0.00708 -0.00185
N2 3 0.678200 0.680232 0.539429 11.00000 0.07537 0.05430 =
0.06801 0.00322 0.00069 -0.01002
H2NA 2 0.751409 0.690362 0.510148 11.00000 0.08999
H2NB 2 0.828558 0.718972 0.561647 11.00000 0.07959
C1 1 0.464722 0.524564 0.604407 11.00000 0.06303 0.05074 =
0.06186 0.00376 -0.00046 0.00791
C2 1 0.528839 0.569543 0.551334 11.00000 0.05341 0.05141 =
0.06375 0.00518 -0.00018 0.00327
C3 1 0.408023 0.483469 0.514417 11.00000 0.06325 0.05521 =
0.05660 -0.00012 0.00059 0.00420
C4 1 0.425738 0.493557 0.457145 11.00000 0.06798 0.05737 =
0.05934 -0.00076 0.00180 0.00743
C5 1 0.277026 0.394871 0.376401 11.00000 0.10617 0.08993 =
0.05915 -0.00565 -0.00983 0.00362
AFIX 137
H5A 2 0.182862 0.471159 0.362582 11.00000 -1.50000
H5B 2 0.148297 0.324580 0.363958 11.00000 -1.50000
H5C 2 0.504661 0.386723 0.364444 11.00000 -1.50000
AFIX 0
C6 1 0.561572 0.590872 0.653737 11.00000 0.05751 0.06120 =
0.06097 0.00235 -0.00054 -0.00276
C7 1 0.713677 0.527290 0.695196 11.00000 0.07625 0.07154 =
0.06426 0.00901 -0.00348 0.00042
AFIX 43
H7 2 0.760580 0.442141 0.691773 11.00000 -1.20000
AFIX 0
C8 1 0.796232 0.589111 0.741520 11.00000 0.08910 0.09248 =
0.05903 0.00024 -0.00887 -0.00576
AFIX 43
H8 2 0.895947 0.544633 0.769183 11.00000 -1.20000
AFIX 0
C9 1 0.735385 0.713141 0.747643 11.00000 0.08887 0.09214 =
0.05876 -0.00780 -0.00464 -0.01768
AFIX 43
H9 2 0.794107 0.753853 0.779057 11.00000 -1.20000
AFIX 0
C10 1 0.584163 0.778844 0.706427 11.00000 0.09939 0.06475 =
0.07919 -0.00915 0.00911 -0.01085
AFIX 43
H10 2 0.540439 0.864097 0.710404 11.00000 -1.20000
AFIX 0
C11 1 0.497891 0.719279 0.659632 11.00000 0.08575 0.06007 =
0.06586 0.00116 0.00139 0.00916
AFIX 43
H11 2 0.397894 0.764232 0.632133 11.00000 -1.20000
AFIX 0
HKLF 4
REM 1a.res in P2(1)2(1)2(1)
REM R1 = 0.0551 for 1448 Fo > 4sig(Fo) and 0.0708 for all 1884 data
REM 154 parameters refined using 0 restraints
END
WGHT 0.0835 0.0000
REM Highest difference peak 0.324, deepest hole -0.274, 1-sigma level 0.056
Q1 1 0.0817 0.4978 0.4625 11.00000 0.05 0.19
Q2 1 0.9293 0.5817 0.6573 11.00000 0.05 0.17
Q3 1 0.0523 0.4780 0.6358 11.00000 0.05 0.17
Q4 1 0.7745 0.5775 0.6406 11.00000 0.05 0.17
Q5 1 0.0524 0.4754 0.5038 11.00000 0.05 0.17
Q6 1 0.2554 0.4000 0.6612 11.00000 0.05 0.16
Q7 1 0.7433 0.4516 0.5166 11.00000 0.05 0.16
Q8 1 0.0465 0.4822 0.5996 11.00000 0.05 0.15
Q9 1 0.5054 0.4453 0.3589 11.00000 0.05 0.15
Q10 1 -0.0839 0.3655 0.5404 11.00000 0.05 0.15
Q11 1 0.4557 0.5206 0.3412 11.00000 0.05 0.15
Q12 1 0.7707 0.4351 0.5838 11.00000 0.05 0.15
Q13 1 0.0332 0.4284 0.3610 11.00000 0.05 0.15
Q14 1 0.2574 0.3564 0.3593 11.00000 0.05 0.15
Q15 1 -0.1633 0.4590 0.3638 11.00000 0.05 0.15
Q16 1 0.9729 0.6948 0.5377 11.00000 0.05 0.14
Q17 1 0.7627 0.5330 0.3996 11.00000 0.05 0.14
Q18 1 0.2380 0.6201 0.6564 11.00000 0.05 0.14
Q19 1 1.0011 0.3542 0.6491 11.00000 0.05 0.14
Q20 1 0.9660 0.6837 0.6528 11.00000 0.05 0.14
;
_shelx_res_checksum 12184
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 0.2394(4) 0.35815(11) 0.54763(5) 0.0668(5) Uani d 1 . .
O O1 0.5651(12) 0.5782(4) 0.43313(14) 0.0764(12) Uani d 1 . .
O O2 0.2700(12) 0.3981(3) 0.43330(12) 0.0717(10) Uani d 1 . .
N N1 0.3181(13) 0.4133(4) 0.60720(15) 0.0676(12) Uani d 1 . .
N N2 0.6782(13) 0.6802(4) 0.5394(2) 0.0659(12) Uani d 1 . .
H H2NA 0.751(17) 0.690(6) 0.510(2) 0.09(2) Uiso d 1 . .
H H2NB 0.829(16) 0.719(6) 0.562(2) 0.080(19) Uiso d 1 . .
C C1 0.4647(13) 0.5246(5) 0.60441(19) 0.0585(12) Uani d 1 . .
C C2 0.5288(12) 0.5695(5) 0.55133(19) 0.0562(11) Uani d 1 . .
C C3 0.4080(13) 0.4835(5) 0.51442(18) 0.0584(13) Uani d 1 . .
C C4 0.4257(13) 0.4936(5) 0.4571(2) 0.0616(12) Uani d 1 . .
C C5 0.277(2) 0.3949(6) 0.37640(19) 0.0851(18) Uani d 1 . .
H H5A 0.182862 0.471159 0.362582 0.128 Uiso calc 1 . .
H H5B 0.148297 0.324580 0.363958 0.128 Uiso calc 1 . .
H H5C 0.504661 0.386723 0.364444 0.128 Uiso calc 1 . .
C C6 0.5616(13) 0.5909(5) 0.65374(18) 0.0599(13) Uani d 1 . .
C C7 0.7137(16) 0.5273(5) 0.69520(19) 0.0707(14) Uani d 1 . .
H H7 0.760580 0.442141 0.691773 0.085 Uiso calc 1 . .
C C8 0.7962(19) 0.5891(6) 0.74152(19) 0.0802(17) Uani d 1 . .
H H8 0.895947 0.544633 0.769183 0.096 Uiso calc 1 . .
C C9 0.7354(18) 0.7131(6) 0.74764(19) 0.0799(16) Uani d 1 . .
H H9 0.794107 0.753853 0.779057 0.096 Uiso calc 1 . .
C C10 0.5842(16) 0.7788(6) 0.7064(2) 0.0811(17) Uani d 1 . .
H H10 0.540439 0.864097 0.710404 0.097 Uiso calc 1 . .
C C11 0.4979(17) 0.7193(5) 0.6596(2) 0.0706(15) Uani d 1 . .
H H11 0.397894 0.764232 0.632133 0.085 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 0.0790(9) 0.0541(8) 0.0673(8) -0.0041(8) 0.0023(8) 0.0014(5)
O1 0.101(3) 0.062(2) 0.066(2) -0.006(2) 0.013(2) 0.0047(19)
O2 0.092(3) 0.064(2) 0.0594(18) -0.004(2) -0.0054(19) -0.0047(16)
N1 0.086(3) 0.054(3) 0.063(2) -0.002(2) 0.007(2) 0.0063(19)
N2 0.075(3) 0.054(3) 0.068(3) -0.010(2) 0.001(2) 0.003(2)
C1 0.063(3) 0.051(3) 0.062(3) 0.008(2) 0.000(2) 0.004(2)
C2 0.053(3) 0.051(3) 0.064(3) 0.003(2) 0.000(2) 0.005(2)
C3 0.063(3) 0.055(3) 0.057(3) 0.004(2) 0.001(2) 0.000(2)
C4 0.068(3) 0.057(3) 0.059(3) 0.007(2) 0.002(2) -0.001(2)
C5 0.106(5) 0.090(4) 0.059(3) 0.004(4) -0.010(3) -0.006(3)
C6 0.058(3) 0.061(3) 0.061(3) -0.003(2) -0.001(2) 0.002(2)
C7 0.076(4) 0.072(4) 0.064(3) 0.000(3) -0.003(3) 0.009(2)
C8 0.089(4) 0.092(5) 0.059(3) -0.006(4) -0.009(3) 0.000(3)
C9 0.089(4) 0.092(5) 0.059(3) -0.018(4) -0.005(3) -0.008(3)
C10 0.099(4) 0.065(4) 0.079(3) -0.011(3) 0.009(3) -0.009(3)
C11 0.086(4) 0.060(4) 0.066(3) 0.009(3) 0.001(3) 0.001(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N1 S1 C3 . . 95.1(2) ?
C4 O2 C5 . . 117.2(4) ?
C1 N1 S1 . . 111.0(3) ?
C2 N2 H2NA . . 119(5) ?
C2 N2 H2NB . . 123(4) ?
H2NA N2 H2NB . . 105(6) ?
N1 C1 C2 . . 115.2(4) ?
N1 C1 C6 . . 119.9(4) ?
C2 C1 C6 . . 124.8(5) ?
N2 C2 C3 . . 125.4(5) ?
N2 C2 C1 . . 124.9(5) ?
C3 C2 C1 . . 109.7(5) ?
C2 C3 C4 . . 126.7(5) ?
C2 C3 S1 . . 109.0(4) ?
C4 C3 S1 . . 124.2(4) ?
O1 C4 O2 . . 123.7(5) ?
O1 C4 C3 . . 124.8(5) ?
O2 C4 C3 . . 111.6(5) ?
O2 C5 H5A . . 109.5 ?
O2 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
O2 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
C7 C6 C11 . . 118.6(5) ?
C7 C6 C1 . . 120.8(5) ?
C11 C6 C1 . . 120.6(5) ?
C8 C7 C6 . . 120.5(6) ?
C8 C7 H7 . . 119.8 ?
C6 C7 H7 . . 119.8 ?
C9 C8 C7 . . 121.4(6) ?
C9 C8 H8 . . 119.3 ?
C7 C8 H8 . . 119.3 ?
C8 C9 C10 . . 119.1(5) ?
C8 C9 H9 . . 120.5 ?
C10 C9 H9 . . 120.5 ?
C11 C10 C9 . . 120.8(6) ?
C11 C10 H10 . . 119.6 ?
C9 C10 H10 . . 119.6 ?
C10 C11 C6 . . 119.7(5) ?
C10 C11 H11 . . 120.2 ?
C6 C11 H11 . . 120.2 ?
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 N1 . 1.637(4) ?
S1 C3 . 1.711(5) ?
O1 C4 . 1.219(6) ?
O2 C4 . 1.334(6) ?
O2 C5 . 1.429(6) ?
N1 C1 . 1.323(6) ?
N2 C2 . 1.354(7) ?
N2 H2NA . 0.80(6) ?
N2 H2NB . 0.92(7) ?
C1 C2 . 1.439(6) ?
C1 C6 . 1.477(7) ?
C2 C3 . 1.390(7) ?
C3 C4 . 1.444(7) ?
C5 H5A . 0.9600 ?
C5 H5B . 0.9600 ?
C5 H5C . 0.9600 ?
C6 C7 . 1.382(7) ?
C6 C11 . 1.399(7) ?
C7 C8 . 1.376(7) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.352(9) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.387(8) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.379(7) ?
C10 H10 . 0.9300 ?
C11 H11 . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2NA O1 . 0.80(6) 2.39(6) 2.917(6) 124(6)
N2 H2NA N2 4_566 0.80(6) 2.52(6) 3.179(8) 141(6)
N2 H2NB O1 4_566 0.92(7) 2.36(7) 3.078(6) 135(5)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C3 S1 N1 C1 . . . . 0.8(4) ?
S1 N1 C1 C2 . . . . -1.6(6) ?
S1 N1 C1 C6 . . . . -179.3(4) ?
N1 C1 C2 N2 . . . . -179.5(5) ?
C6 C1 C2 N2 . . . . -1.9(8) ?
N1 C1 C2 C3 . . . . 1.7(7) ?
C6 C1 C2 C3 . . . . 179.3(5) ?
N2 C2 C3 C4 . . . . 1.7(9) ?
C1 C2 C3 C4 . . . . -179.5(5) ?
N2 C2 C3 S1 . . . . -179.8(5) ?
C1 C2 C3 S1 . . . . -1.1(5) ?
N1 S1 C3 C2 . . . . 0.2(4) ?
N1 S1 C3 C4 . . . . 178.7(5) ?
C5 O2 C4 O1 . . . . 1.6(8) ?
C5 O2 C4 C3 . . . . -178.3(5) ?
C2 C3 C4 O1 . . . . 3.4(9) ?
S1 C3 C4 O1 . . . . -174.8(4) ?
C2 C3 C4 O2 . . . . -176.6(5) ?
S1 C3 C4 O2 . . . . 5.1(7) ?
N1 C1 C6 C7 . . . . 43.4(8) ?
C2 C1 C6 C7 . . . . -134.1(6) ?
N1 C1 C6 C11 . . . . -135.9(6) ?
C2 C1 C6 C11 . . . . 46.6(8) ?
C11 C6 C7 C8 . . . . 0.9(9) ?
C1 C6 C7 C8 . . . . -178.5(6) ?
C6 C7 C8 C9 . . . . -0.8(11) ?
C7 C8 C9 C10 . . . . 0.5(11) ?
C8 C9 C10 C11 . . . . -0.3(11) ?
C9 C10 C11 C6 . . . . 0.4(10) ?
C7 C6 C11 C10 . . . . -0.7(9) ?
C1 C6 C11 C10 . . . . 178.7(5) ?