#------------------------------------------------------------------------------
#$Date: 2019-08-29 07:13:12 +0300 (Thu, 29 Aug 2019) $
#$Revision: 217821 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021757.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_2021757
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 N2 O2)2 (H2 O)2]'
_chemical_formula_moiety 'C8 H10 Co N4 O6'
_chemical_formula_sum 'C8 H10 Co N4 O6'
_chemical_formula_weight 317.13
_chemical_name_systematic
Diaquabis(1H-imidazole-2-carboxylato-\k^2^N^3^,O)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 97.858(10)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.1145(7)
_cell_length_b 10.6123(12)
_cell_length_c 10.4179(13)
_cell_measurement_reflns_used 2611
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 29.45
_cell_measurement_theta_min 2.75
_cell_volume 560.14(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
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_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 0.0266
_diffrn_reflns_av_unetI/netI 0.0511
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 3303
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.173
_diffrn_reflns_theta_min 2.753
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 1.564
_exptl_absorpt_correction_T_max 0.948
_exptl_absorpt_correction_T_min 0.944
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour 'pale orange'
_exptl_crystal_density_diffrn 1.880
_exptl_crystal_description block
_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 0.323
_refine_diff_density_min -0.280
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.835
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 99
_refine_ls_number_reflns 1495
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.835
_refine_ls_R_factor_all 0.0403
_refine_ls_R_factor_gt 0.0234
_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^)+(0.0227P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0459
_refine_ls_wR_factor_ref 0.0478
_reflns_number_gt 1078
_reflns_number_total 1495
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file fn3320sup1.cif
_cod_data_source_block Co-2Hima
_cod_database_code 2021757
_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 0.745
_shelx_estimated_absorpt_t_max 0.847
_shelx_hkl_file
;
7 0 -2 136.42 15.96
7 0 -3 5.90 19.51
6 7 -1 83.36 15.55
6 7 -2 -10.72 19.78
6 7 -3 98.27 20.63
6 7 -4 7.34 18.93
6 6 -1 2.86 14.62
6 6 -2 124.33 18.73
6 6 -3 5.75 18.00
6 6 -4 119.82 18.94
6 6 -5 -10.89 18.64
6 5 -1 142.78 19.05
6 5 -2 14.73 13.75
6 5 -3 146.20 14.33
6 5 -4 15.77 17.52
6 5 -5 116.09 18.42
6 5 -6 -0.75 20.20
6 5 -7 193.09 21.60
6 4 -1 64.78 16.13
6 4 -2 38.15 12.65
6 4 -3 68.37 13.01
6 4 -4 52.38 13.50
6 4 -5 2.82 16.42
6 4 -6 127.72 20.22
6 4 -7 9.49 19.17
6 3 -1 119.11 17.00
6 3 -2 93.14 15.68
6 3 -3 316.96 17.45
6 3 -4 4.40 17.55
6 3 -5 221.53 14.24
6 3 -6 17.49 14.40
6 3 -7 116.95 18.25
6 3 -8 15.05 19.17
6 2 -1 61.30 11.99
6 2 -2 329.60 15.31
6 2 -3 24.26 12.41
6 2 -4 510.15 20.34
6 2 -5 22.92 16.12
6 2 -6 400.21 19.54
6 2 -7 15.15 19.05
6 2 -8 27.14 18.90
6 1 -1 18.14 11.16
6 1 -2 15.83 12.08
6 1 -3 144.06 16.30
6 1 -4 5.09 15.19
6 1 -5 335.31 17.88
6 1 -6 4.92 16.56
6 1 -7 8.23 18.89
6 1 -8 -5.40 20.31
6 0 -1 -5.29 16.87
6 0 -2 20.48 16.89
6 0 -3 -4.32 11.95
6 0 -4 399.52 17.47
6 0 -5 -6.90 16.00
6 0 -6 -1.73 16.78
6 0 -7 0.54 14.54
6 0 -8 63.30 20.97
6 -1 0 7.87 11.57
6 -1 -1 6.55 12.33
6 -1 -2 17.65 16.67
6 -1 -3 165.47 12.67
6 -1 -4 10.86 12.45
6 -1 -5 348.95 20.14
6 -1 -6 1.00 16.92
6 -1 -7 10.72 17.89
6 -1 -8 4.40 21.54
6 -2 0 42.37 15.40
6 -2 -1 65.94 12.78
6 -2 -2 368.73 17.93
6 -2 -3 4.55 16.33
6 -2 -4 543.14 18.76
6 -2 -5 16.88 17.39
6 -2 -6 396.40 20.15
6 -2 -7 17.96 17.89
6 -2 -8 17.87 22.54
6 -3 0 52.03 17.02
6 -3 -1 94.76 16.21
6 -3 -2 82.61 15.90
6 -3 -3 315.23 18.90
6 -3 -4 2.08 12.76
6 -3 -5 222.07 14.26
6 -3 -6 8.33 19.33
6 -3 -7 137.70 20.65
6 -3 -8 27.92 22.65
6 -4 0 196.80 17.66
6 -4 -1 79.61 19.09
6 -4 -2 38.05 17.76
6 -4 -3 78.32 19.64
6 -4 -4 64.16 19.91
6 -4 -5 -3.40 18.80
6 -4 -6 139.30 19.45
6 -4 -7 16.54 22.40
-6 5 0 14.85 18.28
6 -5 0 -0.70 17.40
6 -5 -1 164.22 15.10
6 -5 -2 16.64 18.64
6 -5 -3 127.73 18.87
6 -5 -4 3.28 14.77
6 -5 -5 139.66 19.03
6 -5 -6 -4.56 21.72
6 -5 -7 206.98 22.79
-6 6 0 104.82 18.61
6 -6 0 91.53 15.07
6 -6 -1 -0.96 19.68
-6 6 1 -1.40 18.26
6 -6 -2 125.34 19.98
6 -6 -3 9.89 18.18
6 -6 -4 130.93 21.05
6 -6 -5 6.98 20.14
6 -7 0 7.15 19.60
-6 7 0 -0.54 20.94
-6 7 1 84.00 16.33
6 -7 -1 89.02 16.73
-6 7 2 -6.57 15.30
6 -7 -2 -3.56 19.69
6 -7 -3 115.60 20.04
6 -7 -4 20.71 20.36
5 9 -1 194.74 19.71
5 8 -1 19.02 12.79
5 7 -1 116.25 15.19
5 7 -2 -4.13 11.24
5 7 -7 108.71 19.35
5 7 -8 27.39 20.57
5 6 -1 25.06 11.24
5 6 -2 101.75 14.10
5 6 -3 29.68 14.03
5 6 -8 112.49 18.51
5 6 -9 68.51 20.24
5 5 -1 368.64 17.93
5 5 -2 30.71 10.45
5 5 -3 63.75 14.13
5 5 -4 130.86 13.88
5 5 -9 177.36 15.57
5 4 -1 26.45 12.91
5 4 -2 65.87 10.22
5 4 -3 48.70 14.60
5 4 -4 91.08 14.79
5 4 -5 22.68 15.22
5 4 -6 254.58 12.93
5 4 -7 31.99 12.40
5 4 -9 14.08 17.01
5 4 -10 45.93 20.39
5 3 -1 294.99 15.14
5 3 -2 4.94 13.81
5 3 -3 855.57 22.27
5 3 -4 8.55 10.93
5 3 -5 53.28 13.92
5 3 -6 52.79 14.57
5 3 -7 359.47 16.63
5 3 -8 136.57 15.45
5 3 -9 75.79 16.03
5 3 -9 86.33 17.10
5 3 -10 20.65 17.68
5 3 -10 20.76 18.62
5 2 -1 237.84 14.52
5 2 -2 423.88 13.27
5 2 -3 57.74 14.11
5 2 -4 775.69 23.16
5 2 -5 92.80 13.48
5 2 -6 257.01 15.44
5 2 -7 44.11 16.25
5 2 -8 122.93 16.20
5 2 -9 15.51 16.76
5 2 -10 215.01 21.88
5 2 -10 218.83 20.50
5 2 -11 20.44 21.62
5 2 -11 17.37 20.39
5 1 -1 91.98 12.59
5 1 -2 55.78 12.57
5 1 -3 78.82 13.60
5 1 -4 247.17 15.13
5 1 -5 490.37 14.73
5 1 -6 7.50 13.70
5 1 -7 146.34 12.79
5 1 -8 42.99 15.92
5 1 -9 216.61 18.25
5 1 -10 -4.39 18.58
5 1 -10 6.15 20.50
5 1 -11 225.85 22.95
5 1 -11 233.28 23.23
5 0 -1 -7.60 13.62
5 0 -2 198.37 10.47
5 0 -3 10.71 9.31
5 0 -4 78.06 13.94
5 0 -5 -0.88 9.98
5 0 -6 155.86 15.41
5 0 -7 -2.80 15.40
5 0 -8 159.66 17.11
5 0 -9 5.18 18.01
5 0 -10 20.14 20.66
5 0 -10 31.82 20.43
5 0 -11 -2.93 21.54
5 0 -11 4.42 23.93
5 -1 0 20.25 12.78
5 -1 -1 83.27 9.86
5 -1 -2 72.52 10.64
5 -1 -3 87.09 12.76
5 -1 -4 203.31 11.29
5 -1 -5 501.74 16.76
5 -1 -6 -0.72 15.54
5 -1 -7 144.90 15.58
5 -1 -8 50.55 16.06
5 -1 -9 195.22 18.80
5 -1 -10 0.09 21.97
5 -1 -10 5.03 20.79
5 -1 -11 173.46 29.80
5 -1 -11 227.48 28.37
5 -2 0 291.39 13.40
5 -2 -1 238.22 10.85
5 -2 -2 437.94 16.55
5 -2 -3 49.80 10.08
5 -2 -4 789.24 19.11
5 -2 -5 104.31 15.12
5 -2 -6 284.90 17.45
5 -2 -7 49.21 14.69
5 -2 -8 123.39 17.73
5 -2 -9 11.70 19.11
5 -2 -10 211.67 24.08
5 -2 -10 180.34 24.73
5 -2 -11 8.65 36.02
5 -2 -11 10.17 35.20
5 -3 0 23.40 13.64
-5 3 0 5.92 13.67
5 -3 -1 333.33 12.65
5 -3 -2 3.83 13.25
5 -3 -3 870.46 19.47
5 -3 -4 8.72 14.31
5 -3 -5 59.57 15.73
5 -3 -6 49.53 14.02
5 -3 -7 436.66 19.93
5 -3 -8 161.11 19.38
5 -3 -9 81.76 23.89
5 -3 -10 16.26 29.41
5 -3 -10 12.15 29.29
-5 4 0 145.00 14.99
5 -4 0 152.94 16.13
-5 4 1 1.74 14.85
5 -4 -1 43.53 16.14
5 -4 -2 67.86 13.95
5 -4 -3 25.33 10.00
5 -4 -4 82.18 14.12
5 -4 -5 45.30 15.19
5 -4 -6 284.64 17.67
5 -4 -7 37.88 17.55
5 -4 -8 268.78 23.16
5 -4 -9 10.87 26.38
-5 5 0 125.13 15.60
5 -5 0 116.46 16.65
5 -5 -1 383.37 15.81
-5 5 1 374.65 14.73
5 -5 -2 11.47 14.18
-5 5 2 19.44 14.96
5 -5 -3 58.87 15.10
5 -5 -4 124.45 12.51
5 -5 -5 333.20 18.61
5 -5 -6 10.57 16.33
5 -5 -7 84.23 18.38
5 -5 -8 106.94 22.76
5 -5 -9 114.97 41.48
5 -5 -9 128.89 42.75
-5 6 0 142.75 16.84
5 -6 0 125.86 16.62
-5 6 1 34.06 11.84
5 -6 -1 39.77 11.54
5 -6 -2 126.36 12.41
-5 6 2 117.09 15.66
5 -6 -3 20.25 15.92
-5 6 3 15.00 15.69
5 -6 -4 146.77 17.33
5 -6 -5 25.15 16.55
5 -6 -6 158.14 20.00
5 -6 -7 12.48 18.52
5 -6 -8 114.41 28.32
5 -7 0 36.38 13.19
-5 7 0 25.36 15.34
-5 7 1 114.19 16.03
5 -7 -1 140.21 13.13
-5 7 2 1.12 16.32
5 -7 -2 -0.56 17.09
-5 7 3 158.18 17.45
5 -7 -3 158.03 17.49
5 -7 -4 185.19 18.65
-5 7 4 180.96 17.87
5 -7 -5 213.04 17.97
5 -7 -6 2.39 18.96
5 -7 -7 105.28 23.85
5 -7 -8 6.79 31.88
-5 8 0 514.18 21.78
5 -8 0 487.03 18.88
-5 8 1 26.34 16.34
5 -8 -1 33.00 13.08
5 -8 -2 314.83 18.72
-5 8 2 302.94 18.90
-5 8 3 102.29 17.39
5 -8 -3 82.62 18.94
5 -8 -4 171.50 19.66
-5 8 4 166.87 17.63
5 -8 -5 5.94 18.74
5 -8 -6 205.57 23.17
5 -8 -7 65.65 25.60
-5 9 0 5.13 18.23
5 -9 0 15.04 18.06
5 -9 -1 214.65 18.77
-5 9 1 193.05 15.97
5 -9 -2 -3.30 18.59
-5 9 2 1.93 18.53
-5 9 3 112.56 20.13
5 -9 -3 102.90 19.55
-5 9 4 -0.73 21.73
5 -9 -4 19.99 19.44
5 -9 -5 76.87 22.46
5 -9 -6 2.97 26.04
-5 10 0 34.44 22.86
5 -10 0 22.95 22.73
-5 10 1 8.65 22.06
5 -10 -1 -3.80 22.41
5 -10 -2 192.80 17.34
-5 10 2 187.28 22.77
-5 10 3 7.05 20.31
4 11 -2 35.22 14.11
4 11 -4 14.96 15.56
4 11 -5 219.16 18.33
4 10 -5 10.73 16.84
4 10 -6 109.18 16.18
4 10 -7 -0.51 21.07
4 9 -6 -8.08 13.41
4 9 -7 30.77 14.57
4 9 -8 65.26 19.80
4 8 -7 -4.30 16.43
4 8 -8 109.85 19.88
4 8 -9 22.12 15.42
4 7 -6 16.46 11.28
4 7 -7 64.78 17.32
4 7 -8 5.13 16.58
4 7 -9 82.91 14.94
4 7 -10 8.47 16.06
4 6 -7 3.55 11.52
4 6 -8 90.03 13.46
4 6 -9 -0.65 16.65
4 6 -10 249.53 21.07
4 6 -11 1.43 19.58
4 5 -8 -0.53 14.36
4 5 -9 164.67 17.83
4 5 -10 27.01 18.78
4 5 -11 135.84 21.73
4 4 -1 6.39 8.39
4 4 -9 81.52 13.27
4 4 -10 191.47 18.63
4 4 -11 3.48 18.51
4 4 -12 36.68 20.42
4 3 -1 1665.63 35.58
4 3 -2 85.62 9.50
4 3 -3 407.44 14.80
4 3 -8 6.89 14.34
4 3 -9 368.81 18.81
4 3 -10 15.71 15.96
4 3 -11 20.01 20.14
4 3 -12 9.93 20.55
4 2 -1 1.72 11.26
4 2 -2 452.84 13.40
4 2 -3 72.48 11.72
4 2 -4 276.62 11.08
4 2 -5 144.84 12.24
4 2 -9 20.04 16.38
4 2 -10 3.63 17.19
4 2 -11 8.17 18.74
4 2 -12 80.13 22.11
4 1 -1 771.56 19.29
4 1 -2 9.54 10.70
4 1 -3 103.06 11.60
4 1 -4 8.01 8.44
4 1 -5 216.61 10.77
4 1 -6 315.58 14.97
4 1 -7 957.70 27.94
4 1 -8 7.36 13.30
4 1 -9 190.34 16.12
4 1 -9 187.95 16.82
4 1 -10 3.49 18.59
4 1 -10 -0.55 15.62
4 1 -11 47.47 20.01
4 1 -11 49.49 20.71
4 1 -12 56.54 23.99
4 1 -12 53.97 23.83
4 0 -1 7.47 11.67
4 0 -2 1289.98 37.74
4 0 -3 -12.81 11.19
4 0 -4 205.08 13.25
4 0 -5 -0.85 11.67
4 0 -6 1243.88 32.02
4 0 -7 3.06 12.38
4 0 -8 901.74 22.27
4 0 -9 -2.45 15.45
4 0 -9 -1.92 14.38
4 0 -10 217.08 18.30
4 0 -10 217.82 20.11
4 0 -11 -0.34 21.38
4 0 -11 -1.70 20.93
4 0 -12 146.28 27.04
4 0 -12 94.23 25.24
4 -1 0 3.34 8.91
4 -1 -1 724.25 16.31
4 -1 -2 3.66 10.86
4 -1 -3 101.50 12.22
4 -1 -4 8.08 11.59
4 -1 -5 252.24 13.80
4 -1 -6 324.23 14.90
4 -1 -7 984.48 32.16
4 -1 -8 11.87 16.58
4 -1 -9 182.46 19.14
4 -1 -9 174.78 16.39
4 -1 -10 2.06 21.64
4 -1 -10 3.59 18.78
4 -1 -11 48.67 27.15
4 -1 -11 42.90 23.59
-4 2 0 720.27 17.47
4 -2 0 718.43 15.62
4 -2 -1 -0.87 10.67
-4 2 1 -3.51 11.63
4 -2 -2 483.50 16.63
4 -2 -3 91.20 11.63
4 -2 -4 290.75 13.98
4 -2 -5 165.12 13.96
4 -2 -6 73.28 13.17
4 -2 -7 95.75 15.91
4 -2 -8 359.19 21.03
4 -2 -9 27.96 18.14
4 -2 -9 24.01 19.14
4 -2 -10 9.12 25.13
4 -2 -10 11.31 26.24
-4 3 0 -0.24 13.02
4 -3 0 2.63 8.66
4 -3 -1 1672.77 31.30
-4 3 1 1687.65 34.24
4 -3 -2 96.75 11.37
-4 3 2 81.56 12.38
4 -3 -3 458.97 17.73
4 -3 -4 23.69 11.57
4 -3 -5 230.48 14.96
4 -3 -6 49.56 13.01
4 -3 -7 473.71 19.35
4 -3 -8 2.44 16.70
4 -3 -9 340.38 27.18
4 -3 -9 378.18 28.81
-4 4 0 449.99 12.98
4 -4 0 470.52 14.83
-4 4 1 6.44 12.13
4 -4 -1 8.95 9.10
-4 4 2 249.25 15.04
4 -4 -2 259.20 11.64
-4 4 3 10.49 12.03
4 -4 -3 9.69 11.58
4 -4 -4 518.27 17.43
4 -4 -5 139.48 14.18
4 -4 -6 714.33 22.41
4 -4 -7 19.74 16.93
4 -4 -8 419.55 26.45
4 -5 0 145.66 10.42
-4 5 0 151.79 10.39
-4 5 1 73.85 13.35
4 -5 -1 75.38 13.27
-4 5 2 10.81 13.60
4 -5 -2 7.53 12.76
-4 5 3 156.56 13.90
4 -5 -3 169.80 14.06
-4 5 4 10.12 12.67
4 -5 -4 16.78 11.94
4 -5 -5 33.73 13.28
4 -5 -6 8.27 17.27
4 -5 -7 167.81 18.92
4 -5 -8 -0.49 32.38
4 -6 0 57.45 12.95
-4 6 0 48.71 14.10
-4 6 1 6.78 10.14
4 -6 -1 10.57 13.62
4 -6 -2 382.12 13.15
-4 6 2 368.52 16.38
-4 6 3 76.18 14.08
4 -6 -3 60.52 13.11
4 -6 -4 338.64 15.86
-4 6 4 340.11 16.00
4 -6 -5 74.71 15.39
4 -6 -6 382.99 20.30
4 -6 -7 5.68 21.61
-4 7 0 5.18 14.25
4 -7 0 14.76 10.79
4 -7 -1 279.93 16.52
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2 5 11 46.04 18.08
2 5 12 9.63 25.23
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2 6 6 485.64 16.54
2 6 7 87.46 13.14
2 6 8 77.48 15.09
2 6 9 9.12 15.89
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2 7 6 82.17 13.98
2 7 7 396.21 18.23
2 7 8 5.69 15.63
2 7 9 56.89 17.78
2 7 10 38.56 18.83
2 7 11 96.90 24.37
2 8 5 19.83 12.86
2 8 6 799.03 25.01
2 8 7 39.48 15.55
2 8 8 545.57 20.03
2 8 9 5.94 18.26
2 8 10 67.40 20.77
2 9 0 80.64 14.64
2 9 5 431.77 17.68
2 9 6 21.90 11.45
2 9 7 315.53 20.01
2 9 8 10.36 18.61
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2 10 6 311.30 18.79
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2 11 6 13.93 17.29
2 11 7 106.01 22.15
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2 12 5 9.95 20.83
2 12 6 187.92 22.53
2 12 6 166.93 20.06
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4 2 8 20.28 15.99
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4 2 10 10.41 16.23
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4 3 1 599.77 14.20
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4 3 6 10.19 14.76
4 3 7 443.92 14.96
4 3 8 6.60 12.61
4 3 9 21.34 14.05
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4 4 3 60.23 13.20
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4 4 6 257.61 16.47
4 4 7 17.86 15.96
4 4 8 465.94 19.31
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4 5 7 21.49 16.77
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4 6 1 7.24 12.00
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4 10 2 451.25 19.09
4 10 3 20.31 19.10
4 10 4 174.15 19.28
4 10 5 10.40 21.51
4 11 2 20.66 19.64
4 11 3 176.70 21.95
-5 9 -1 131.17 19.85
5 -9 1 121.15 15.73
-5 9 -2 16.35 14.96
5 -9 2 0.46 18.86
-5 9 -3 137.45 22.10
5 -9 3 142.83 20.65
5 -8 1 60.04 16.83
-5 8 -1 48.47 13.83
-5 8 -2 50.75 18.02
5 -8 2 67.78 17.81
-5 8 -3 13.29 14.88
5 -8 3 17.83 14.31
-5 8 -4 55.87 20.81
5 -8 4 99.76 15.97
5 -7 1 292.44 19.66
-5 7 -1 273.90 14.43
5 -7 2 3.69 16.30
-5 7 -2 -4.63 17.57
5 -7 3 64.52 16.92
-5 7 -3 41.22 17.14
5 -7 4 1.97 18.87
-5 7 -4 21.66 18.91
5 -7 5 98.98 15.11
-5 7 -5 96.29 18.86
5 -6 1 14.96 12.51
-5 6 -1 25.52 16.56
5 -6 2 52.69 12.60
-5 6 -2 52.97 12.80
5 -6 3 18.62 17.30
-5 6 -3 23.66 12.14
5 -6 4 195.78 14.51
-5 6 -4 159.00 18.54
5 -6 5 113.65 19.78
-5 6 -5 117.74 19.19
5 -6 6 261.13 21.35
-5 6 -6 247.80 21.05
-5 5 -1 178.28 15.43
5 -5 1 192.34 16.49
-5 5 -2 102.24 14.90
5 -5 2 86.04 10.96
5 -5 3 49.50 16.18
-5 5 -3 54.73 15.69
5 -5 4 76.77 16.20
-5 5 -4 69.16 12.83
5 -5 5 124.13 17.08
-5 5 -5 104.54 13.26
5 -5 6 103.11 19.42
-5 5 -6 90.01 14.15
5 -5 7 56.95 19.20
-5 5 -7 98.36 20.58
-5 4 -1 29.05 14.69
5 -4 1 36.22 10.62
-5 4 -2 437.22 14.79
5 -4 2 458.61 15.84
-5 4 -3 38.03 14.69
5 -4 3 48.54 14.27
-5 4 -4 52.39 12.07
5 -4 4 65.98 15.33
5 -4 5 25.97 12.64
-5 4 -5 34.14 16.07
5 -4 6 62.27 18.84
-5 4 -6 62.73 17.35
5 -4 7 -10.74 15.21
-5 4 -7 5.42 14.82
-5 3 -1 182.64 12.05
5 -3 1 177.78 14.95
-5 3 -2 33.62 14.96
5 -3 2 28.88 13.90
-5 3 -3 374.37 15.66
5 -3 3 379.87 16.06
-5 3 -4 17.43 14.48
5 -3 4 6.10 11.38
-5 3 -5 60.84 11.84
5 -3 5 61.70 15.28
5 -3 6 22.61 16.89
-5 3 -6 14.94 16.09
5 -3 7 63.65 14.01
-5 3 -7 60.53 13.70
5 -3 8 -5.25 16.29
-5 3 -8 -11.50 19.67
5 -2 1 43.34 10.05
-5 2 -1 39.22 10.30
-5 2 -2 298.30 15.01
5 -2 2 305.74 15.53
-5 2 -3 10.73 10.61
5 -2 3 12.04 10.08
-5 2 -4 406.87 14.82
5 -2 4 430.97 16.99
-5 2 -5 100.22 16.49
5 -2 5 115.68 16.75
-5 2 -6 47.47 15.98
5 -2 6 46.58 17.10
5 -2 7 17.31 18.77
-5 2 -7 -6.80 19.08
5 -2 8 94.04 21.20
-5 2 -8 89.04 16.04
5 -1 1 310.59 14.39
5 -1 2 86.89 14.49
5 -1 3 284.44 11.73
-5 1 -3 286.82 16.82
-5 1 -4 15.49 11.21
5 -1 4 16.77 10.96
-5 1 -5 137.44 15.28
5 -1 5 144.20 15.33
-5 1 -6 1.86 12.17
5 -1 6 -1.12 17.26
5 -1 7 65.73 17.18
-5 1 -7 67.96 13.78
5 -1 8 -4.60 15.57
-5 1 -8 22.01 20.49
5 0 0 154.79 10.71
5 0 1 -5.53 12.90
5 0 2 146.81 14.20
5 0 3 -4.25 13.76
5 0 4 14.30 11.41
5 0 5 -6.94 11.57
5 0 6 69.76 16.39
5 0 7 -7.47 14.21
5 0 8 29.76 18.73
5 1 0 22.51 9.73
5 1 1 321.98 12.36
5 1 2 84.68 10.47
5 1 3 294.23 15.34
5 1 4 6.01 14.39
5 1 5 143.14 15.49
5 1 6 1.51 11.77
5 1 7 72.58 18.81
5 1 8 -0.31 20.53
5 2 0 312.01 15.62
5 2 1 37.90 13.66
5 2 2 322.61 15.06
5 2 3 20.85 13.50
5 2 4 429.89 17.53
5 2 5 98.01 16.95
5 2 6 26.41 17.70
5 2 7 12.41 17.38
5 2 8 92.88 18.99
5 3 0 5.73 12.52
5 3 1 177.73 15.59
5 3 2 30.98 10.63
5 3 3 386.24 17.26
5 3 4 -1.97 11.45
5 3 5 64.15 11.97
5 3 6 20.88 13.09
5 3 7 77.92 18.42
5 3 8 -11.09 20.93
5 4 0 156.29 14.40
5 4 1 28.44 10.26
5 4 2 451.86 20.33
5 4 3 46.02 11.42
5 4 4 48.66 12.11
5 4 5 32.45 12.46
5 4 6 64.88 13.98
5 4 7 14.36 17.59
5 5 0 96.39 14.66
5 5 1 158.64 11.22
5 5 2 94.76 14.40
5 5 3 47.19 11.73
5 5 4 93.07 13.11
5 5 5 108.85 13.35
5 5 6 84.32 18.50
5 5 7 94.99 20.93
5 6 0 123.32 11.72
5 6 1 14.29 11.40
5 6 2 54.57 14.69
5 6 3 11.37 16.54
5 6 4 189.21 17.19
5 6 5 105.79 19.36
5 6 6 275.01 20.34
5 7 0 37.55 15.18
5 7 1 308.39 14.50
5 7 2 -3.71 16.68
5 7 3 49.87 13.35
5 7 4 19.21 14.88
5 7 5 104.59 18.11
5 8 0 532.91 17.57
5 8 1 43.71 13.61
5 8 2 59.57 17.94
5 8 3 29.98 17.34
5 8 4 75.03 18.95
5 9 0 10.95 17.90
5 9 1 141.96 17.88
5 9 2 16.26 14.75
5 9 3 146.39 20.25
5 10 0 8.56 19.85
6 -7 1 108.01 20.61
6 -6 1 9.73 18.82
-6 6 -1 7.59 14.73
6 -6 2 79.97 19.54
-6 6 -2 71.00 21.64
6 -5 1 67.29 15.12
-6 5 -1 94.10 20.16
6 -5 2 4.66 14.34
-6 5 -2 -0.94 14.64
6 -5 3 126.26 18.89
-6 5 -3 129.71 15.60
6 -4 1 -4.05 13.39
-6 4 -1 -3.63 17.28
6 -4 2 214.66 19.20
-6 4 -2 200.07 19.11
6 -4 3 15.92 18.15
-6 4 -3 2.09 18.87
6 -4 4 75.75 19.43
-6 4 -4 48.33 19.12
6 -3 1 38.00 16.03
6 -3 2 4.67 13.61
-6 3 -3 120.10 18.92
6 -3 3 134.99 14.37
6 -3 4 10.85 17.96
-6 3 -4 7.13 19.31
6 -3 5 69.37 22.39
6 -2 1 7.06 16.56
6 -2 2 298.30 18.64
6 -2 3 4.56 16.35
6 -2 4 188.95 15.42
6 -2 5 -5.54 19.05
6 -1 1 356.43 15.81
6 -1 2 32.07 15.70
6 -1 3 278.33 17.71
6 -1 4 12.88 17.03
6 -1 5 11.10 16.42
6 0 0 38.05 16.12
6 0 1 8.70 15.60
6 0 2 172.82 13.17
6 0 3 9.17 16.34
6 0 4 30.90 19.28
6 0 5 -7.53 20.27
6 1 0 3.21 14.86
6 1 1 357.70 18.52
6 1 2 33.29 15.74
6 1 3 298.66 14.76
6 1 4 5.66 14.48
6 1 5 30.34 15.26
6 2 0 52.81 17.02
6 2 1 13.55 12.26
6 2 2 292.87 17.14
6 2 3 5.03 18.29
6 2 4 194.86 18.84
6 2 5 -4.08 14.79
6 3 0 52.34 12.63
6 3 1 30.64 16.82
6 3 2 14.30 16.14
6 3 3 128.73 18.79
6 3 4 12.98 19.76
6 3 5 64.77 15.58
6 4 0 207.59 18.32
6 4 1 -0.22 17.57
6 4 2 183.65 17.51
6 4 3 -1.56 18.65
6 4 4 66.88 18.69
6 5 0 5.04 13.35
6 5 1 81.85 17.63
6 5 2 10.28 17.54
6 5 3 135.75 19.10
6 6 0 103.95 20.45
6 6 1 1.77 17.96
6 6 2 66.00 19.04
6 7 0 1.46 21.26
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 34977
_shelx_res_file
;
TITL shelxt_a.res in P2(1)/c
shelx.res
created by SHELXL-2018/3 at 13:37:33 on 01-Aug-2019
CELL 0.71073 5.1145 10.6123 10.4179 90.000 97.858 90.000
ZERR 2.00 0.0007 0.0012 0.0013 0.000 0.010 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H CO N O
UNIT 16 20 2 8 12
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 N2 O1_$2
HTAB N2 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 N2 O1_$2
HTAB N2 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 3
L.S. 4
TEMP -123.00
WGHT 0.022700
FVAR 0.83755
CO1 3 0.500000 0.500000 0.500000 10.50000 0.01397 0.01072 =
0.01381 0.00071 0.00483 0.00019
C2 1 0.269114 0.891708 0.427263 11.00000 0.02269 0.01614 =
0.02304 -0.00204 0.00787 0.00636
AFIX 44
H2 2 0.192547 0.964691 0.430846 11.00000 -1.20000
AFIX 0
O1 5 0.737267 0.547663 0.357437 11.00000 0.01633 0.01212 =
0.01913 0.00216 0.00711 0.00179
O3 5 0.215176 0.443959 0.347018 11.00000 0.01515 0.01420 =
0.02211 -0.00358 0.00316 0.00184
O2 5 0.815244 0.700894 0.220671 11.00000 0.02541 0.01803 =
0.02237 0.00346 0.01290 0.00183
N1 4 0.389479 0.691309 0.466007 11.00000 0.01573 0.01337 =
0.01601 0.00040 0.00402 0.00072
C3 1 0.514531 0.736938 0.372290 11.00000 0.01581 0.01404 =
0.01612 0.00038 0.00326 0.00011
C4 1 0.704363 0.659126 0.310277 11.00000 0.01362 0.01461 =
0.01495 -0.00111 0.00255 -0.00171
C1 1 0.235902 0.788375 0.501378 11.00000 0.01704 0.01857 =
0.02034 -0.00169 0.00843 0.00355
AFIX 44
H1 2 0.128588 0.784312 0.564526 11.00000 -1.20000
AFIX 0
N2 4 0.445506 0.858183 0.346654 11.00000 0.02643 0.01363 =
0.02095 0.00414 0.00885 0.00258
AFIX 44
H2A 2 0.502579 0.905514 0.289806 11.00000 -1.20000
AFIX 0
H3A 2 0.198455 0.368140 0.336781 11.00000 0.03051
H3B 2 0.075959 0.474375 0.343291 11.00000 0.04368
HKLF 4
REM shelxt_a.res in P2(1)/c
REM wR2 = 0.0478, GooF = S = 0.835, Restrained GooF = 0.835 for all data
REM R1 = 0.0234 for 1078 Fo > 4sig(Fo) and 0.0403 for all 1495 data
REM 99 parameters refined using 0 restraints
END
WGHT 0.0227 0.0000
REM Highest difference peak 0.323, deepest hole -0.280, 1-sigma level 0.063
Q1 1 0.6087 0.7026 0.3434 11.00000 0.05 0.32
Q2 1 0.4108 0.4282 0.5213 11.00000 0.05 0.30
Q3 1 0.3123 0.8545 0.4975 11.00000 0.05 0.27
Q4 1 0.3425 0.7373 0.4917 11.00000 0.05 0.27
Q5 1 0.3229 0.4754 0.4309 11.00000 0.05 0.26
Q6 1 0.8399 0.5084 0.3347 11.00000 0.05 0.26
Q7 1 0.6564 0.5030 0.3550 11.00000 0.05 0.26
Q8 1 0.6731 0.5826 0.3247 11.00000 0.05 0.24
Q9 1 0.3769 0.5575 0.5199 11.00000 0.05 0.24
Q10 1 0.4050 0.7088 0.4026 11.00000 0.05 0.23
Q11 1 0.4502 0.5982 0.4608 11.00000 0.05 0.22
Q12 1 0.4589 0.7799 0.3386 11.00000 0.05 0.22
Q13 1 0.3214 0.8678 0.3852 11.00000 0.05 0.20
Q14 1 0.6910 0.5775 0.4010 11.00000 0.05 0.20
Q15 1 0.5022 0.7104 0.4548 11.00000 0.05 0.20
Q16 1 0.2826 0.6413 0.4446 11.00000 0.05 0.19
Q17 1 0.1605 0.8392 0.4446 11.00000 0.05 0.19
Q18 1 0.5555 0.5591 0.3945 11.00000 0.05 0.18
Q19 1 -0.1331 0.4973 0.2204 11.00000 0.05 0.18
Q20 1 0.6828 0.7612 0.1859 11.00000 0.05 0.18
;
_shelx_res_checksum 77353
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 0.01256(8) Uani d 1
C C2 0.2691(3) 0.89171(17) 0.42726(16) 0.0202(4) Uani d 1
H H2 0.1925(19) 0.9647(17) 0.43085(18) 0.024 Uiso calc 1
O O1 0.7373(2) 0.54766(10) 0.35744(11) 0.0154(2) Uani d 1
O O3 0.2152(2) 0.44396(13) 0.34702(12) 0.0171(2) Uani d 1
O O2 0.8152(2) 0.70089(11) 0.22067(12) 0.0210(3) Uani d 1
N N1 0.3895(3) 0.69131(12) 0.46601(13) 0.0149(3) Uani d 1
C C3 0.5145(3) 0.73694(15) 0.37229(15) 0.0152(3) Uani d 1
C C4 0.7044(3) 0.65913(15) 0.31028(15) 0.0143(3) Uani d 1
C C1 0.2359(3) 0.78838(15) 0.50138(17) 0.0181(3) Uani d 1
H H1 0.129(2) 0.78431(18) 0.5645(14) 0.022 Uiso calc 1
N N2 0.4455(3) 0.85818(13) 0.34665(14) 0.0198(3) Uani d 1
H H2A 0.5026(15) 0.9055(12) 0.2898(14) 0.024 Uiso calc 1
H H3A 0.198(4) 0.368(2) 0.337(2) 0.031(6) Uiso d 1
H H3B 0.076(5) 0.474(2) 0.343(2) 0.044(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 0.01397(13) 0.01072(13) 0.01381(14) 0.00019(14) 0.00483(9) 0.00071(15)
C2 0.0227(8) 0.0161(8) 0.0230(9) 0.0064(6) 0.0079(7) -0.0020(7)
O1 0.0163(5) 0.0121(5) 0.0191(6) 0.0018(4) 0.0071(4) 0.0022(4)
O3 0.0152(6) 0.0142(6) 0.0221(6) 0.0018(5) 0.0032(4) -0.0036(5)
O2 0.0254(6) 0.0180(6) 0.0224(6) 0.0018(5) 0.0129(5) 0.0035(5)
N1 0.0157(6) 0.0134(7) 0.0160(6) 0.0007(5) 0.0040(5) 0.0004(5)
C3 0.0158(7) 0.0140(8) 0.0161(8) 0.0001(6) 0.0033(6) 0.0004(6)
C4 0.0136(7) 0.0146(8) 0.0149(8) -0.0017(6) 0.0025(6) -0.0011(6)
C1 0.0170(7) 0.0186(8) 0.0203(8) 0.0036(6) 0.0084(6) -0.0017(7)
N2 0.0264(7) 0.0136(7) 0.0210(7) 0.0026(5) 0.0088(6) 0.0041(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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 93.48(5)
O3 Co1 O1 3_666 3_666 86.52(5)
O3 Co1 O1 . . 86.52(5)
O3 Co1 O1 3_666 . 93.48(5)
O1 Co1 O1 3_666 . 180.0
O3 Co1 N1 . 3_666 89.83(5)
O3 Co1 N1 3_666 3_666 90.17(5)
O1 Co1 N1 3_666 3_666 79.55(5)
O1 Co1 N1 . 3_666 100.45(5)
O3 Co1 N1 . . 90.17(5)
O3 Co1 N1 3_666 . 89.83(5)
O1 Co1 N1 3_666 . 100.45(5)
O1 Co1 N1 . . 79.55(5)
N1 Co1 N1 3_666 . 180.0
N2 C2 C1 . . 106.45(15)
N2 C2 H2 . . 126.8
C1 C2 H2 . . 126.8
C4 O1 Co1 . . 115.71(10)
Co1 O3 H3A . . 115.5(14)
Co1 O3 H3B . . 117.2(18)
H3A O3 H3B . . 109(2)
C3 N1 C1 . . 105.88(13)
C3 N1 Co1 . . 109.07(10)
C1 N1 Co1 . . 145.04(12)
N1 C3 N2 . . 110.67(14)
N1 C3 C4 . . 121.65(14)
N2 C3 C4 . . 127.67(15)
O2 C4 O1 . . 124.67(15)
O2 C4 C3 . . 121.46(15)
O1 C4 C3 . . 113.87(14)
C2 C1 N1 . . 109.28(15)
C2 C1 H1 . . 125.4
N1 C1 H1 . . 125.4
C3 N2 C2 . . 107.71(15)
C3 N2 H2A . . 126.1
C2 N2 H2A . . 126.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O3 . 2.0931(11)
Co1 O3 3_666 2.0931(11)
Co1 O1 3_666 2.1041(12)
Co1 O1 . 2.1041(12)
Co1 N1 3_666 2.1241(13)
Co1 N1 . 2.1242(13)
C2 N2 . 1.361(2)
C2 C1 . 1.365(2)
C2 H2 . 0.87(2)
O1 C4 . 1.2831(19)
O3 H3A . 0.81(2)
O3 H3B . 0.78(2)
O2 C4 . 1.239(2)
N1 C3 . 1.329(2)
N1 C1 . 1.376(2)
C3 N2 . 1.351(2)
C3 C4 . 1.488(2)
C1 H1 . 0.91(2)
N2 H2A . 0.86(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 0.91 2.44 3.347(2) 172.4 yes
N2 H2A O1 2_655 0.86 2.37 2.9824(18) 128.7 yes
N2 H2A O3 2_655 0.86 2.20 2.978(2) 150.6 yes
O3 H3A O2 2_645 0.81(2) 1.87(2) 2.6731(18) 168(2) yes
O3 H3B O1 1_455 0.78(2) 1.92(3) 2.6963(17) 173(2) 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 N2 -0.31(16)
Co1 N1 C3 N2 179.03(10)
C1 N1 C3 C4 178.99(14)
Co1 N1 C3 C4 -1.67(16)
Co1 O1 C4 O2 -175.67(11)
Co1 O1 C4 C3 3.72(15)
N1 C3 C4 O2 178.08(14)
N2 C3 C4 O2 -2.8(2)
N1 C3 C4 O1 -1.3(2)
N2 C3 C4 O1 177.84(14)
N2 C2 C1 N1 -0.45(18)
C3 N1 C1 C2 0.47(17)
Co1 N1 C1 C2 -178.44(14)
N1 C3 N2 C2 0.04(17)
C4 C3 N2 C2 -179.21(14)
C1 C2 N2 C3 0.25(18)
_cod_database_fobs_code 2021757