#------------------------------------------------------------------------------
#$Date: 2022-09-13 03:50:53 +0200 (Tue, 13 Sep 2022) $
#$Revision: 277789 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022670.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_2022670
loop_
_publ_author_name
'Cheng, Hong'
'Yan, Dingce'
'Wu, Liqing'
'Liang, Ping'
'Cai, Yuncheng'
'Li, Li'
_publ_section_title
;
Chemical characterization, absolute configuration and optical purity of
(1S)-(+)- and (1R)-(--)-10-camphorsulfonic acid
;
_journal_coeditor_code YP3225
_journal_issue 10
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229622008592
_journal_volume 78
_journal_year 2022
_chemical_absolute_configuration ad
_chemical_formula_iupac 'H3 O +, C10 H15 O4 S -'
_chemical_formula_moiety 'H3 O +, C10 H15 O4 S -'
_chemical_formula_sum 'C10 H18 O5 S'
_chemical_formula_weight 250.30
_chemical_name_systematic
;Hydronium
(1S,4R)-(7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl)methanesulfonate
;
_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
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.72815(4)
_cell_length_b 11.24661(6)
_cell_length_c 15.51195(8)
_cell_measurement_reflns_used 11038
_cell_measurement_temperature 99.8(4)
_cell_measurement_theta_max 73.8320
_cell_measurement_theta_min 2.8330
_cell_volume 1173.772(11)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 99.8(4)
_diffrn_detector 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
;
Rigaku XtaLAB0 PRO MM007HF (rotating anode) diffractometer equipped with a
PILATUS200K CCD plate detector
;
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0280
_diffrn_reflns_av_unetI/netI 0.0123
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 11811
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 73.951
_diffrn_reflns_theta_min 4.857
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 2.522
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.62841
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_density_diffrn 1.416
_exptl_crystal_description block
_exptl_crystal_F_000 536
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.3
_refine_diff_density_max 0.246
_refine_diff_density_min -0.303
_refine_ls_abs_structure_details
;
Flack x determined using 956 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.011(6)
_refine_ls_extinction_coef 0.0195(9)
_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 1.139
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 159
_refine_ls_number_reflns 2349
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.139
_refine_ls_R_factor_all 0.0217
_refine_ls_R_factor_gt 0.0217
_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^)+(0.0280P)^2^+0.3955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0567
_refine_ls_wR_factor_ref 0.0567
_reflns_number_gt 2349
_reflns_number_total 2349
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yp3225sup1.cif
_cod_data_source_block 20220428_1
_cod_original_cell_volume 1173.772(10)
_cod_database_code 2022670
_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 0.365
_shelx_estimated_absorpt_t_max 0.518
_shelx_hkl_file
;
0 0 1 12.10 0.29
0 0 1 3.73 0.17
0 0 2 4120.98 7.47
0 0 -2 4041.75 7.02
0 0 3 9.89 0.49
0 0 -3 0.48 0.22
0 0 4 1830.25 7.16
0 0 -4 1771.45 6.55
0 0 5 1.93 0.38
0 0 -5 0.44 0.29
0 0 -6 3020.33 10.48
0 0 6 2934.17 11.12
0 0 -7 8.03 0.63
0 0 -7 8.47 0.67
0 0 8 927.57 8.85
0 0 -8 933.08 6.59
0 0 -8 940.67 9.24
0 0 -9 1.64 0.75
0 0 -9 2.05 0.79
0 0 -10 741.97 9.75
0 0 10 747.06 9.27
0 0 10 707.86 8.58
0 0 -10 717.25 9.49
0 0 11 22.07 1.72
0 0 11 14.97 1.60
0 0 12 655.57 9.74
0 0 12 640.80 9.11
0 0 -12 669.83 10.39
0 0 13 4.46 1.11
0 0 -13 5.67 1.35
0 0 13 4.47 1.21
0 0 14 24.79 2.19
0 0 -14 21.05 2.10
0 0 15 0.52 0.82
0 0 15 12.10 1.64
0 0 16 51.05 2.48
0 0 16 57.22 2.94
0 0 17 1.77 0.90
0 0 -18 46.81 2.25
0 0 18 48.04 2.14
0 0 19 0.83 0.46
0 0 19 0.04 0.39
0 1 0 2.96 0.24
0 1 0 5.61 0.25
0 1 1 38.20 0.68
0 -1 -1 35.70 0.64
0 1 2 4865.20 7.84
0 -1 -2 4862.84 7.98
0 1 -3 9999.00 17.81
0 -1 -3 9166.27 12.79
0 1 4 7620.85 13.06
0 -1 -4 7595.97 13.30
0 1 5 4722.25 11.62
0 1 -5 4741.67 14.25
0 1 6 487.87 4.03
0 -1 6 500.58 5.07
0 1 7 1500.29 7.55
0 -1 7 1577.76 9.82
0 1 -7 1594.31 9.64
0 1 7 1408.97 11.86
0 -1 7 1411.03 11.68
0 1 8 3532.27 17.75
0 -1 -8 3677.44 19.18
0 1 -8 3694.38 15.52
0 1 -8 3642.34 17.04
0 1 -8 3723.44 18.27
0 -1 8 3693.53 16.06
0 1 8 3564.68 17.08
0 1 8 3372.65 19.84
0 1 8 3432.70 11.86
0 -1 8 3614.48 16.39
0 1 -8 3787.93 19.91
0 -1 8 3452.83 19.67
0 -1 9 1301.53 10.56
0 -1 -9 1393.10 12.72
0 -1 9 1189.09 12.12
0 1 9 1271.53 11.10
0 -1 -9 1342.92 11.87
0 1 -9 1367.51 9.83
0 1 9 1322.51 11.54
0 1 -9 1447.95 13.39
0 1 9 1134.71 12.09
0 1 -9 1358.93 12.08
0 -1 9 1339.97 9.91
0 -1 -10 771.10 9.80
0 1 10 755.29 9.18
0 -1 -10 784.20 10.51
0 1 10 732.07 9.35
0 1 -10 796.78 11.04
0 1 -10 760.05 10.03
0 -1 11 79.20 3.27
0 -1 -11 87.43 3.62
0 1 -11 83.94 3.65
0 -1 -11 91.28 4.01
0 1 11 84.92 3.30
0 1 11 87.33 3.49
0 1 -11 85.90 3.73
0 1 -11 84.41 4.03
0 1 -12 178.22 6.03
0 -1 12 179.39 5.10
0 1 -12 158.90 5.19
0 -1 -12 164.12 5.08
0 -1 12 158.54 4.46
0 -1 -12 176.77 5.78
0 1 -12 164.32 5.29
0 1 12 165.70 5.00
0 1 12 161.34 4.74
0 1 -13 427.80 8.71
0 -1 13 413.44 7.37
0 1 13 440.75 8.43
0 1 -13 459.59 9.81
0 -1 -13 435.29 9.19
0 1 13 420.16 7.70
0 -1 13 407.52 7.84
0 1 -14 53.83 3.35
0 -1 14 54.63 2.75
0 1 14 55.70 2.89
0 -1 -14 55.08 3.42
0 1 14 59.24 3.24
0 -1 14 59.75 3.15
0 1 -14 54.81 3.63
0 1 -15 4.68 1.66
0 1 -15 6.79 1.38
0 -1 -15 4.05 1.47
0 1 15 5.76 1.14
0 -1 15 10.01 1.31
0 -1 15 8.05 1.49
0 -1 16 510.64 8.40
0 -1 16 496.81 7.35
0 1 16 495.89 7.64
0 1 16 518.46 8.50
0 -1 17 128.59 3.34
0 -1 17 135.70 4.00
0 1 17 131.14 3.97
0 1 -18 961.46 9.25
0 1 18 971.44 9.53
0 1 18 950.55 9.17
0 -1 18 961.99 9.28
0 1 19 4.66 0.61
0 -1 19 4.94 0.65
0 -1 19 4.94 0.66
0 1 19 4.76 0.65
0 2 0 227.18 2.15
0 2 0 235.09 2.62
0 2 1 1153.18 4.65
0 -2 1 1152.67 5.31
0 2 1 1169.78 4.97
0 -2 1 1199.66 3.36
0 2 -1 1188.64 6.51
0 2 1 1173.47 3.61
0 -2 -2 9544.98 14.81
0 2 2 9584.87 14.61
0 2 -3 2636.03 11.76
0 2 3 2684.25 8.04
0 -2 4 3519.73 8.29
0 2 4 3316.34 9.30
0 -2 -4 3198.27 8.98
0 2 -4 3406.81 13.57
0 -2 -5 5074.47 12.00
0 2 5 5011.34 11.87
0 -2 6 5509.73 21.05
0 2 6 6161.68 13.65
0 2 -6 6164.26 20.12
0 -2 7 6000.24 23.16
0 2 -7 6626.01 22.33
0 2 -7 6329.31 22.25
0 2 7 6052.10 13.76
0 -2 7 6070.62 21.43
0 2 7 5968.53 21.88
0 -2 7 5695.79 20.53
0 2 -7 6251.44 22.67
0 2 7 6084.15 21.77
0 -2 8 676.97 7.13
0 -2 8 711.10 7.44
0 2 8 670.39 7.86
0 -2 -8 695.15 8.19
0 2 -8 709.20 8.31
0 2 -8 721.89 8.22
0 -2 8 612.71 8.01
0 2 -8 733.43 9.04
0 2 -8 744.19 7.98
0 2 8 583.99 8.09
0 2 8 681.78 8.04
0 2 -9 580.69 7.92
0 -2 9 544.49 6.86
0 2 9 587.43 8.00
0 -2 -9 595.72 8.50
0 2 -9 592.39 7.38
0 2 -9 560.59 8.10
0 2 -9 556.96 8.75
0 -2 9 580.61 7.12
0 2 9 556.00 7.74
0 2 -10 3.48 1.24
0 -2 -10 5.13 1.24
0 -2 10 3.52 0.80
0 2 10 3.77 1.00
0 2 -10 3.20 0.99
0 2 -11 31.45 2.36
0 2 11 32.46 2.21
0 2 11 36.26 2.42
0 2 -11 34.83 2.79
0 -2 11 27.88 1.88
0 2 12 182.17 5.36
0 -2 -12 171.56 5.56
0 2 -12 168.60 5.49
0 2 -12 173.51 6.01
0 2 -12 169.00 5.52
0 2 12 162.54 4.92
0 -2 -13 242.09 6.78
0 2 -13 251.71 6.91
0 -2 13 225.03 5.44
0 2 13 250.00 6.38
0 2 13 237.67 6.09
0 2 -13 253.68 7.46
0 2 -14 107.12 4.65
0 2 14 113.87 4.45
0 2 -14 113.73 5.07
0 -2 -14 111.53 4.64
0 2 14 117.29 4.22
0 -2 14 108.65 3.80
0 2 15 227.24 5.58
0 -2 15 209.37 5.03
0 2 15 215.41 5.85
0 2 -15 219.42 6.41
0 -2 -15 224.34 6.43
0 2 16 41.52 2.50
0 -2 16 41.04 2.12
0 2 -17 296.47 5.47
0 -2 -17 305.37 6.59
0 2 17 311.58 6.20
0 -2 17 293.28 4.77
0 2 17 302.38 5.83
0 -2 18 56.06 2.27
0 -2 -18 59.71 2.52
0 2 18 57.56 2.34
0 2 18 59.19 2.25
0 -2 19 4.12 0.59
0 -2 19 5.29 0.64
0 2 19 4.18 0.58
0 -3 0 1.29 0.35
0 3 0 0.53 0.46
0 3 1 5511.87 12.16
0 -3 -1 5296.75 13.89
0 3 1 5768.84 14.19
0 3 -1 5900.13 17.55
0 -3 -1 5572.22 5.72
0 -3 1 5359.06 13.76
0 3 2 226.37 2.20
0 -3 2 241.05 3.19
0 3 2 243.17 2.62
0 -3 2 226.33 2.03
0 3 -2 244.60 3.90
0 3 2 235.44 2.43
0 3 3 4612.06 12.75
0 -3 -3 4735.72 13.32
0 -3 3 4860.31 15.85
0 -3 3 4895.12 12.32
0 3 3 4976.51 7.98
0 -3 4 7011.30 18.16
0 -3 -4 6954.53 16.10
0 -3 5 4037.36 15.62
0 -3 -5 4539.58 12.50
0 3 5 4338.26 17.24
0 3 -5 4870.65 19.81
0 3 6 722.48 7.58
0 -3 -6 810.10 5.26
0 3 -6 871.10 8.64
0 3 6 815.59 7.98
0 -3 6 797.33 7.25
0 -3 6 780.95 7.47
0 3 -7 106.15 3.30
0 3 7 88.58 2.92
0 -3 -7 108.32 3.05
0 3 7 100.40 3.04
0 -3 7 92.10 2.86
0 -3 7 98.17 2.75
0 -3 7 98.00 2.64
0 3 7 111.56 3.18
0 3 -7 106.97 3.25
0 -3 8 43.24 2.16
0 -3 8 47.86 2.16
0 3 8 42.41 2.22
0 -3 8 44.82 2.29
0 3 -8 68.14 2.76
0 3 -8 52.87 2.38
0 3 -8 53.37 2.63
0 -3 8 50.93 2.27
0 -3 -8 62.22 2.58
0 3 8 49.19 2.33
0 -3 8 60.58 2.24
0 -3 9 627.79 8.00
0 -3 -9 646.69 8.72
0 3 9 611.34 8.50
0 3 -9 651.70 8.74
0 3 -9 554.89 8.36
0 3 9 623.28 8.68
0 -3 9 606.59 7.81
0 -3 9 588.17 7.29
0 3 -9 616.08 8.67
0 3 -9 634.30 9.67
0 3 10 5.42 1.18
0 -3 10 2.27 0.83
0 -3 -10 5.50 1.23
0 -3 10 4.73 0.90
0 3 -10 5.42 1.20
0 3 10 5.70 1.14
0 3 -10 3.99 1.36
0 -3 11 191.62 5.02
0 -3 11 199.94 4.74
0 3 -11 205.21 5.87
0 -3 -11 212.85 5.76
0 3 -11 214.28 6.40
0 3 11 214.77 5.57
0 3 11 215.43 5.73
0 -3 -12 7.92 1.60
0 3 -12 7.72 1.78
0 3 12 10.30 1.55
0 3 -12 10.15 1.76
0 3 13 524.02 9.33
0 3 -13 508.97 10.26
0 -3 -13 489.50 9.03
0 3 13 528.46 9.00
0 3 -13 504.16 9.99
0 3 -13 515.46 10.06
0 3 -14 313.65 7.94
0 3 14 348.56 7.57
0 -3 14 301.33 6.07
0 -3 -14 318.04 7.41
0 3 -14 337.15 8.50
0 3 15 461.55 9.03
0 3 15 479.78 8.47
0 3 -15 473.62 9.49
0 -3 -16 97.53 4.09
0 -3 16 90.34 2.96
0 3 16 90.68 3.52
0 3 -16 92.65 4.01
0 3 16 91.97 3.77
0 3 17 70.80 2.95
0 -3 -17 69.48 3.09
0 3 17 70.84 2.75
0 -3 -18 268.44 4.90
0 3 18 279.51 4.50
0 3 18 264.86 4.70
0 -4 0 229.50 3.52
0 4 0 243.14 3.79
0 -4 -1 900.00 6.69
0 4 -1 988.65 8.20
0 4 1 932.88 6.83
0 -4 1 985.33 6.66
0 -4 2 1389.27 8.56
0 4 -2 1258.02 3.75
0 4 -2 1493.57 10.87
0 4 2 1186.54 4.28
0 -4 -2 1341.50 4.27
0 4 2 1302.73 6.81
0 4 2 1304.02 7.03
0 -4 -2 1245.02 7.80
0 -4 2 1364.73 4.08
0 4 3 8.49 0.58
0 -4 -3 3.30 0.48
0 -4 3 8.21 0.52
0 4 -3 3.14 0.66
0 4 3 6.47 0.51
0 -4 3 6.03 0.70
0 4 3 5.28 0.43
0 4 4 3196.85 12.52
0 4 4 3320.51 10.80
0 -4 4 3022.13 11.18
0 -4 -4 2862.30 11.73
0 -4 4 3182.05 15.24
0 4 -5 2878.18 15.74
0 -4 -5 2658.82 11.26
0 4 -5 2979.92 17.35
0 -4 5 2718.50 12.43
0 4 5 2562.78 13.01
0 -4 5 2989.80 10.31
0 4 -5 2707.91 15.06
0 -4 5 2700.06 15.18
0 4 -6 349.72 6.16
0 -4 6 320.66 4.80
0 -4 -6 334.42 3.78
0 -4 6 322.29 4.65
0 4 6 338.38 5.49
0 4 6 308.64 5.07
0 4 -6 340.78 5.88
0 4 -6 312.51 4.86
0 -4 6 350.62 5.92
0 4 -6 333.52 5.55
0 -4 6 326.66 4.87
0 -4 7 23.44 1.42
0 -4 -7 27.30 1.59
0 -4 7 24.39 1.52
0 4 7 24.26 1.64
0 -4 7 25.28 1.56
0 -4 7 22.92 1.37
0 4 -7 24.85 1.73
0 4 -7 23.83 1.44
0 4 -7 25.40 1.70
0 4 -7 27.56 1.90
0 4 -7 24.18 1.74
0 4 7 24.47 1.60
0 4 -8 130.06 4.09
0 -4 8 116.15 3.44
0 -4 8 110.04 3.36
0 4 8 138.90 4.10
0 4 8 125.18 3.82
0 -4 -8 128.64 3.67
0 4 -8 123.02 3.95
0 -4 8 129.61 3.39
0 4 8 104.68 3.45
0 -4 -9 1759.98 14.45
0 -4 9 1736.63 13.99
0 4 9 1704.18 15.13
0 4 9 1678.85 14.67
0 4 -9 1758.38 15.97
0 -4 9 1642.69 12.72
0 -4 -10 14.91 1.58
0 4 10 14.47 1.64
0 -4 10 14.53 1.39
0 4 -10 12.35 1.68
0 -4 10 8.75 1.27
0 -4 11 13.70 1.44
0 4 11 14.80 1.74
0 -4 11 13.65 1.59
0 -4 -11 15.94 1.78
0 4 12 1303.99 15.85
0 -4 -12 1304.22 14.01
0 4 -12 1295.53 15.60
0 -4 12 1266.70 12.31
0 -4 12 1303.84 13.76
0 4 -12 1250.59 15.69
0 4 -13 1.53 1.38
0 4 13 1.20 1.06
0 4 -13 2.26 1.34
0 4 13 4.65 1.49
0 -4 13 3.35 1.16
0 4 -13 1.03 1.26
0 4 14 261.44 6.44
0 4 -14 254.33 7.27
0 -4 14 244.83 6.08
0 4 14 252.04 6.95
0 -4 15 370.04 6.24
0 4 -15 368.06 8.37
0 4 15 383.27 7.47
0 -4 15 370.60 7.10
0 4 15 374.85 7.89
0 -4 -16 2.14 1.12
0 -4 16 2.45 1.00
0 4 16 3.46 0.98
0 4 -16 2.38 1.16
0 4 16 3.52 1.16
0 -4 16 4.14 0.77
0 4 17 315.89 5.79
0 -4 -17 309.56 5.94
0 4 17 317.40 5.36
0 -4 17 323.81 5.64
0 4 18 79.71 2.40
0 -4 -18 78.08 2.43
0 -4 18 79.91 2.38
0 5 0 0.32 0.44
0 -5 0 0.07 0.35
0 -5 1 4533.95 15.56
0 -5 1 4486.17 18.51
0 -5 -1 4531.79 17.34
0 -5 -2 3.47 0.57
0 5 2 2.52 0.68
0 5 2 4.01 0.57
0 5 -2 3.59 0.74
0 -5 2 4.54 0.69
0 -5 2 4.67 0.66
0 -5 -3 7.18 0.71
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0 0 0 0.00 0.00
TITL 20220428_1 in P2(1)2(1)2(1)
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184 6.728150 11.246613 15.511954 90.0000 90.0000 90.0000
ZERR 5.00 0.000036 0.000058 0.000076 0.0000 0.0000 0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O
UNIT 55.00 50.00 5.00 5.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 21919
_shelx_res_file
;
TITL 20220428_1_a.res in P2(1)2(1)2(1)
20220428_1.res
created by SHELXL-2019/2 at 16:51:40 on 28-Apr-2022
REM Old TITL 20220428_1 in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.071, Rweak 0.038, Alpha 0.002, Orientation as input
REM Flack x = 0.142 ( 0.007 ) from Parsons' quotients
REM Formula found by SHELXT: C8 O5 Cl
CELL 1.54184 6.72815 11.246613 15.511954 90 90 90
ZERR 4 0.000036 0.000058 0.000076 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 O S
UNIT 40 72 20 4
DFIX 0.84 0.005 O5 H5c O5 H5e O5 H5d
L.S. 4 0 0
PLAN 1
SIZE 0.3 0.35 0.5
CONF
BOND $H
list 4
MORE -1
fmap 2 53
acta
OMIT 2 2 0
REM
REM
REM
WGHT 0.028000 0.395500
EXTI 0.019451
FVAR 1.23429
S01 4 0.730679 0.556834 0.456975 11.00000 0.00855 0.00958 =
0.01134 -0.00114 -0.00064 0.00077
O1 3 1.157438 0.385413 0.392674 11.00000 0.01116 0.01974 =
0.02389 -0.00600 -0.00214 -0.00055
O2 3 0.897228 0.523501 0.512324 11.00000 0.01088 0.01683 =
0.01377 0.00010 -0.00200 0.00090
O3 3 0.723355 0.684159 0.438498 11.00000 0.02078 0.00894 =
0.01857 -0.00118 -0.00103 0.00184
O4 3 0.543639 0.511519 0.491804 11.00000 0.00966 0.01612 =
0.01685 -0.00194 0.00154 0.00077
C1 1 0.807445 0.358547 0.351377 11.00000 0.01054 0.00964 =
0.01033 -0.00074 0.00078 -0.00025
C2 1 1.024432 0.323391 0.365819 11.00000 0.01235 0.01391 =
0.01095 -0.00029 0.00060 0.00082
C3 1 1.044245 0.195817 0.332834 11.00000 0.01606 0.01277 =
0.02055 -0.00293 0.00070 0.00297
AFIX 23
H3A 2 1.072040 0.140894 0.379517 11.00000 -1.20000
H3B 2 1.147860 0.189331 0.289609 11.00000 -1.20000
AFIX 0
C4 1 0.837479 0.173373 0.293674 11.00000 0.01733 0.01020 =
0.01702 -0.00344 0.00168 -0.00123
AFIX 13
H4 2 0.834221 0.111168 0.249455 11.00000 -1.20000
AFIX 0
C5 1 0.695986 0.152288 0.369640 11.00000 0.02000 0.01175 =
0.02238 0.00063 0.00426 -0.00334
AFIX 23
H5A 2 0.749484 0.093795 0.409306 11.00000 -1.20000
H5B 2 0.566423 0.126072 0.349869 11.00000 -1.20000
AFIX 0
C6 1 0.683840 0.277207 0.412338 11.00000 0.01419 0.01213 =
0.01611 0.00074 0.00446 -0.00147
AFIX 23
H6A 2 0.740537 0.275911 0.469824 11.00000 -1.20000
H6B 2 0.547177 0.304227 0.415927 11.00000 -1.20000
AFIX 0
C7 1 0.775973 0.298797 0.261014 11.00000 0.01510 0.01168 =
0.01196 -0.00207 -0.00050 -0.00116
C8 1 0.913067 0.348795 0.190781 11.00000 0.02604 0.01770 =
0.01190 -0.00272 0.00394 -0.00360
AFIX 137
H8A 2 1.046681 0.352807 0.212298 11.00000 -1.50000
H8B 2 0.869281 0.427038 0.174930 11.00000 -1.50000
H8C 2 0.909020 0.297823 0.141170 11.00000 -1.50000
AFIX 0
C9 1 0.561473 0.305526 0.228727 11.00000 0.02058 0.02058 =
0.02043 -0.00353 -0.00631 -0.00145
AFIX 137
H9A 2 0.534716 0.384243 0.207793 11.00000 -1.50000
H9B 2 0.472289 0.287334 0.275200 11.00000 -1.50000
H9C 2 0.542780 0.249226 0.182922 11.00000 -1.50000
AFIX 0
C10 1 0.766818 0.491318 0.353894 11.00000 0.01450 0.01078 =
0.00966 0.00057 -0.00031 0.00157
AFIX 23
H10A 2 0.649314 0.506833 0.319452 11.00000 -1.20000
H10B 2 0.877245 0.531550 0.326228 11.00000 -1.20000
AFIX 0
O5 3 1.222336 0.624341 0.472407 11.00000 0.01139 0.01156 =
0.02199 -0.00253 -0.00043 -0.00014
H5C 2 1.119337 0.585463 0.485329 11.00000 -1.20000
H5D 2 1.328953 0.586131 0.478409 11.00000 0.04674
H5E 2 1.222219 0.687985 0.500849 11.00000 0.04144
HKLF 4
REM 20220428_1_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0567, GooF = S = 1.139, Restrained GooF = 1.139 for all data
REM R1 = 0.0217 for 2349 Fo > 4sig(Fo) and 0.0217 for all 2349 data
REM 159 parameters refined using 3 restraints
END
WGHT 0.0280 0.3955
REM Highest difference peak 0.246, deepest hole -0.303, 1-sigma level 0.044
Q1 1 0.9166 0.3414 0.3618 11.00000 0.05 0.25
;
_shelx_res_checksum 78481
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 S01 0.73068(6) 0.55683(3) 0.45697(3) 0.00982(13) Uani d 1 . .
O O1 1.1574(2) 0.38541(13) 0.39267(9) 0.0183(3) Uani d 1 . .
O O2 0.89723(19) 0.52350(12) 0.51232(8) 0.0138(3) Uani d 1 . .
O O3 0.7234(2) 0.68416(11) 0.43850(8) 0.0161(3) Uani d 1 . .
O O4 0.54364(19) 0.51152(12) 0.49180(9) 0.0142(3) Uani d 1 . .
C C1 0.8074(3) 0.35855(15) 0.35138(11) 0.0102(3) Uani d 1 . .
C C2 1.0244(3) 0.32339(16) 0.36582(11) 0.0124(4) Uani d 1 . .
C C3 1.0442(3) 0.19582(17) 0.33283(13) 0.0165(4) Uani d 1 . .
H H3A 1.072040 0.140894 0.379517 0.020 Uiso calc 1 . .
H H3B 1.147860 0.189331 0.289609 0.020 Uiso calc 1 . .
C C4 0.8375(3) 0.17337(16) 0.29367(12) 0.0148(4) Uani d 1 . .
H H4 0.834221 0.111168 0.249455 0.018 Uiso calc 1 . .
C C5 0.6960(3) 0.15229(16) 0.36964(13) 0.0180(4) Uani d 1 . .
H H5A 0.749484 0.093795 0.409306 0.022 Uiso calc 1 . .
H H5B 0.566423 0.126072 0.349869 0.022 Uiso calc 1 . .
C C6 0.6838(3) 0.27721(16) 0.41234(12) 0.0141(4) Uani d 1 . .
H H6A 0.740537 0.275911 0.469824 0.017 Uiso calc 1 . .
H H6B 0.547177 0.304227 0.415927 0.017 Uiso calc 1 . .
C C7 0.7760(3) 0.29880(15) 0.26101(11) 0.0129(4) Uani d 1 . .
C C8 0.9131(3) 0.34879(18) 0.19078(12) 0.0185(4) Uani d 1 . .
H H8A 1.046681 0.352807 0.212298 0.028 Uiso calc 1 . .
H H8B 0.869281 0.427038 0.174930 0.028 Uiso calc 1 . .
H H8C 0.909020 0.297823 0.141170 0.028 Uiso calc 1 . .
C C9 0.5615(3) 0.30553(19) 0.22873(14) 0.0205(4) Uani d 1 . .
H H9A 0.534716 0.384243 0.207793 0.031 Uiso calc 1 . .
H H9B 0.472289 0.287334 0.275200 0.031 Uiso calc 1 . .
H H9C 0.542780 0.249226 0.182922 0.031 Uiso calc 1 . .
C C10 0.7668(3) 0.49132(14) 0.35389(10) 0.0116(3) Uani d 1 . .
H H10A 0.649314 0.506833 0.319452 0.014 Uiso calc 1 . .
H H10B 0.877245 0.531550 0.326228 0.014 Uiso calc 1 . .
O O5 1.22234(19) 0.62434(11) 0.47241(9) 0.0150(3) Uani d 1 . .
H H5C 1.119(2) 0.5855(19) 0.4853(16) 0.018 Uiso d 1 . .
H H5D 1.329(3) 0.586(3) 0.478(2) 0.047(9) Uiso d 1 . .
H H5E 1.222(5) 0.6880(15) 0.5008(16) 0.041(8) Uiso d 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
S01 0.0086(2) 0.0096(2) 0.0113(2) 0.00077(15) -0.00064(15) -0.00114(14)
O1 0.0112(6) 0.0197(7) 0.0239(7) -0.0005(5) -0.0021(5) -0.0060(6)
O2 0.0109(6) 0.0168(6) 0.0138(6) 0.0009(5) -0.0020(5) 0.0001(5)
O3 0.0208(7) 0.0089(6) 0.0186(6) 0.0018(5) -0.0010(5) -0.0012(5)
O4 0.0097(6) 0.0161(6) 0.0168(6) 0.0008(5) 0.0015(5) -0.0019(5)
C1 0.0105(8) 0.0096(7) 0.0103(8) -0.0002(6) 0.0008(6) -0.0007(6)
C2 0.0123(9) 0.0139(8) 0.0109(8) 0.0008(7) 0.0006(7) -0.0003(7)
C3 0.0161(10) 0.0128(9) 0.0205(9) 0.0030(8) 0.0007(7) -0.0029(7)
C4 0.0173(9) 0.0102(9) 0.0170(8) -0.0012(7) 0.0017(7) -0.0034(7)
C5 0.0200(9) 0.0117(8) 0.0224(9) -0.0033(7) 0.0043(8) 0.0006(7)
C6 0.0142(9) 0.0121(8) 0.0161(8) -0.0015(7) 0.0045(7) 0.0007(7)
C7 0.0151(9) 0.0117(8) 0.0120(8) -0.0012(7) -0.0005(7) -0.0021(6)
C8 0.0260(10) 0.0177(9) 0.0119(8) -0.0036(8) 0.0039(8) -0.0027(7)
C9 0.0206(10) 0.0206(10) 0.0204(9) -0.0014(8) -0.0063(8) -0.0035(8)
C10 0.0145(9) 0.0108(8) 0.0097(7) 0.0016(7) -0.0003(7) 0.0006(6)
O5 0.0114(6) 0.0116(6) 0.0220(7) -0.0001(5) -0.0004(6) -0.0025(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
O2 S01 O3 . . 113.12(8) ?
O2 S01 O4 . . 110.72(8) ?
O2 S01 C10 . . 108.51(8) ?
O3 S01 C10 . . 103.56(7) ?
O4 S01 O3 . . 112.66(8) ?
O4 S01 C10 . . 107.81(8) ?
C2 C1 C6 . . 105.61(14) ?
C2 C1 C7 . . 98.57(14) ?
C6 C1 C7 . . 102.65(14) ?
C10 C1 C2 . . 114.99(15) ?
C10 C1 C6 . . 117.78(14) ?
C10 C1 C7 . . 114.83(14) ?
O1 C2 C1 . . 127.46(17) ?
O1 C2 C3 . . 126.32(17) ?
C1 C2 C3 . . 106.07(15) ?
C2 C3 H3A . . 111.4 ?
C2 C3 H3B . . 111.4 ?
C2 C3 C4 . . 101.96(15) ?
H3A C3 H3B . . 109.2 ?
C4 C3 H3A . . 111.4 ?
C4 C3 H3B . . 111.4 ?
C3 C4 H4 . . 114.4 ?
C3 C4 C7 . . 102.73(15) ?
C5 C4 C3 . . 106.46(16) ?
C5 C4 H4 . . 114.4 ?
C5 C4 C7 . . 103.03(15) ?
C7 C4 H4 . . 114.4 ?
C4 C5 H5A . . 111.2 ?
C4 C5 H5B . . 111.2 ?
C4 C5 C6 . . 102.72(14) ?
H5A C5 H5B . . 109.1 ?
C6 C5 H5A . . 111.2 ?
C6 C5 H5B . . 111.2 ?
C1 C6 H6A . . 110.9 ?
C1 C6 H6B . . 110.9 ?
C5 C6 C1 . . 104.13(14) ?
C5 C6 H6A . . 110.9 ?
C5 C6 H6B . . 110.9 ?
H6A C6 H6B . . 108.9 ?
C4 C7 C1 . . 93.53(13) ?
C8 C7 C1 . . 113.35(15) ?
C8 C7 C4 . . 113.82(16) ?
C9 C7 C1 . . 113.50(15) ?
C9 C7 C4 . . 113.75(16) ?
C9 C7 C8 . . 108.46(16) ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8B . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C7 C9 H9A . . 109.5 ?
C7 C9 H9B . . 109.5 ?
C7 C9 H9C . . 109.5 ?
H9A C9 H9B . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
S01 C10 H10A . . 108.0 ?
S01 C10 H10B . . 108.0 ?
C1 C10 S01 . . 117.09(12) ?
C1 C10 H10A . . 108.0 ?
C1 C10 H10B . . 108.0 ?
H10A C10 H10B . . 107.3 ?
H5C O5 H5D . . 114(3) ?
H5C O5 H5E . . 108(3) ?
H5D O5 H5E . . 112(3) ?
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
S01 O2 . 1.4606(13) ?
S01 O3 . 1.4612(12) ?
S01 O4 . 1.4613(13) ?
S01 C10 . 1.7773(17) ?
O1 C2 . 1.209(2) ?
C1 C2 . 1.529(2) ?
C1 C6 . 1.556(2) ?
C1 C7 . 1.569(2) ?
C1 C10 . 1.519(2) ?
C2 C3 . 1.529(3) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C3 C4 . 1.539(3) ?
C4 H4 . 0.9800 ?
C4 C5 . 1.533(3) ?
C4 C7 . 1.555(2) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C5 C6 . 1.555(2) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 C8 . 1.534(3) ?
C7 C9 . 1.530(3) ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
O5 H5C . 0.844(7) ?
O5 H5D . 0.841(7) ?
O5 H5E . 0.841(7) ?
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
O1 C2 C3 C4 . . . . -170.45(18) ?
O2 S01 C10 C1 . . . . 51.98(16) ?
O3 S01 C10 C1 . . . . 172.43(14) ?
O4 S01 C10 C1 . . . . -67.99(16) ?
C1 C2 C3 C4 . . . . 5.36(18) ?
C2 C1 C6 C5 . . . . -72.10(17) ?
C2 C1 C7 C4 . . . . 56.44(15) ?
C2 C1 C7 C8 . . . . -61.42(18) ?
C2 C1 C7 C9 . . . . 174.26(16) ?
C2 C1 C10 S01 . . . . -83.86(17) ?
C2 C3 C4 C5 . . . . -76.13(18) ?
C2 C3 C4 C7 . . . . 31.79(16) ?
C3 C4 C5 C6 . . . . 69.27(18) ?
C3 C4 C7 C1 . . . . -54.99(16) ?
C3 C4 C7 C8 . . . . 62.48(18) ?
C3 C4 C7 C9 . . . . -172.61(15) ?
C4 C5 C6 C1 . . . . 4.32(19) ?
C5 C4 C7 C1 . . . . 55.52(16) ?
C5 C4 C7 C8 . . . . 172.99(16) ?
C5 C4 C7 C9 . . . . -62.10(18) ?
C6 C1 C2 O1 . . . . -118.24(19) ?
C6 C1 C2 C3 . . . . 66.02(17) ?
C6 C1 C7 C4 . . . . -51.79(16) ?
C6 C1 C7 C8 . . . . -169.65(16) ?
C6 C1 C7 C9 . . . . 66.04(18) ?
C6 C1 C10 S01 . . . . 41.7(2) ?
C7 C1 C2 O1 . . . . 135.98(19) ?
C7 C1 C2 C3 . . . . -39.77(16) ?
C7 C1 C6 C5 . . . . 30.68(18) ?
C7 C1 C10 S01 . . . . 162.77(13) ?
C7 C4 C5 C6 . . . . -38.44(18) ?
C10 C1 C2 O1 . . . . 13.4(3) ?
C10 C1 C2 C3 . . . . -162.36(14) ?
C10 C1 C6 C5 . . . . 157.89(16) ?
C10 C1 C7 C4 . . . . 179.15(15) ?
C10 C1 C7 C8 . . . . 61.3(2) ?
C10 C1 C7 C9 . . . . -63.0(2) ?
_cod_database_fobs_code 2022670