#------------------------------------------------------------------------------
#$Date: 2019-08-29 07:13:12 +0300 (Thu, 29 Aug 2019) $
#$Revision: 217821 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021758.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_2021758
loop_
_publ_author_name
'Meundaeng, Natthaya'
'Prior, Timothy John'
'Rujiwatra, Apinpus'
_publ_section_title
;
Crystal structures and Hirshfeld surface analysis of transition-metal
complexes of 1,3-azolecarboxylic acids
;
_journal_coeditor_code FN3320
_journal_issue 9
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229619011525
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac '[Co (C4 H2 N O3)2 (H2 O)2]'
_chemical_formula_moiety 'C8 H8 Co N2 O8'
_chemical_formula_sum 'C8 H8 Co N2 O8'
_chemical_formula_weight 319.09
_chemical_name_systematic
;
Diaquabis(1,3-oxazole-4-carboxylato-\k^2^N,O^4^)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'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 99.378(10)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.1664(7)
_cell_length_b 10.9879(15)
_cell_length_c 9.7550(11)
_cell_measurement_reflns_used 2467
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 29.4
_cell_measurement_theta_min 2.8
_cell_volume 546.37(12)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2016)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2016)
;
_computing_data_reduction
;
SORTAV (Blessing, 1987, 1989)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Stoe IPDS2'
_diffrn_measurement_method \w-scans
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0244
_diffrn_reflns_av_unetI/netI 0.0416
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 2995
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.161
_diffrn_reflns_theta_min 2.813
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 1.613
_exptl_absorpt_correction_T_max 0.948
_exptl_absorpt_correction_T_min 0.942
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour pink
_exptl_crystal_density_diffrn 1.940
_exptl_crystal_description rod
_exptl_crystal_F_000 322
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.110
_exptl_crystal_size_min 0.110
_refine_diff_density_max 0.371
_refine_diff_density_min -0.278
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.908
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 98
_refine_ls_number_reflns 1458
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.908
_refine_ls_R_factor_all 0.0401
_refine_ls_R_factor_gt 0.0247
_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^)+(0.0281P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0502
_refine_ls_wR_factor_ref 0.0522
_reflns_number_gt 1104
_reflns_number_total 1458
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file fn3320sup1.cif
_cod_data_source_block Co-4oxa
_cod_database_code 2021758
_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 0.739
_shelx_estimated_absorpt_t_max 0.843
_shelx_hkl_file
;
-7 -2 2 73.11 17.12
-7 -1 1 251.94 14.56
-7 -1 2 -24.29 18.37
-7 -1 3 170.51 17.24
-7 0 1 7.33 16.03
-7 0 2 317.94 14.71
-7 0 3 -13.39 18.10
-7 0 4 83.24 17.09
-7 1 1 243.29 19.17
-7 1 2 0.15 12.83
-7 1 3 160.99 18.23
-7 2 2 74.88 16.74
-6 -7 1 242.90 18.20
6 7 -1 211.67 17.08
-6 -7 2 -0.98 17.76
6 7 -2 -3.97 15.71
-6 -7 3 54.81 18.18
6 7 -3 66.48 17.60
6 7 -4 -10.14 18.31
-6 -7 4 19.95 13.86
-6 -7 5 117.18 18.93
6 7 -5 103.33 18.76
6 6 -1 9.89 11.73
-6 -6 1 -5.60 16.42
6 6 -2 240.47 15.83
-6 -6 2 255.26 17.54
6 6 -3 15.20 12.26
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6 6 -4 173.89 15.99
-6 -6 4 184.67 18.01
-6 -6 5 9.38 12.87
6 6 -5 10.29 12.49
-6 -6 6 132.04 14.19
6 6 -6 141.81 16.87
-6 -5 1 71.01 16.33
6 5 -1 63.18 15.77
6 5 -2 34.50 11.42
-6 -5 2 26.34 15.69
-6 -5 3 139.14 11.80
6 5 -3 165.52 15.76
6 5 -4 19.81 16.15
-6 -5 4 27.46 16.58
-6 -5 5 147.49 17.47
6 5 -5 144.43 16.82
6 5 -6 18.77 12.51
-6 -5 6 4.48 17.49
6 5 -7 32.00 18.60
-6 -5 7 23.34 17.13
-6 -4 1 98.29 15.96
6 4 -1 71.93 14.70
6 4 -2 24.79 13.46
-6 -4 2 21.60 14.18
-6 -4 3 3.48 14.71
6 4 -3 9.58 14.75
6 4 -4 195.88 15.55
-6 -4 4 201.72 12.49
6 4 -5 7.42 15.64
-6 -4 5 15.25 11.66
6 4 -6 93.94 14.94
-6 -4 6 116.52 12.85
6 4 -7 2.64 17.27
-6 -4 7 -0.77 18.34
-6 -3 1 143.36 15.22
-6 -3 2 132.10 11.55
6 3 -2 132.76 11.29
6 3 -3 274.37 15.14
-6 -3 3 251.09 16.00
-6 -3 4 28.16 14.41
6 3 -4 10.50 15.18
6 3 -5 301.04 15.84
-6 -3 5 285.18 16.17
6 3 -6 0.80 11.23
-6 -3 6 -4.92 15.82
6 3 -7 143.44 17.72
-6 -3 7 138.42 12.89
-6 -3 8 3.21 17.60
6 3 -8 13.95 18.75
-6 -2 1 59.79 14.65
-6 -2 2 445.03 12.41
-6 -2 3 -10.98 13.26
6 2 -4 426.65 15.13
-6 -2 4 442.31 16.34
-6 -2 5 47.77 13.90
6 2 -5 48.24 10.85
6 2 -6 404.84 15.82
-6 -2 6 392.33 13.45
6 2 -7 26.07 12.26
-6 -2 7 22.92 16.01
6 2 -8 -1.41 12.60
-6 -2 8 12.98 18.10
-6 -1 1 33.36 13.00
-6 -1 2 18.91 12.97
-6 -1 3 282.37 12.11
-6 -1 4 21.37 10.72
-6 -1 5 477.01 15.44
-6 -1 6 42.88 14.70
-6 -1 7 33.28 16.17
-6 -1 8 3.05 18.16
-6 0 1 1.00 10.16
-6 0 2 38.96 14.13
-6 0 3 1.99 13.98
-6 0 4 648.34 16.99
-6 0 5 3.80 13.71
-6 0 6 3.30 15.65
-6 0 7 6.73 15.58
-6 0 8 42.87 18.13
-6 1 0 75.69 10.80
-6 1 1 29.34 14.08
-6 1 2 5.41 10.23
-6 1 3 284.53 11.49
-6 1 4 31.31 10.77
-6 1 5 497.02 17.22
-6 1 6 36.73 11.69
-6 1 7 45.90 12.72
-6 1 8 6.50 17.56
-6 2 0 99.64 13.07
-6 2 1 43.50 10.36
-6 2 2 435.55 15.78
-6 2 3 12.80 14.33
-6 2 4 450.50 16.37
-6 2 5 34.38 11.17
-6 2 6 407.76 16.29
-6 2 7 16.36 15.60
-6 2 8 -0.38 18.51
-6 3 0 103.00 14.82
-6 3 1 144.50 13.98
-6 3 2 119.92 13.18
-6 3 3 265.07 11.95
-6 3 4 28.21 14.68
-6 3 5 301.88 15.42
-6 3 6 -2.30 15.70
-6 3 7 175.36 16.28
-6 3 8 17.45 19.20
-6 4 0 419.30 17.83
-6 4 1 73.02 14.74
-6 4 2 18.45 13.57
-6 4 3 1.06 10.57
-6 4 4 182.72 14.72
-6 4 5 8.76 14.42
-6 4 6 125.84 17.02
-6 4 7 -1.84 16.09
-6 5 0 -6.37 15.44
-6 5 1 63.89 14.51
-6 5 2 31.99 13.92
-6 5 3 170.18 11.96
-6 5 4 15.76 15.29
-6 5 5 147.90 15.29
-6 5 6 32.64 17.24
-6 5 7 21.88 13.37
-6 6 0 102.29 12.46
-6 6 1 11.12 11.69
-6 6 2 244.89 16.36
-6 6 3 15.58 16.26
-6 6 4 206.83 17.12
-6 6 5 6.20 12.89
-6 6 6 155.17 14.46
-6 7 0 4.33 16.77
-6 7 1 199.10 17.07
-6 7 2 -2.26 12.76
-6 7 3 56.87 12.93
-6 7 4 17.09 13.15
-6 7 5 116.43 18.23
-5 -10 1 22.38 18.07
5 10 -1 -2.50 17.50
-5 -10 2 115.15 13.63
5 10 -2 126.69 16.15
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5 10 -3 29.28 17.20
5 10 -4 219.61 19.35
-5 -10 4 224.75 18.37
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-5 -9 1 316.70 18.23
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5 9 -2 1.47 16.04
5 9 -3 205.99 15.97
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-5 -9 4 6.09 16.76
5 9 -4 -2.44 12.22
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5 9 -5 140.16 17.59
5 9 -6 18.38 13.84
-5 -9 6 7.16 17.06
-5 -8 1 9.15 13.84
5 8 -1 3.86 14.96
-5 -8 2 892.50 18.22
5 8 -2 879.26 18.66
-5 -8 3 19.97 15.12
5 8 -3 29.45 14.29
-5 -8 4 259.29 12.93
5 8 -4 257.56 12.84
-5 -8 5 3.60 16.51
5 8 -5 7.78 16.10
5 8 -6 72.37 15.65
-5 -8 6 106.27 17.73
5 8 -7 24.19 17.80
-5 -8 7 23.97 18.06
-5 -7 1 150.61 11.11
5 7 -1 162.92 14.39
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5 7 -2 34.85 10.54
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5 7 -3 320.38 15.41
5 7 -4 15.12 14.78
-5 -7 4 18.14 10.73
5 7 -5 13.51 15.54
-5 -7 5 19.62 11.60
5 7 -6 18.26 11.93
-5 -7 6 13.03 11.73
-5 -7 7 190.46 13.32
5 7 -7 173.97 17.16
-5 -7 8 76.28 19.01
5 7 -8 96.61 18.42
5 6 -1 26.23 13.56
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5 6 -2 318.82 15.07
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5 6 -3 -2.05 10.38
5 6 -4 400.27 12.07
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5 6 -5 21.71 10.93
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5 6 -6 85.72 15.10
-5 -6 6 75.07 14.58
-5 -6 7 47.73 15.81
5 6 -7 51.16 11.55
5 6 -8 52.61 13.03
-5 -6 8 62.09 16.55
5 6 -9 34.47 18.88
-5 -6 9 41.05 17.33
-5 -5 1 409.40 14.80
5 5 -1 398.43 13.55
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5 5 -2 157.88 13.31
5 5 -3 345.91 11.33
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5 5 -4 188.74 14.09
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5 5 -7 118.72 11.31
-5 -5 8 15.03 12.39
5 5 -8 7.26 15.22
-5 -5 9 244.27 16.90
5 5 -9 252.22 13.79
5 4 -1 -0.91 12.73
-5 -4 1 3.00 9.28
-5 -4 2 176.01 13.38
5 4 -2 185.91 13.33
-5 -4 3 38.68 13.15
5 4 -3 40.58 9.47
-5 -4 4 2.23 13.05
5 4 -4 -1.02 11.98
5 4 -5 15.94 9.58
-5 -4 5 15.70 13.34
5 4 -6 55.23 13.03
-5 -4 6 47.71 10.41
-5 -4 7 7.72 13.60
5 4 -7 7.03 10.24
-5 -4 8 223.75 16.15
5 4 -8 221.91 12.54
-5 -4 9 12.64 15.72
5 4 -9 15.51 15.80
5 4 -10 138.59 18.84
-5 -4 10 133.85 14.78
5 3 -1 455.55 11.48
-5 -3 1 442.77 14.25
5 3 -2 54.29 9.48
-5 -3 2 49.97 9.18
5 3 -3 1294.63 23.32
-5 -3 3 1309.10 17.35
-5 -3 4 11.88 12.83
5 3 -4 5.73 12.14
5 3 -5 218.01 13.06
-5 -3 5 232.90 13.26
-5 -3 6 0.01 13.48
5 3 -6 -4.14 13.16
-5 -3 7 402.77 15.84
5 3 -7 415.15 16.65
-5 -3 8 74.18 15.78
5 3 -8 76.79 14.24
5 3 -9 451.28 18.96
-5 -3 9 482.34 19.31
-5 -3 10 180.53 17.95
5 3 -10 179.22 17.10
-5 -2 1 413.50 11.26
5 2 -1 408.72 14.19
5 2 -2 752.11 15.34
-5 -2 2 729.94 14.08
5 2 -3 2.78 8.98
-5 -2 3 2.49 9.11
5 2 -4 1095.22 21.31
-5 -2 4 1101.06 17.66
5 2 -5 50.49 9.40
-5 -2 5 48.33 9.53
-5 -2 6 442.77 14.73
5 2 -6 459.94 15.50
-5 -2 7 94.68 13.32
5 2 -7 107.00 11.03
-5 -2 8 625.00 14.77
5 2 -8 670.54 16.10
5 2 -9 15.38 16.56
-5 -2 9 -4.82 16.60
5 2 -10 93.13 13.47
-5 -2 10 102.58 18.53
-5 -1 1 99.02 11.72
-5 -1 2 85.13 11.55
-5 -1 3 111.86 12.03
5 1 -3 118.61 9.76
5 1 -4 198.33 9.87
-5 -1 4 220.05 10.14
-5 -1 5 222.03 10.26
5 1 -5 232.30 10.27
-5 -1 6 31.72 9.90
5 1 -6 38.54 13.12
5 1 -7 245.02 11.05
-5 -1 7 246.97 14.29
-5 -1 8 -2.72 14.99
5 1 -8 8.38 13.25
5 1 -9 83.09 15.42
-5 -1 9 82.50 16.32
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5 1 -10 15.80 17.24
-5 0 1 2.15 11.61
-5 0 2 180.34 12.49
-5 0 3 -2.95 12.11
-5 0 4 85.87 9.24
-5 0 5 4.12 9.04
5 0 -6 258.82 13.36
-5 0 6 248.41 10.94
-5 0 7 -4.64 13.78
5 0 -7 -13.13 13.62
-5 0 8 69.31 14.97
5 0 -8 94.11 14.94
-5 0 9 -4.83 16.23
-5 0 10 167.70 16.72
-5 1 0 28.02 10.84
-5 1 1 83.56 11.93
-5 1 2 75.75 11.49
-5 1 3 90.37 12.12
-5 1 4 205.68 9.50
-5 1 5 210.89 10.04
-5 1 6 36.40 13.33
-5 1 7 254.92 11.33
-5 1 8 6.02 10.51
-5 1 9 81.97 16.13
-5 1 10 8.57 16.71
-5 2 0 201.96 9.66
-5 2 1 414.45 13.91
-5 2 2 744.66 18.79
-5 2 3 12.48 11.86
-5 2 4 1082.44 20.46
-5 2 5 50.67 13.01
-5 2 6 453.51 15.43
-5 2 7 95.34 14.02
-5 2 8 666.39 17.90
-5 2 9 17.15 15.10
-5 2 10 92.46 19.09
-5 3 0 43.80 8.82
-5 3 1 434.86 14.93
-5 3 2 45.96 11.81
-5 3 3 1245.06 25.20
-5 3 4 -6.18 12.14
-5 3 5 203.69 13.68
-5 3 6 -0.68 9.43
-5 3 7 412.79 12.90
-5 3 8 81.19 15.37
-5 3 9 464.14 17.67
-5 3 10 166.68 19.27
-5 4 0 134.18 11.88
-5 4 1 4.89 11.30
-5 4 2 181.24 9.75
-5 4 3 30.61 12.11
-5 4 4 1.61 9.18
-5 4 5 32.65 9.88
-5 4 6 41.06 13.75
-5 4 7 12.03 14.17
-5 4 8 210.22 15.71
-5 4 9 8.47 16.48
-5 4 10 134.59 18.61
-5 5 0 21.09 11.93
-5 5 1 416.23 11.57
-5 5 2 137.99 9.67
-5 5 3 331.79 11.05
-5 5 4 188.77 12.88
-5 5 5 340.31 14.40
-5 5 6 15.00 13.89
-5 5 7 108.37 15.20
-5 5 8 2.59 15.31
-5 5 9 291.70 19.25
-5 6 0 112.06 12.85
-5 6 1 33.56 9.38
-5 6 2 318.26 10.75
-5 6 3 6.73 9.67
-5 6 4 397.93 15.13
-5 6 5 3.94 13.95
-5 6 6 89.23 13.78
-5 6 7 44.24 15.74
-5 6 8 77.74 18.35
-5 6 9 33.73 18.61
-5 7 0 129.01 10.75
-5 7 1 139.81 13.34
-5 7 2 12.73 12.21
-5 7 3 291.87 14.90
-5 7 4 12.10 13.11
-5 7 5 27.28 13.68
-5 7 6 16.05 15.29
-5 7 7 194.06 17.34
-5 7 8 99.60 18.08
-5 8 0 218.54 13.57
-5 8 1 19.67 10.55
-5 8 2 797.34 20.69
-5 8 3 11.38 13.67
-5 8 4 258.34 16.11
-5 8 5 5.44 14.44
-5 8 6 95.20 16.83
-5 8 7 20.09 16.46
-5 9 0 74.21 14.00
-5 9 1 269.52 12.39
-5 9 2 -6.93 15.52
-5 9 3 210.50 16.45
-5 9 4 4.41 12.25
-5 9 5 171.63 16.30
-5 9 6 -5.04 17.82
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-5 10 2 101.49 15.48
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-4 -12 1 31.95 17.03
4 12 -1 31.74 13.37
4 12 -2 43.71 18.27
-4 -12 2 51.10 17.15
4 12 -3 84.04 18.30
-4 -12 3 102.58 13.39
-4 -12 4 13.75 14.17
4 11 -1 386.88 17.63
-4 -11 1 403.81 17.51
4 11 -2 65.84 14.91
-4 -11 2 57.55 16.03
4 11 -3 133.10 17.01
-4 -11 3 157.90 17.94
4 11 -4 20.07 16.81
-4 -11 4 5.70 16.78
-4 -11 5 164.76 16.35
4 11 -5 145.46 12.84
-4 -11 6 213.36 18.68
4 11 -6 160.30 18.86
4 10 -1 -2.52 10.99
-4 -10 1 1.14 13.55
4 10 -2 64.18 13.78
-4 -10 2 80.67 14.95
-4 -10 3 69.28 15.89
4 10 -3 57.54 11.57
4 10 -4 337.06 13.00
-4 -10 4 350.21 13.79
-4 -10 5 36.94 16.90
4 10 -5 33.57 15.66
-4 -10 6 165.46 13.21
4 10 -6 136.00 13.13
-4 -10 7 17.37 18.17
4 10 -7 -10.59 15.86
-4 -9 1 8.94 13.88
4 9 -1 -1.88 13.72
4 9 -2 56.19 10.09
-4 -9 2 85.22 14.00
4 9 -3 316.67 15.31
-4 -9 3 323.74 11.91
4 9 -4 79.91 14.83
-4 -9 4 75.32 13.94
4 9 -5 228.85 11.77
-4 -9 5 223.23 11.97
4 9 -6 39.96 15.53
-4 -9 6 20.40 15.81
-4 -9 7 145.14 16.62
4 9 -7 137.75 16.84
-4 -9 8 36.01 17.62
4 9 -8 47.89 17.51
4 8 -1 2.60 12.09
-4 -8 1 5.56 12.57
4 8 -2 822.63 14.25
-4 -8 2 836.78 18.61
-4 -8 3 80.83 9.75
4 8 -3 90.34 13.34
4 8 -4 792.53 18.81
-4 -8 4 809.45 19.97
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-6 -3 -2 32.42 11.74
-6 -3 -3 89.26 17.56
-6 -3 -4 -1.30 18.28
-6 -4 0 444.38 16.90
-6 -4 -1 -9.02 15.52
-6 -4 -2 257.70 13.68
-6 -4 -3 -2.48 15.75
-6 -4 -4 108.90 17.29
-6 -5 0 2.73 16.01
6 5 0 -0.62 15.43
-6 -5 -1 202.89 16.13
-6 -5 -2 -9.60 16.06
-6 -5 -3 54.56 13.61
-6 -6 0 96.56 17.52
6 6 0 90.90 14.83
-6 -6 -1 -5.17 13.25
6 6 1 8.32 12.38
-6 -6 -2 184.17 18.68
-6 -7 0 13.57 18.37
6 7 0 5.52 17.09
-6 -7 -1 219.30 14.50
6 7 1 175.69 17.55
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 21527
_shelx_res_file
;
TITL shelxt_a.res in P2(1)/c
shelx.res
created by SHELXL-2018/3 at 13:44:10 on 01-Aug-2019
CELL 0.71073 5.1664 10.9879 9.7550 90.000 99.378 90.000
ZERR 2.00 0.0007 0.0015 0.0011 0.000 0.010 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H CO N O
UNIT 16 16 2 4 16
MERG 2
MORE -1
EQIV $1 x-1, -y+3/2, z+1/2
HTAB C1 O2_$1
EQIV $2 -x+1, y+1/2, -z+1/2
HTAB C2 O3_$2
EQIV $3 -x+1, y-1/2, -z+1/2
HTAB O3 O2_$3
EQIV $4 x-1, y, z
HTAB O3 O1_$4
HTAB C1 O2_$1
HTAB C2 O3_$2
HTAB O3 O2_$3
HTAB O3 O1_$4
FMAP 2
PLAN 20
SIZE 0.110 0.110 0.200
ACTA
BOND $H
CONF
LIST 6
L.S. 4
TEMP -123.00
WGHT 0.028100
FVAR 0.89183
CO1 3 0.500000 0.500000 0.500000 10.50000 0.01175 0.01075 =
0.01405 0.00083 0.00491 -0.00006
O4 5 0.266259 0.881574 0.482134 11.00000 0.02679 0.01588 =
0.02387 -0.00003 0.01237 0.00422
O1 5 0.737342 0.568022 0.363089 11.00000 0.01442 0.01269 =
0.01989 0.00086 0.00700 0.00095
O3 5 0.208296 0.469008 0.329521 11.00000 0.01386 0.01635 =
0.02129 -0.00443 0.00276 0.00194
O2 5 0.839516 0.734586 0.251894 11.00000 0.02006 0.01781 =
0.02068 0.00509 0.01113 0.00112
N1 4 0.386789 0.688231 0.494040 11.00000 0.01375 0.01464 =
0.01292 0.00020 0.00430 -0.00089
C3 1 0.520713 0.749310 0.400198 11.00000 0.01467 0.01523 =
0.01312 0.00079 0.00441 -0.00107
C4 1 0.713633 0.680664 0.331751 11.00000 0.01147 0.01538 =
0.01331 -0.00091 0.00192 0.00012
C1 1 0.242008 0.770437 0.537877 11.00000 0.01741 0.01703 =
0.01662 -0.00035 0.00461 0.00010
AFIX 44
H1 2 0.131676 0.754753 0.601635 11.00000 -1.20000
AFIX 0
C2 1 0.445140 0.866035 0.393483 11.00000 0.02412 0.01615 =
0.02092 0.00206 0.01133 0.00048
AFIX 44
H2 2 0.498594 0.921109 0.343048 11.00000 -1.20000
AFIX 0
H3A 2 0.194480 0.398437 0.302624 11.00000 0.03120
H3B 2 0.075902 0.497335 0.334340 11.00000 0.04518
HKLF 4
REM shelxt_a.res in P2(1)/c
REM wR2 = 0.0522, GooF = S = 0.908, Restrained GooF = 0.908 for all data
REM R1 = 0.0247 for 1104 Fo > 4sig(Fo) and 0.0401 for all 1458 data
REM 98 parameters refined using 0 restraints
END
WGHT 0.0281 0.0000
REM Highest difference peak 0.371, deepest hole -0.278, 1-sigma level 0.066
Q1 1 0.6112 0.7169 0.3599 11.00000 0.05 0.37
Q2 1 0.3857 0.7915 0.3723 11.00000 0.05 0.28
Q3 1 0.4207 0.4320 0.4729 11.00000 0.05 0.27
Q4 1 0.5592 0.8136 0.4145 11.00000 0.05 0.26
Q5 1 0.1203 0.7999 0.6080 11.00000 0.05 0.25
Q6 1 0.4424 0.6415 0.5385 11.00000 0.05 0.25
Q7 1 0.4267 0.7046 0.4260 11.00000 0.05 0.25
Q8 1 0.3340 0.6439 0.4673 11.00000 0.05 0.23
Q9 1 0.3843 0.4881 0.5818 11.00000 0.05 0.23
Q10 1 0.3595 0.5735 0.5012 11.00000 0.05 0.23
Q11 1 0.7207 0.6115 0.3386 11.00000 0.05 0.22
Q12 1 0.5389 0.9525 0.3933 11.00000 0.05 0.22
Q13 1 0.6806 0.5460 0.4138 11.00000 0.05 0.21
Q14 1 0.1583 0.9260 0.4672 11.00000 0.05 0.21
Q15 1 0.7226 0.8023 0.1955 11.00000 0.05 0.21
Q16 1 0.3424 0.7173 0.5370 11.00000 0.05 0.20
Q17 1 0.4011 0.9547 0.3221 11.00000 0.05 0.20
Q18 1 0.3510 0.8742 0.4351 11.00000 0.05 0.19
Q19 1 0.8319 0.7887 0.2426 11.00000 0.05 0.19
Q20 1 0.8067 0.5555 0.4062 11.00000 0.05 0.19
;
_shelx_res_checksum 48017
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
Co Co1 0.500000 0.500000 0.500000 0.01187(9) Uani d 1
O O4 0.2663(2) 0.88157(11) 0.48213(14) 0.0213(3) Uani d 1
O O1 0.7373(2) 0.56802(10) 0.36309(13) 0.0152(2) Uani d 1
O O3 0.2083(2) 0.46901(12) 0.32952(14) 0.0172(3) Uani d 1
O O2 0.8395(2) 0.73459(11) 0.25189(14) 0.0186(3) Uani d 1
N N1 0.3868(3) 0.68823(13) 0.49404(15) 0.0135(3) Uani d 1
C C3 0.5207(3) 0.74931(15) 0.40020(18) 0.0141(3) Uani d 1
C C4 0.7136(3) 0.68066(14) 0.33175(17) 0.0134(3) Uani d 1
C C1 0.2420(3) 0.77044(15) 0.53788(19) 0.0168(3) Uani d 1
H H1 0.132(2) 0.7548(4) 0.6016(14) 0.020 Uiso calc 1
C C2 0.4451(3) 0.86603(16) 0.3935(2) 0.0195(4) Uani d 1
H H2 0.4986(14) 0.9211(15) 0.3430(13) 0.023 Uiso calc 1
H H3A 0.194(4) 0.398(3) 0.303(3) 0.031(6) Uiso d 1
H H3B 0.076(5) 0.497(3) 0.334(3) 0.045(7) 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 0.01175(13) 0.01075(13) 0.01405(16) -0.00006(13) 0.00491(10) 0.00083(16)
O4 0.0268(6) 0.0159(6) 0.0239(8) 0.0042(5) 0.0124(5) 0.0000(5)
O1 0.0144(5) 0.0127(5) 0.0199(7) 0.0010(4) 0.0070(5) 0.0009(5)
O3 0.0139(5) 0.0164(7) 0.0213(7) 0.0019(4) 0.0028(5) -0.0044(5)
O2 0.0201(5) 0.0178(6) 0.0207(7) 0.0011(4) 0.0111(5) 0.0051(5)
N1 0.0138(6) 0.0146(7) 0.0129(8) -0.0009(5) 0.0043(5) 0.0002(5)
C3 0.0147(7) 0.0152(7) 0.0131(9) -0.0011(5) 0.0044(6) 0.0008(6)
C4 0.0115(7) 0.0154(7) 0.0133(9) 0.0001(5) 0.0019(6) -0.0009(6)
C1 0.0174(7) 0.0170(8) 0.0166(9) 0.0001(6) 0.0046(7) -0.0004(7)
C2 0.0241(8) 0.0162(8) 0.0209(10) 0.0005(6) 0.0113(7) 0.0021(7)
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'
Co Co 0.3494 0.9721 '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'
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
O3 Co1 O3 3_666 . 180.0
O3 Co1 O1 3_666 3_666 88.38(5)
O3 Co1 O1 . 3_666 91.62(5)
O3 Co1 O1 3_666 . 91.62(5)
O3 Co1 O1 . . 88.38(5)
O1 Co1 O1 3_666 . 180.00(4)
O3 Co1 N1 3_666 . 91.30(5)
O3 Co1 N1 . . 88.71(5)
O1 Co1 N1 3_666 . 100.13(4)
O1 Co1 N1 . . 79.87(4)
O3 Co1 N1 3_666 3_666 88.70(5)
O3 Co1 N1 . 3_666 91.29(5)
O1 Co1 N1 3_666 3_666 79.87(5)
O1 Co1 N1 . 3_666 100.13(4)
N1 Co1 N1 . 3_666 180.0
C1 O4 C2 . . 104.88(13)
C4 O1 Co1 . . 117.13(9)
Co1 O3 H3A . . 115.2(18)
Co1 O3 H3B . . 115(2)
H3A O3 H3B . . 112(3)
C1 N1 C3 . . 104.80(14)
C1 N1 Co1 . . 146.70(11)
C3 N1 Co1 . . 108.47(10)
C2 C3 N1 . . 108.59(14)
C2 C3 C4 . . 132.31(15)
N1 C3 C4 . . 119.08(14)
O2 C4 O1 . . 124.94(13)
O2 C4 C3 . . 119.69(14)
O1 C4 C3 . . 115.36(13)
N1 C1 O4 . . 113.76(14)
N1 C1 H1 . . 123.1
O4 C1 H1 . . 123.1
C3 C2 O4 . . 107.97(15)
C3 C2 H2 . . 126.0
O4 C2 H2 . . 126.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O3 3_666 2.0823(14)
Co1 O3 . 2.0823(14)
Co1 O1 3_666 2.0928(11)
Co1 O1 . 2.0928(11)
Co1 N1 . 2.1476(14)
Co1 N1 3_666 2.1476(14)
O4 C1 . 1.351(2)
O4 C2 . 1.3753(19)
O1 C4 . 1.2760(19)
O3 H3A . 0.82(3)
O3 H3B . 0.76(3)
O2 C4 . 1.2434(19)
N1 C1 . 1.289(2)
N1 C3 . 1.405(2)
C3 C2 . 1.339(2)
C3 C4 . 1.492(2)
C1 H1 . 0.93(2)
C2 H2 . 0.85(2)
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
_geom_hbond_publ_flag
C1 H1 O2 4_476 0.93 2.27 3.1781(19) 166.0 yes
C2 H2 O3 2_655 0.85 2.50 3.238(2) 145.8 yes
O3 H3A O2 2_645 0.82(3) 1.88(3) 2.6949(18) 178(2) yes
O3 H3B O1 1_455 0.76(3) 1.98(3) 2.7333(16) 175(3) yes
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
C1 N1 C3 C2 -0.3(2)
Co1 N1 C3 C2 178.36(13)
C1 N1 C3 C4 178.41(16)
Co1 N1 C3 C4 -2.98(17)
Co1 O1 C4 O2 -179.81(13)
Co1 O1 C4 C3 1.07(18)
C2 C3 C4 O2 0.6(3)
N1 C3 C4 O2 -177.72(16)
C2 C3 C4 O1 179.7(2)
N1 C3 C4 O1 1.4(2)
C3 N1 C1 O4 0.0(2)
Co1 N1 C1 O4 -177.65(16)
C2 O4 C1 N1 0.3(2)
N1 C3 C2 O4 0.4(2)
C4 C3 C2 O4 -177.97(17)
C1 O4 C2 C3 -0.5(2)
_cod_database_fobs_code 2021758