#------------------------------------------------------------------------------
#$Date: 2024-12-18 04:06:38 +0100 (Wed, 18 Dec 2024) $
#$Revision: 296911 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023335.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_2023335
loop_
_publ_author_name
'Kinshakova, Ekaterina'
'Torambetov, Batirbay'
'Kaur, Simranjeet'
'Ashurov, Jamshid'
'Kadirova, Shakhnoza'
_publ_section_title
;
Synthesis, crystal structure, Hirshfeld surface analysis and DFT
calculations of the coordination compound
tetraaquabis{2-[(5-methyl-1,3,4-thiadiazol-2-yl)sulfanyl]acetato-\kO}cobalt(II)
;
_journal_coeditor_code WM5739
_journal_issue 1
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024011939
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac '[Co (C5 H5 N2 O2 S2)2 (H2 O1)4]'
_chemical_formula_moiety 'C10 H18 Co N4 O8 S4'
_chemical_formula_sum 'C10 H18 Co N4 O8 S4'
_chemical_formula_weight 509.45
_chemical_name_systematic
Tetraaquabis{2-[(5-methyl-1,3,4-thiadiazol-2-yl)sulfanyl]acetato-\kO}cobalt(II)
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 91.892(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.1950(2)
_cell_length_b 10.0347(3)
_cell_length_c 18.9090(6)
_cell_measurement_reflns_used 2568
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 74.8470
_cell_measurement_theta_min 4.3700
_cell_volume 985.19(6)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Ruby'
_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 0.0546
_diffrn_reflns_av_unetI/netI 0.0509
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 6554
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.077
_diffrn_reflns_theta_min 4.680
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 11.229
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.80823
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour pink
_exptl_crystal_density_diffrn 1.717
_exptl_crystal_description block
_exptl_crystal_F_000 522
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.337
_refine_diff_density_min -0.267
_refine_ls_extinction_coef 0.0100(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 137
_refine_ls_number_reflns 2023
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all 0.0450
_refine_ls_R_factor_gt 0.0376
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.2531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0911
_refine_ls_wR_factor_ref 0.0984
_reflns_number_gt 1770
_reflns_number_total 2023
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5739.cif
_cod_data_source_block I
_cod_database_code 2023335
_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 0 -2 10.56 2.55
0 0 -3 3.40 2.35
0 0 -4 64.15 8.01
0 0 -5 0.20 3.71
0 0 6 78.89 13.05
0 0 -6 80.36 11.14
0 0 -7 0.81 3.26
0 0 7 6.11 5.91
0 0 -8 22.98 7.09
0 0 8 29.85 9.32
0 0 9 4.10 5.62
0 0 -9 1.35 4.46
0 0 10 1000.14 57.63
0 0 -10 1090.04 52.20
0 0 11 4.21 9.25
0 0 -11 5.65 5.37
0 0 -12 547.66 40.78
0 0 12 522.33 46.57
0 0 -13 -9.48 7.39
0 0 13 9.39 10.27
0 0 -14 26.95 8.87
0 0 14 32.76 9.63
0 0 14 36.34 15.58
0 0 -15 3.82 4.68
0 0 15 -2.47 7.77
0 0 -16 511.66 36.89
0 0 16 516.42 53.97
0 0 -17 6.10 6.65
0 0 -18 184.92 22.91
0 0 19 -4.99 6.74
0 0 -19 -2.40 6.64
0 0 20 63.69 13.31
0 0 21 5.11 6.00
0 0 22 300.39 22.13
0 0 23 4.71 3.95
0 1 0 25.06 3.17
0 -1 0 24.45 3.56
0 -1 0 17.77 2.51
0 -1 -1 997.11 22.92
0 -1 1 951.21 22.59
0 -1 -1 975.34 22.95
0 -1 -2 0.78 1.27
0 -1 -2 1.40 1.64
0 1 -2 1.47 1.33
0 1 -3 3748.09 41.30
0 -1 -3 3385.03 57.49
0 1 -4 42.78 5.67
0 -1 -4 54.38 8.37
0 -1 -5 131.38 14.35
0 1 -5 148.41 12.00
0 -1 5 134.63 13.88
0 1 -6 34.45 6.49
0 1 6 30.85 8.14
0 -1 -6 45.46 9.84
0 -1 6 26.21 6.70
0 -1 -7 2478.99 69.90
0 -1 7 2429.80 70.80
0 1 -7 2556.75 59.71
0 1 7 2344.38 73.85
0 1 -8 1761.33 54.35
0 -1 -8 1697.76 61.66
0 -1 8 1712.19 64.83
0 1 8 1775.43 68.51
0 -1 -9 38.10 11.00
0 -1 9 32.55 10.41
0 1 -9 51.05 10.95
0 1 9 67.05 16.46
0 -1 -10 105.32 17.54
0 1 -10 126.79 17.08
0 1 10 115.80 20.56
0 -1 10 80.45 17.15
0 -1 11 8.61 7.13
0 -1 -11 36.10 11.01
0 1 -11 22.89 9.36
0 1 11 26.16 11.89
0 -1 -12 368.53 35.40
0 1 12 415.77 41.99
0 -1 12 356.44 37.86
0 -1 -13 1140.44 64.61
0 -1 13 1053.35 67.96
0 1 13 1021.67 69.21
0 -1 -14 36.66 14.46
0 -1 14 35.24 10.52
0 -1 14 28.82 12.37
0 1 14 34.26 12.50
0 1 -14 26.46 10.42
0 -1 -14 35.44 10.30
0 1 -15 155.77 20.41
0 -1 15 130.22 19.01
0 1 15 171.63 30.53
0 -1 -15 171.03 21.45
0 -1 -15 190.12 28.21
0 -1 15 136.09 27.90
0 -1 -16 514.01 37.25
0 1 -16 513.60 37.07
0 -1 16 472.45 35.10
0 1 16 572.72 56.85
0 -1 16 587.54 57.25
0 1 -17 35.41 11.11
0 -1 -17 32.49 11.05
0 -1 -18 215.41 24.31
0 1 -18 250.35 26.33
0 -1 18 278.14 24.99
0 -1 19 514.13 32.31
0 1 19 410.87 32.26
0 -1 -19 441.77 33.38
0 1 -19 423.54 33.04
0 -1 19 449.04 32.67
0 1 20 35.28 9.40
0 -1 20 35.73 9.92
0 -1 21 24.73 8.99
0 1 21 20.93 8.72
0 1 22 3.32 4.25
0 -1 22 -1.12 4.36
0 1 23 184.24 14.79
0 -1 23 187.14 14.15
0 2 0 3603.92 52.01
0 -2 0 3798.60 60.55
0 -2 -1 2939.26 54.81
0 2 -1 3046.80 44.45
0 -2 -1 2906.38 48.96
0 2 1 2962.72 37.25
0 -2 -2 448.08 21.74
0 -2 -2 460.98 22.73
0 -2 2 489.14 12.28
0 2 -2 475.80 17.86
0 -2 2 437.66 22.09
0 2 2 491.27 19.80
0 2 -3 421.09 18.44
0 -2 -3 418.25 23.12
0 -2 -3 372.05 21.45
0 -2 3 411.12 16.25
0 2 3 388.87 20.96
0 2 -4 171.43 13.23
0 -2 -4 188.73 17.00
0 -2 4 191.83 13.64
0 2 4 188.76 16.37
0 -2 -5 392.77 26.52
0 2 5 383.44 26.17
0 2 -5 396.37 17.27
0 -2 5 389.06 22.64
0 -2 6 617.85 32.03
0 -2 -6 596.18 34.68
0 2 -6 648.93 24.88
0 2 6 650.88 37.21
0 -2 -7 262.48 24.60
0 2 7 298.43 27.54
0 2 -7 315.38 19.08
0 -2 7 305.02 24.38
0 -2 8 975.88 47.50
0 -2 -8 920.59 48.32
0 2 8 971.52 52.31
0 2 -8 1022.00 37.64
0 2 9 1240.60 63.04
0 -2 -9 1259.14 59.52
0 2 -9 1419.74 48.00
0 -2 9 1328.63 59.68
0 -2 -10 3577.58 105.55
0 2 10 3526.84 112.13
0 -2 10 3774.15 107.44
0 2 11 5.51 9.06
0 -2 11 29.78 10.94
0 -2 -11 21.44 9.60
0 -2 12 262.66 31.66
0 -2 -12 246.93 30.07
0 2 12 232.41 32.15
0 -2 -13 122.52 22.02
0 2 13 131.48 26.94
0 -2 13 136.10 24.52
0 -2 14 180.56 29.13
0 2 14 160.90 29.32
0 -2 14 150.58 19.16
0 -2 -14 150.81 26.04
0 2 -14 187.28 22.19
0 -2 -14 172.60 21.15
0 2 15 119.32 27.35
0 2 -15 112.20 17.71
0 -2 -15 69.70 18.26
0 -2 -15 101.19 16.90
0 -2 15 78.73 14.12
0 -2 15 130.12 26.52
0 -2 16 540.43 37.82
0 2 -16 614.14 40.53
0 -2 -16 627.63 40.51
0 -2 -17 -14.82 7.88
0 -2 17 -0.19 6.44
0 2 -17 -3.13 8.15
0 -2 18 18.45 8.13
0 -2 -18 36.11 11.22
0 2 -18 18.74 8.91
0 2 18 37.78 11.67
0 -2 18 35.55 10.27
0 -2 19 1.20 6.49
0 -2 19 -3.37 7.16
0 2 19 10.30 5.74
0 2 20 369.38 28.33
0 -2 20 336.61 25.96
0 -2 20 371.14 26.40
0 2 21 64.77 11.78
0 -2 21 68.68 11.10
0 -2 21 50.51 9.99
0 2 22 93.41 11.92
0 -2 22 99.33 11.68
0 2 23 14.43 5.52
0 -3 0 14.22 5.23
0 3 0 3.81 2.95
0 3 1 307.94 19.83
0 -3 -1 337.67 19.96
0 -3 1 301.54 21.50
0 -3 -1 350.81 23.29
0 3 1 344.39 12.56
0 3 -1 314.96 17.87
0 3 -2 221.57 14.69
0 -3 -2 223.21 18.89
0 3 2 210.61 13.28
0 -3 -2 234.05 17.94
0 -3 2 235.34 19.74
0 3 -3 517.27 23.35
0 -3 3 487.84 12.67
0 -3 -3 497.66 28.26
0 -3 -3 491.60 28.90
0 3 3 509.20 24.77
0 -3 3 509.89 29.78
0 -3 -4 1896.34 58.97
0 -3 -4 1803.93 57.35
0 -3 4 1904.55 36.31
0 3 4 1743.31 51.80
0 3 -4 1857.27 47.01
0 -3 4 1837.29 60.10
0 3 -5 59.83 6.28
0 3 -5 57.17 9.18
0 -3 5 63.11 12.81
0 -3 -5 55.59 11.11
0 -3 5 49.02 7.27
0 3 5 59.99 10.40
0 3 -6 79.73 7.72
0 3 6 88.16 14.77
0 -3 -6 67.94 13.18
0 -3 6 67.74 10.59
0 3 7 76.25 14.58
0 -3 7 50.49 9.67
0 -3 -7 81.58 15.02
0 3 8 26.18 10.05
0 -3 -8 27.47 10.20
0 -3 8 26.99 8.40
0 -3 9 2494.17 78.76
0 -3 -9 2333.97 86.18
0 3 9 2310.79 88.18
0 3 10 4.21 8.86
0 -3 10 19.71 8.49
0 -3 -10 1.10 7.67
0 3 11 77.51 18.39
0 -3 11 119.54 20.58
0 -3 -11 92.20 19.88
0 -3 -12 53.68 15.26
0 -3 12 61.93 15.54
0 3 13 1914.01 96.74
0 -3 13 1971.11 67.42
0 -3 -13 1914.41 91.31
0 -3 14 63.62 12.93
0 -3 -14 79.41 14.14
0 3 -14 66.27 13.20
0 3 14 87.53 22.19
0 -3 -14 76.19 20.43
0 -3 -15 34.35 9.01
0 3 15 55.03 20.24
0 -3 15 40.22 11.04
0 3 -15 36.08 10.49
0 -3 -15 33.02 13.29
0 -3 -16 93.26 16.02
0 3 -16 98.23 16.11
0 -3 16 73.74 13.95
0 -3 -17 706.23 42.13
0 3 17 602.11 39.23
0 -3 17 573.09 39.22
0 -3 17 714.24 40.66
0 3 -17 646.92 41.43
0 -3 18 10.86 7.53
0 -3 18 8.43 8.19
0 3 18 -1.63 6.52
0 -3 19 19.68 8.82
0 3 19 27.45 9.20
0 -3 19 29.34 9.07
0 -3 20 113.19 15.25
0 3 20 104.84 15.17
0 -3 20 118.77 14.76
0 -3 21 156.61 15.81
0 3 21 142.10 15.92
0 3 22 65.09 9.47
0 -3 22 50.24 7.14
0 -4 0 65.56 12.10
0 4 0 62.72 10.27
0 -4 -1 2523.40 72.98
0 4 1 2372.88 63.51
0 -4 1 2391.52 70.48
0 4 2 391.09 17.51
0 4 -2 378.98 22.09
0 -4 2 380.23 28.92
0 -4 -2 382.63 28.95
0 4 2 328.21 25.11
0 -4 -3 21.54 7.60
0 -4 -3 19.48 7.04
0 4 -3 10.74 2.74
0 4 3 13.91 4.57
0 -4 3 22.68 8.84
0 -4 -4 431.33 30.81
0 -4 -4 427.31 32.02
0 -4 4 448.37 33.71
0 4 -4 465.56 25.67
0 4 4 458.91 26.82
0 -4 -5 910.06 47.64
0 4 -5 958.89 39.21
0 4 5 961.77 43.16
0 -4 5 889.62 49.62
0 4 6 634.92 38.32
0 -4 -6 686.54 43.35
0 -4 6 665.17 45.12
0 4 7 6.92 5.99
0 -4 7 6.18 7.17
0 -4 -7 1.46 8.07
0 4 8 190.98 24.80
0 -4 -8 223.26 27.20
0 -4 8 205.73 27.90
0 4 9 201.93 26.30
0 -4 9 168.92 26.20
0 -4 -9 179.35 25.14
0 -4 10 1938.97 91.89
0 -4 -10 2068.99 89.27
0 4 10 2158.06 92.35
0 -4 11 9.51 7.65
0 4 11 5.01 7.31
0 -4 -11 -3.68 5.98
0 -4 -12 47.14 14.70
0 -4 12 57.00 18.38
0 -4 12 54.12 12.45
0 4 12 85.40 21.85
0 -4 13 53.21 11.96
0 -4 -13 14.22 10.79
0 -4 13 68.60 21.08
0 4 13 73.27 22.52
0 -4 13 66.07 12.62
0 -4 -14 68.83 20.23
0 -4 14 92.63 24.76
0 -4 14 64.11 13.13
0 -4 14 71.85 14.65
0 4 14 103.58 23.96
0 -4 -15 35.13 11.23
0 -4 15 19.25 8.55
0 4 -15 33.91 10.25
0 -4 15 29.76 7.56
0 4 16 290.38 26.73
0 -4 16 245.79 25.67
0 -4 -16 283.71 25.70
0 -4 -17 13.13 6.67
0 4 17 19.54 8.29
0 -4 17 10.49 8.19
0 4 18 -2.65 6.60
0 -4 -18 2.84 4.76
0 -4 18 13.64 10.23
0 4 19 1.97 6.61
0 -4 19 0.40 5.43
0 -4 20 209.88 19.57
0 4 20 212.83 19.03
0 4 21 2.62 4.45
0 -4 21 3.20 4.52
0 4 22 -3.76 3.00
0 -4 22 5.58 3.40
0 -4 -22 -1.98 2.67
0 5 0 2.81 3.45
0 -5 0 -1.97 5.82
0 -5 -1 861.00 48.12
0 5 -1 908.02 39.88
0 -5 1 797.47 46.94
0 5 1 872.08 43.03
0 -5 -2 737.47 45.37
0 -5 2 708.56 45.10
0 5 2 711.71 40.59
0 5 -2 801.32 36.29
0 5 -3 1836.58 55.00
0 -5 -3 1730.52 69.58
0 -5 3 1556.34 67.56
0 5 3 1566.18 63.20
0 5 4 873.77 49.22
0 -5 4 885.62 53.25
0 5 -4 1000.92 41.45
0 -5 -4 950.98 52.99
0 -5 5 35.21 12.12
0 -5 -5 29.07 11.40
0 5 5 41.40 11.57
0 -5 6 560.62 45.89
0 -5 -6 537.72 41.50
0 -5 -7 449.31 39.43
0 -5 7 390.99 39.97
0 5 7 449.56 35.82
0 -5 8 630.35 52.35
0 5 8 724.37 48.74
0 -5 -8 588.70 47.01
0 5 9 52.02 13.76
0 -5 -9 53.10 15.37
0 -5 9 28.57 12.63
0 -5 -10 3.62 7.02
0 5 10 -2.34 5.74
0 -5 10 8.41 12.00
0 5 11 1818.87 90.88
0 -5 -11 1548.05 84.21
0 -5 -11 1670.89 59.76
0 -5 11 1598.58 60.45
0 -5 -11 1633.62 60.90
0 -5 12 83.69 14.76
0 -5 -12 66.24 13.03
0 5 12 94.95 22.10
0 -5 -12 78.55 13.39
0 -5 12 30.92 11.84
0 -5 12 99.12 15.58
0 -5 13 441.37 33.23
0 -5 -13 478.62 32.43
0 -5 13 488.15 34.62
0 -5 13 464.13 52.37
0 5 13 501.79 51.29
0 -5 -13 478.51 33.96
0 -5 14 80.22 15.15
0 -5 14 76.27 14.43
0 -5 -14 78.71 14.43
0 5 15 26.22 9.05
0 -5 -15 18.35 8.36
0 -5 15 20.68 9.63
0 -5 15 26.73 9.21
0 -5 -16 26.79 9.64
0 5 16 23.26 9.20
0 -5 16 11.76 7.92
0 -5 16 27.15 10.50
0 -5 17 90.61 15.60
0 -5 -17 88.36 13.82
0 5 17 108.86 16.03
0 -5 -18 217.20 18.86
0 -5 18 198.90 21.71
0 5 18 220.07 20.91
0 -5 18 173.80 20.07
0 5 19 57.83 10.53
0 -5 19 42.69 10.56
0 -5 -20 304.90 21.35
0 5 20 298.49 18.83
0 -5 20 291.83 21.36
0 -5 -21 8.58 4.23
0 -5 21 6.43 3.71
0 -6 0 2702.83 96.42
0 -6 -1 220.71 27.42
0 -6 1 204.07 26.94
0 6 1 208.17 22.76
0 -6 2 7.44 6.64
0 -6 -2 20.10 10.46
0 6 2 20.68 7.89
0 -6 3 58.95 15.75
0 -6 -3 54.09 13.94
0 6 3 41.38 10.43
0 -6 -4 758.28 52.66
0 6 4 621.00 45.43
0 -6 4 670.91 51.05
0 6 5 193.43 26.43
0 -6 5 229.28 30.37
0 -6 -5 221.39 29.06
0 6 6 45.48 13.57
0 -6 6 35.79 14.29
0 -6 7 111.70 23.93
0 6 7 117.14 20.97
0 6 8 1398.38 80.86
0 -6 -8 1635.92 60.23
0 -6 8 1448.42 86.49
0 6 9 825.78 64.32
0 -6 -9 904.62 45.29
0 -6 9 819.72 66.76
0 -6 9 919.24 44.45
0 -6 -9 971.92 47.13
0 -6 -10 235.37 23.57
0 6 10 226.68 35.21
0 -6 10 196.59 34.33
0 -6 -10 201.71 22.16
0 -6 10 210.83 22.52
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-6 3 -3 88.13 10.51
-6 -3 -4 10.01 4.71
-6 -3 -4 20.22 5.27
-6 3 -4 24.75 5.71
-6 -3 -5 30.78 6.87
-6 -3 -6 15.02 4.65
-6 -4 1 -5.15 3.17
-6 -4 0 54.74 8.17
-6 -4 -1 5.02 2.72
-6 -4 -2 6.42 2.97
-6 -4 -3 11.78 4.28
-6 -4 -4 57.25 7.87
-6 -4 -5 -0.61 2.22
0 0 0 0.00 0.00
TITL exp_399_CoNO3_4A_Bo in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 5.195003 10.034654 18.908977 90.0000 91.8924 90.0000
ZERR 4.00 0.000181 0.000304 0.000625 0.0000 0.0031 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 44.00 40.00 4.00 4.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 29067
_shelx_res_file
;
TITL exp_399_cono3_4a_bo_a.res in P2(1)/c
exp_399_cono3_4a_bo.res
created by SHELXL-2016/6 at 14:55:27 on 28-Nov-2024
REM Old TITL exp_399_cono3_4a_bo_a.res in Pc
REM SHELXT solution in P2(1)/c: R1 0.201, Rweak 0.018, Alpha 0.032
REM 0.693 for 127 systematic absences, Orientation as input
REM Formula found by SHELXT: C18 N1 O6 Co
CELL 1.54184 5.195 10.0347 18.909 90 91.892 90
ZERR 2 0.0002 0.0003 0.0006 0 0.003 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Co N O S
UNIT 20 36 2 8 16 8
EQIV $1 +X,1.5-Y,0.5+Z
EQIV $2 2-X,1-Y,1-Z
DFIX 0.88 O3 H3b
L.S. 4 0 0
PLAN 1
HTAB O4 N2_$1
HTAB C4 S1
HTAB O4 O1_$2
HTAB O3 O2
HTAB O3 N1_$1
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
OMIT -3 10 9
OMIT -1 11 11
REM
REM
REM
WGHT 0.042300 0.253100
EXTI 0.009968
FVAR 0.72483
CO1 3 0.500000 0.500000 0.500000 10.50000 0.02185 0.02329 =
0.02218 -0.00019 -0.00071 0.00377
S2 6 0.934443 0.672626 0.234363 11.00000 0.04053 0.03681 =
0.03161 0.00568 0.00253 -0.00942
S1 6 0.516297 0.465823 0.192318 11.00000 0.04297 0.03232 =
0.03009 0.00962 -0.00319 -0.00586
O1 5 0.729844 0.497065 0.411515 11.00000 0.02981 0.03480 =
0.02593 0.00371 0.00382 0.00629
O3 5 0.311960 0.684475 0.473159 11.00000 0.03740 0.02771 =
0.03041 -0.00011 -0.00129 0.00731
O2 5 0.547041 0.662823 0.348429 11.00000 0.03924 0.04256 =
0.03260 0.00598 0.00318 0.01563
AFIX 6
O4 5 0.784895 0.599442 0.554445 11.00000 0.02482 0.04178 =
0.05340 -0.02174 -0.01205 0.00744
H4A 2 0.754101 0.661162 0.583781 11.00000 -1.50000
H4B 2 0.939850 0.576984 0.564102 11.00000 -1.50000
AFIX 0
N2 4 0.614719 0.675496 0.123055 11.00000 0.05097 0.04270 =
0.03750 0.01558 -0.00775 -0.00747
N1 4 0.421111 0.611546 0.084613 11.00000 0.05712 0.04725 =
0.03479 0.01230 -0.00766 -0.00387
C5 1 0.713501 0.577031 0.359501 11.00000 0.02634 0.02750 =
0.02422 -0.00123 -0.00076 -0.00111
C4 1 0.934687 0.559804 0.308431 11.00000 0.02985 0.03503 =
0.02757 0.00222 0.00183 0.00438
AFIX 23
H4C 2 0.929270 0.469381 0.290307 11.00000 -1.20000
H4D 2 1.096227 0.570265 0.335059 11.00000 -1.20000
AFIX 0
C2 1 0.682107 0.612618 0.180582 11.00000 0.03733 0.03015 =
0.02703 0.00621 0.00358 0.00156
C1 1 0.350115 0.501129 0.113521 11.00000 0.04223 0.03474 =
0.02814 0.00469 0.00102 0.00557
C3 1 0.140073 0.414774 0.083946 11.00000 0.04842 0.04635 =
0.04366 0.00154 -0.01151 -0.00027
AFIX 137
H3C 2 0.208492 0.355386 0.049477 11.00000 -1.50000
H3D 2 0.008604 0.469362 0.061893 11.00000 -1.50000
H3E 2 0.067607 0.363860 0.121388 11.00000 -1.50000
AFIX 0
H3A 2 0.311246 0.749901 0.500540 11.00000 0.06104
H3B 2 0.383444 0.707106 0.434071 11.00000 0.06977
HKLF 4
REM exp_399_cono3_4a_bo_a.res in P2(1)/c
REM R1 = 0.0376 for 1770 Fo > 4sig(Fo) and 0.0450 for all 2023 data
REM 137 parameters refined using 1 restraints
END
WGHT 0.0423 0.2531
REM Highest difference peak 0.337, deepest hole -0.267, 1-sigma level 0.072
Q1 1 0.8067 0.6145 0.1982 11.00000 0.05 0.34
;
_shelx_res_checksum 84186
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Co Co1 0.500000 0.500000 0.500000 0.0225(2) Uani d 1 . .
S S2 0.93444(16) 0.67263(8) 0.23436(4) 0.0363(2) Uani d 1 . .
S S1 0.51630(16) 0.46582(8) 0.19232(4) 0.0352(2) Uani d 1 . .
O O1 0.7298(4) 0.4971(2) 0.41151(11) 0.0301(5) Uani d 1 . .
O O3 0.3120(5) 0.6845(2) 0.47316(12) 0.0319(5) Uani d 1 . .
O O2 0.5470(5) 0.6628(2) 0.34843(12) 0.0381(5) Uani d 1 . .
O O4 0.7849(4) 0.5994(2) 0.55445(14) 0.0403(6) Uani d 1 . .
H H4A 0.754101 0.661162 0.583781 0.060 Uiso d 1 . .
H H4B 0.939850 0.576984 0.564102 0.060 Uiso d 1 . .
N N2 0.6147(6) 0.6755(3) 0.12306(16) 0.0439(7) Uani d 1 . .
N N1 0.4211(7) 0.6115(3) 0.08461(16) 0.0466(7) Uani d 1 . .
C C5 0.7135(6) 0.5770(3) 0.35950(15) 0.0261(6) Uani d 1 . .
C C4 0.9347(6) 0.5598(3) 0.30843(16) 0.0308(6) Uani d 1 . .
H H4C 0.929270 0.469381 0.290307 0.037 Uiso calc 1 . .
H H4D 1.096227 0.570265 0.335059 0.037 Uiso calc 1 . .
C C2 0.6821(6) 0.6126(3) 0.18058(16) 0.0314(6) Uani d 1 . .
C C1 0.3501(7) 0.5011(3) 0.11352(17) 0.0350(7) Uani d 1 . .
C C3 0.1401(8) 0.4148(4) 0.0839(2) 0.0464(8) Uani d 1 . .
H H3C 0.208492 0.355386 0.049477 0.070 Uiso calc 1 . .
H H3D 0.008604 0.469362 0.061893 0.070 Uiso calc 1 . .
H H3E 0.067607 0.363860 0.121388 0.070 Uiso calc 1 . .
H H3A 0.311(9) 0.750(5) 0.501(2) 0.061(14) Uiso d 1 . .
H H3B 0.383(9) 0.707(5) 0.4341(17) 0.070(15) 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
Co1 0.0219(3) 0.0233(3) 0.0222(3) 0.0038(2) -0.0007(2) -0.0002(2)
S2 0.0405(5) 0.0368(4) 0.0316(4) -0.0094(3) 0.0025(3) 0.0057(3)
S1 0.0430(5) 0.0323(4) 0.0301(4) -0.0059(3) -0.0032(3) 0.0096(3)
O1 0.0298(11) 0.0348(11) 0.0259(10) 0.0063(8) 0.0038(8) 0.0037(8)
O3 0.0374(13) 0.0277(10) 0.0304(11) 0.0073(9) -0.0013(9) -0.0001(8)
O2 0.0392(13) 0.0426(12) 0.0326(11) 0.0156(10) 0.0032(10) 0.0060(9)
O4 0.0248(11) 0.0418(13) 0.0534(15) 0.0074(9) -0.0121(10) -0.0217(10)
N2 0.0510(18) 0.0427(16) 0.0375(15) -0.0075(13) -0.0077(13) 0.0156(12)
N1 0.0571(19) 0.0473(17) 0.0348(15) -0.0039(14) -0.0077(14) 0.0123(13)
C5 0.0263(14) 0.0275(13) 0.0242(13) -0.0011(11) -0.0008(11) -0.0012(10)
C4 0.0299(15) 0.0350(15) 0.0276(14) 0.0044(12) 0.0018(11) 0.0022(11)
C2 0.0373(17) 0.0302(14) 0.0270(14) 0.0016(12) 0.0036(12) 0.0062(11)
C1 0.0422(19) 0.0347(16) 0.0281(15) 0.0056(13) 0.0010(13) 0.0047(11)
C3 0.048(2) 0.0464(19) 0.0437(19) -0.0003(16) -0.0115(16) 0.0015(15)
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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
O1 Co1 O1 3_666 . 180.0 ?
O1 Co1 O3 . . 95.20(8) ?
O1 Co1 O3 3_666 3_666 95.20(8) ?
O1 Co1 O3 . 3_666 84.80(8) ?
O1 Co1 O3 3_666 . 84.80(8) ?
O3 Co1 O3 . 3_666 180.0 ?
O4 Co1 O1 . 3_666 90.76(10) ?
O4 Co1 O1 3_666 . 90.76(10) ?
O4 Co1 O1 3_666 3_666 89.24(10) ?
O4 Co1 O1 . . 89.24(10) ?
O4 Co1 O3 . . 90.83(9) ?
O4 Co1 O3 . 3_666 89.17(9) ?
O4 Co1 O3 3_666 . 89.17(9) ?
O4 Co1 O3 3_666 3_666 90.83(9) ?
O4 Co1 O4 . 3_666 180.00(11) ?
C2 S2 C4 . . 102.60(15) ?
C2 S1 C1 . . 87.22(15) ?
C5 O1 Co1 . . 125.90(19) ?
Co1 O3 H3A . . 123(3) ?
Co1 O3 H3B . . 103(3) ?
H3A O3 H3B . . 109(4) ?
Co1 O4 H4A . . 122.5 ?
Co1 O4 H4B . . 130.3 ?
H4A O4 H4B . . 104.5 ?
C2 N2 N1 . . 112.8(3) ?
C1 N1 N2 . . 112.9(3) ?
O1 C5 C4 . . 112.6(2) ?
O2 C5 O1 . . 127.0(3) ?
O2 C5 C4 . . 120.5(3) ?
S2 C4 H4C . . 108.3 ?
S2 C4 H4D . . 108.3 ?
C5 C4 S2 . . 115.9(2) ?
C5 C4 H4C . . 108.3 ?
C5 C4 H4D . . 108.3 ?
H4C C4 H4D . . 107.4 ?
S1 C2 S2 . . 126.18(18) ?
N2 C2 S2 . . 120.0(2) ?
N2 C2 S1 . . 113.7(3) ?
N1 C1 S1 . . 113.4(3) ?
N1 C1 C3 . . 123.7(3) ?
C3 C1 S1 . . 122.8(2) ?
C1 C3 H3C . . 109.5 ?
C1 C3 H3D . . 109.5 ?
C1 C3 H3E . . 109.5 ?
H3C C3 H3D . . 109.5 ?
H3C C3 H3E . . 109.5 ?
H3D C3 H3E . . 109.5 ?
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
Co1 O1 3_666 2.088(2) ?
Co1 O1 . 2.088(2) y
Co1 O3 . 2.146(2) y
Co1 O3 3_666 2.146(2) ?
Co1 O4 . 2.036(2) y
Co1 O4 3_666 2.036(2) ?
S2 C4 . 1.801(3) ?
S2 C2 . 1.740(3) ?
S1 C2 . 1.724(3) ?
S1 C1 . 1.734(3) ?
O1 C5 . 1.270(3) ?
O3 H3A . 0.84(5) ?
O3 H3B . 0.868(19) ?
O2 C5 . 1.233(4) ?
O4 H4A . 0.8501 ?
O4 H4B . 0.8500 ?
N2 N1 . 1.380(4) ?
N2 C2 . 1.296(4) ?
N1 C1 . 1.295(4) ?
C5 C4 . 1.535(4) ?
C4 H4C . 0.9700 ?
C4 H4D . 0.9700 ?
C1 C3 . 1.488(5) ?
C3 H3C . 0.9600 ?
C3 H3D . 0.9600 ?
C3 H3E . 0.9600 ?
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
O3 H3B O2 . 0.868(19) 1.91(3) 2.700(3) 151(5)
C4 H4C S1 . 0.97 2.79 3.181(3) 105.0
O4 H4A N2 4_576 0.85 1.95 2.764(4) 160.3
O4 H4B O1 3_766 0.85 1.91 2.757(3) 172.2
O3 H3A N1 4_576 0.84(5) 2.17(5) 2.979(4) 162(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
Co1 O1 C5 O2 . . . . -6.9(4) ?
Co1 O1 C5 C4 . . . . 171.97(18) ?
O1 C5 C4 S2 . . . . -178.0(2) ?
O2 C5 C4 S2 . . . . 0.9(4) ?
N2 N1 C1 S1 . . . . 0.4(4) ?
N2 N1 C1 C3 . . . . 178.3(3) ?
N1 N2 C2 S2 . . . . 176.8(2) ?
N1 N2 C2 S1 . . . . 1.1(4) ?
C4 S2 C2 S1 . . . . -8.8(3) ?
C4 S2 C2 N2 . . . . 176.0(3) ?
C2 S2 C4 C5 . . . . -73.2(2) ?
C2 S1 C1 N1 . . . . 0.1(3) ?
C2 S1 C1 C3 . . . . -177.7(3) ?
C2 N2 N1 C1 . . . . -1.0(5) ?
C1 S1 C2 S2 . . . . -176.1(2) ?
C1 S1 C2 N2 . . . . -0.7(3) ?