#------------------------------------------------------------------------------
#$Date: 2023-09-09 04:37:05 +0300 (Sat, 09 Sep 2023) $
#$Revision: 286285 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022856.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_2022856
loop_
_publ_author_name
'N\"ather, Christian'
'Jess, Inke'
_publ_section_title
;
Synthesis and crystal structure of
catena-poly[cobalt(II)-di-\m-chlorido-\m-pyridazine-\k2 N 1:N 2]
;
_journal_coeditor_code HB8073
_journal_issue 10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023007065
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '[Co Cl2 (C4 H4 N2)]'
_chemical_formula_moiety 'C4 H4 Cl2 Co N2'
_chemical_formula_sum 'C4 H4 Cl2 Co N2'
_chemical_formula_weight 209.92
_chemical_name_systematic
catena-poly[cobalt(II)-di-\m-chlorido-\m-pyridazine-\k^2^N^1^:N^2^]
_space_group_crystal_system orthorhombic
_space_group_IT_number 74
_space_group_name_Hall '-I 2b 2'
_space_group_name_H-M_alt 'I m m a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2016/6
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.69350(10)
_cell_length_b 7.20240(10)
_cell_length_c 12.7978(2)
_cell_measurement_reflns_used 2503
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 78.2240
_cell_measurement_theta_min 6.9070
_cell_volume 616.973(16)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0271
_diffrn_reflns_av_unetI/netI 0.0139
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 3164
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 80.178
_diffrn_reflns_theta_min 6.920
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 28.908
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.31624
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour pink
_exptl_crystal_density_diffrn 2.260
_exptl_crystal_description block
_exptl_crystal_F_000 412
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.638
_refine_diff_density_min -0.338
_refine_ls_extinction_coef 0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 30
_refine_ls_number_reflns 395
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.068
_refine_ls_R_factor_all 0.0206
_refine_ls_R_factor_gt 0.0203
_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^)+(0.0390P)^2^+0.9618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0575
_refine_ls_wR_factor_ref 0.0577
_reflns_number_gt 386
_reflns_number_total 395
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8073sup1.cif
_cod_data_source_block I
_cod_database_code 2022856
_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
;
-8 0 0 1885.46 40.63
-8 0 0 1736.27 39.40
-6 0 0 29.25 4.19
-6 0 0 23.81 4.90
-4 0 0 2401.05 48.38
-4 0 0 2471.48 49.77
-2 0 0 134.87 3.47
2 0 0 133.47 3.55
4 0 0 2308.66 46.34
8 0 0 1746.72 39.29
-7 0 -1 283.70 12.28
-7 0 1 262.50 11.72
-5 0 -1 361.92 10.20
-5 0 -1 362.33 11.24
-5 0 1 346.50 10.00
-3 0 1 1257.09 23.63
-3 0 1 1179.10 24.52
-3 0 -1 1199.14 24.50
-3 0 -1 1220.55 23.28
-3 0 -1 1168.49 23.44
-1 0 1 209.79 4.11
-1 0 -1 190.72 3.94
1 0 -1 192.87 4.22
1 0 1 184.64 3.96
1 0 1 193.99 4.17
3 0 -1 1165.59 23.98
3 0 1 1188.61 24.12
5 0 1 324.62 9.77
5 0 -1 363.69 10.57
7 0 -1 255.07 11.48
-8 0 -2 1467.22 33.10
-8 0 2 1549.87 34.58
-6 0 -2 36.05 4.10
-6 0 -2 31.70 4.19
-6 0 -2 32.44 5.24
-6 0 2 28.82 5.18
-4 0 2 3700.86 73.12
-4 0 2 3881.30 74.81
-4 0 -2 3719.79 74.06
-4 0 2 3744.74 71.51
-4 0 -2 3612.72 73.13
-2 0 -2 122.61 2.70
-2 0 -2 124.04 3.50
-2 0 2 125.61 3.07
0 0 -2 2458.59 52.76
0 0 2 2810.86 51.90
2 0 2 116.92 2.98
2 0 2 117.36 3.43
4 0 2 3608.55 69.32
4 0 -2 3413.68 69.24
6 0 -2 32.14 5.34
8 0 2 1433.23 33.31
8 0 -2 1470.81 33.37
-7 0 3 405.55 14.91
-7 0 -3 428.96 14.81
-7 0 -3 440.04 15.51
-5 0 -3 1489.65 31.81
-5 0 -3 1458.86 32.49
-5 0 3 1431.93 31.52
-3 0 3 1174.90 22.92
-3 0 -3 1100.10 23.80
-1 0 -3 2397.92 45.12
-1 0 -3 2277.45 46.09
1 0 3 2275.22 43.35
1 0 -3 2262.40 44.23
3 0 -3 1072.68 23.08
3 0 3 1125.35 23.06
5 0 3 1451.45 31.59
5 0 -3 1398.51 31.28
5 0 -3 1467.56 34.61
7 0 -3 419.84 15.03
-8 0 4 162.22 6.67
-8 0 -4 123.82 4.92
-6 0 -4 107.24 5.77
-6 0 -4 97.82 7.42
-6 0 -4 99.00 6.37
-6 0 -4 95.14 7.72
-6 0 4 101.54 7.73
-4 0 -4 1894.72 38.46
-4 0 4 1963.37 38.75
-4 0 -4 1874.61 38.65
-2 0 -4 2394.35 45.18
-2 0 4 2271.97 46.66
-2 0 -4 2270.42 46.62
-2 0 4 2415.65 45.82
0 0 -4 1305.68 26.52
0 0 4 1300.97 25.06
0 0 4 1281.86 26.07
0 0 -4 1274.97 25.03
2 0 4 2131.48 41.73
2 0 -4 2172.80 42.64
4 0 -4 1741.17 37.59
4 0 4 1857.10 37.81
4 0 -4 1823.57 40.47
6 0 -4 95.85 7.71
6 0 -4 82.89 5.69
-7 0 5 663.01 19.47
-7 0 -5 661.13 18.61
-5 0 -5 89.44 5.16
-5 0 -5 92.03 5.98
-5 0 -5 82.55 4.70
-5 0 5 93.61 6.85
-5 0 5 97.01 7.24
-5 0 -5 90.36 6.92
-5 0 -5 87.58 7.08
-5 0 5 95.34 5.31
-3 0 -5 1365.04 27.94
-3 0 5 1279.04 26.26
-1 0 -5 4629.70 84.26
-1 0 5 4368.62 84.52
-1 0 5 4480.13 85.70
1 0 5 4538.83 85.15
1 0 -5 4244.79 86.97
3 0 -5 1278.55 29.71
3 0 -5 1282.09 27.29
3 0 5 1272.76 27.19
3 0 -5 1260.13 28.79
5 0 -5 87.47 7.16
5 0 5 83.04 4.99
5 0 -5 83.11 5.87
5 0 -5 98.45 5.25
7 0 -5 648.97 19.29
-6 0 6 2193.02 48.84
-6 0 -6 2107.04 48.43
-6 0 6 2074.31 49.11
-4 0 6 94.34 3.81
-4 0 -6 121.63 5.66
-2 0 -6 1653.24 34.27
-2 0 6 1704.57 34.25
0 0 6 381.21 8.61
0 0 6 401.98 9.74
0 0 -6 406.80 10.41
2 0 -6 1624.00 34.25
2 0 6 1634.99 32.80
4 0 -6 92.24 6.03
4 0 6 95.91 5.13
6 0 -6 2034.81 46.51
6 0 -6 1891.39 42.71
-7 0 -7 104.86 5.52
-7 0 7 108.78 6.19
-7 0 -7 100.88 5.19
-5 0 7 768.18 21.87
-5 0 7 759.18 23.37
-5 0 -7 769.05 22.30
-3 0 -7 218.87 7.80
-3 0 7 229.44 7.89
-3 0 7 222.32 6.40
-1 0 7 210.72 5.82
-1 0 -7 243.62 7.84
-1 0 -7 201.68 8.80
-1 0 7 236.69 7.11
1 0 -7 214.13 7.35
1 0 7 215.28 5.59
1 0 7 218.90 6.65
1 0 -7 232.74 9.46
1 0 -7 207.87 7.85
3 0 -7 203.89 7.66
3 0 -7 209.42 9.94
3 0 7 211.54 7.61
3 0 -7 222.79 8.83
5 0 -7 699.04 19.74
5 0 -7 713.09 22.30
7 0 -7 100.65 6.16
-6 0 -8 1720.01 38.80
-6 0 -8 1686.21 38.50
-6 0 8 1780.78 39.35
-6 0 8 1689.39 40.07
-4 0 8 70.28 3.61
-4 0 8 64.48 5.58
-4 0 8 74.12 5.03
-4 0 -8 69.23 4.56
-2 0 8 4418.68 86.51
-2 0 -8 4218.52 88.57
0 0 -8 41.38 3.16
0 0 8 32.43 2.71
0 0 -8 36.30 4.50
0 0 8 33.26 2.15
2 0 -8 4083.06 84.90
2 0 -8 3987.93 87.04
4 0 -8 67.20 5.61
4 0 -8 73.28 5.17
4 0 -8 68.92 4.95
4 0 -8 76.82 7.24
4 0 8 68.91 4.84
6 0 -8 1465.84 33.13
6 0 -8 1604.89 37.11
-7 0 9 -0.15 1.47
-5 0 9 10.49 3.95
-5 0 -9 8.59 3.99
-5 0 9 8.96 4.78
-3 0 -9 0.97 3.16
-3 0 9 2.11 2.50
-3 0 -9 0.74 2.58
-3 0 9 0.90 2.86
-1 0 9 244.30 7.14
-1 0 -9 262.35 8.95
-1 0 9 248.09 8.23
-1 0 -9 252.33 11.00
1 0 -9 237.75 10.66
1 0 9 231.60 6.59
1 0 -9 238.68 8.14
1 0 9 230.97 7.51
3 0 9 0.37 2.26
3 0 -9 0.79 2.75
3 0 9 -0.76 2.46
3 0 -9 2.54 4.38
3 0 -9 2.05 3.25
3 0 -9 1.95 2.77
5 0 -9 9.42 4.61
5 0 -9 5.18 3.11
-6 0 10 956.91 22.09
-6 0 -10 915.15 21.62
-6 0 -10 880.94 20.84
-4 0 10 33.36 4.48
-4 0 -10 30.11 3.64
-4 0 -10 37.14 5.00
-2 0 -10 2593.43 51.99
-2 0 10 2537.14 51.21
-2 0 -10 2384.89 53.20
-2 0 10 2288.36 51.89
-2 0 10 2503.94 49.67
-2 0 -10 2352.38 52.03
0 0 -10 510.68 13.34
0 0 -10 492.91 16.07
0 0 10 421.45 12.12
0 0 10 425.28 11.08
2 0 -10 2414.40 50.03
2 0 -10 2422.88 53.57
2 0 -10 2273.39 48.89
2 0 10 2285.76 48.09
4 0 -10 33.99 4.32
4 0 -10 35.15 5.90
6 0 -10 918.37 22.20
-5 0 11 676.29 18.05
-5 0 11 626.51 16.32
-5 0 -11 629.55 16.99
-3 0 11 731.75 19.26
-3 0 -11 729.13 20.47
-3 0 -11 739.22 20.55
-1 0 11 181.60 6.97
-1 0 -11 176.77 8.58
-1 0 11 176.57 6.18
1 0 -11 173.75 7.72
1 0 -11 180.87 9.65
1 0 11 161.96 6.43
3 0 -11 753.66 22.27
3 0 -11 739.02 19.67
5 0 -11 637.09 17.53
5 0 -11 627.94 15.69
-4 0 -12 61.02 5.01
-4 0 12 67.03 4.30
-4 0 -12 66.21 4.88
-4 0 12 69.38 5.57
-2 0 12 709.58 18.50
-2 0 -12 752.27 20.45
0 0 -12 568.01 16.86
0 0 -12 591.93 18.37
0 0 -12 553.52 15.65
2 0 -12 773.19 22.06
4 0 -12 67.58 5.27
4 0 -12 63.02 4.52
-5 0 -13 502.43 11.83
-5 0 13 533.52 11.89
-3 0 -13 461.18 12.32
-3 0 13 412.59 11.54
-3 0 -13 466.95 13.50
-3 0 -13 429.75 11.64
-1 0 -13 775.97 20.54
1 0 -13 784.49 20.09
1 0 -13 788.97 21.64
3 0 -13 453.19 13.15
3 0 -13 464.46 13.92
-4 0 14 459.21 11.05
-4 0 -14 457.81 10.96
-2 0 -14 35.28 3.61
0 0 -14 792.52 18.94
2 0 -14 33.87 3.57
2 0 -14 30.99 3.76
4 0 -14 424.19 10.05
-3 0 15 188.67 5.53
-1 0 -15 384.82 10.57
1 0 -15 371.07 10.01
1 0 -15 384.33 10.43
3 0 -15 181.43 5.35
0 0 -16 818.86 17.61
-7 -1 0 0.52 3.18
-7 1 0 1.18 4.39
-7 -1 0 4.02 4.08
-5 1 0 0.41 1.93
-5 -1 0 1.17 1.99
-3 -1 0 0.60 0.36
-3 -1 0 -0.04 0.95
-3 1 0 0.14 0.99
-1 1 0 0.07 0.39
-1 -1 0 0.20 0.25
-1 -1 0 0.11 0.32
-1 -1 0 0.11 0.36
1 1 0 -0.08 0.23
1 -1 0 0.27 0.53
1 -1 0 0.60 0.45
3 1 0 0.56 0.95
5 -1 0 -1.47 2.06
5 1 0 1.45 1.96
7 1 0 1.21 3.70
7 -1 0 3.98 3.76
-8 -1 -1 435.30 12.81
-8 -1 1 430.69 12.70
-8 1 1 442.33 12.83
-6 -1 1 373.14 13.66
-6 -1 -1 363.44 13.07
-6 1 1 379.80 13.50
-6 -1 -1 398.95 13.95
-6 1 -1 386.98 14.18
-6 1 -1 376.06 13.29
-6 1 1 398.14 14.20
-4 -1 1 1032.44 22.25
-4 -1 1 1042.22 23.88
-4 1 1 1009.12 23.98
-4 -1 -1 1084.87 22.47
-4 1 1 1071.20 22.48
-4 1 1 1068.31 21.36
-4 -1 -1 1056.27 23.37
-4 1 -1 1092.60 22.64
-4 1 -1 1020.65 21.29
-2 1 -1 1022.21 19.94
-2 1 1 1011.47 20.20
-2 -1 1 987.17 20.05
-2 1 -1 1009.05 20.11
-2 -1 1 983.43 20.05
-2 -1 -1 1004.81 20.07
-2 -1 1 1022.36 19.53
0 1 1 3270.37 63.95
0 -1 -1 3420.81 64.23
2 1 1 1021.09 20.43
2 -1 1 981.62 20.61
4 1 1 1057.69 23.12
4 -1 1 1111.36 23.69
4 -1 -1 1053.08 23.42
8 1 1 391.05 12.36
8 -1 -1 383.06 10.32
-7 -1 2 14.62 4.48
-7 1 -2 16.20 4.11
-7 -1 -2 14.73 3.70
-7 1 2 17.36 4.71
-7 1 -2 15.27 4.91
-7 -1 2 17.19 3.64
-7 -1 -2 19.34 4.67
-5 -1 -2 32.71 3.31
-5 1 2 28.31 3.04
-5 1 -2 35.97 3.26
-5 1 -2 31.21 4.00
-5 -1 2 31.15 2.94
-5 1 2 32.14 4.01
-5 -1 -2 35.21 3.10
-3 1 -2 26.98 1.97
-3 -1 -2 25.32 1.89
-3 -1 2 29.28 1.85
-3 1 -2 27.91 1.40
-3 -1 2 27.23 1.25
-3 1 2 28.45 1.61
-3 1 2 24.81 1.85
-3 -1 2 29.69 1.92
-3 1 2 27.88 1.96
-1 1 -2 2.53 0.76
-1 1 -2 3.03 0.68
-1 1 -2 2.63 0.57
-1 -1 -2 1.54 0.69
-1 -1 -2 2.05 0.67
-1 1 2 3.37 0.65
-1 -1 2 2.28 0.53
1 1 2 1.80 0.21
1 -1 -2 2.62 0.73
1 1 -2 2.46 0.52
3 1 2 25.62 1.77
3 -1 2 27.61 2.02
3 -1 2 28.59 1.81
3 1 -2 29.10 1.92
5 -1 -2 31.79 3.13
5 1 2 31.23 2.72
5 1 -2 28.59 2.82
5 -1 2 33.17 3.35
7 -1 -2 13.20 3.65
7 -1 -2 12.29 4.17
7 1 -2 15.93 4.48
-8 -1 3 424.43 12.24
-8 1 3 435.11 12.29
-8 -1 -3 401.90 11.93
-6 -1 -3 373.91 13.90
-6 1 -3 374.92 14.43
-6 -1 -3 350.55 12.74
-6 1 -3 345.54 12.38
-6 1 3 341.31 13.39
-6 -1 3 361.06 13.49
-4 1 -3 1037.01 23.99
-4 1 3 985.25 23.93
-4 -1 -3 1054.52 22.63
-4 1 -3 1106.68 22.91
-4 -1 3 1051.84 22.51
-4 -1 -3 981.19 22.67
-4 -1 3 1022.87 20.88
-4 1 3 1021.66 21.36
-4 1 3 1078.52 22.75
-4 -1 3 1044.03 22.52
-2 -1 3 1121.59 22.67
-2 1 -3 1118.07 21.83
-2 -1 -3 1090.90 22.45
-2 1 -3 1087.37 22.53
-2 -1 3 1122.35 21.86
-2 1 3 1097.82 22.55
0 1 3 1578.70 31.15
0 1 3 1615.72 30.86
0 -1 -3 1668.52 31.79
0 -1 3 1556.13 30.93
0 1 -3 1650.04 31.80
2 -1 3 1079.45 21.99
2 1 3 1070.18 21.86
2 -1 -3 1100.57 22.16
2 1 -3 1085.55 22.13
4 1 -3 1052.99 25.08
4 -1 -3 1001.17 24.53
4 1 -3 1002.91 22.34
4 1 3 1001.54 21.95
4 -1 3 1048.81 22.75
6 -1 -3 345.51 13.49
6 1 -3 357.58 14.04
8 -1 -3 375.40 10.54
-7 -1 -4 3.95 2.74
-7 1 4 4.90 4.04
-7 -1 -4 2.95 4.03
-7 1 -4 4.84 3.05
-7 -1 4 2.31 2.96
-7 -1 4 5.26 3.86
-5 -1 -4 62.65 5.82
-5 1 4 61.99 4.06
-5 -1 4 54.57 5.42
-5 1 -4 56.31 5.99
-5 1 4 65.52 5.49
-5 1 4 53.74 5.61
-5 -1 4 59.44 3.95
-5 -1 4 57.27 5.92
-5 1 -4 65.02 5.02
-5 -1 -4 53.39 3.80
-5 1 -4 62.67 4.21
-5 -1 -4 63.09 5.19
-5 1 4 55.74 2.80
-5 -1 -4 60.46 4.11
-3 1 -4 15.28 1.05
-3 1 4 11.05 1.43
-3 -1 4 11.85 1.19
-3 -1 -4 14.59 1.91
-3 1 -4 15.01 1.95
-3 1 4 15.23 1.83
-3 -1 4 13.73 1.90
-1 1 4 37.25 1.64
-1 -1 -4 41.45 2.22
-1 -1 4 36.36 2.21
-1 1 -4 39.31 2.17
-1 1 -4 38.34 1.54
-1 1 4 39.72 1.90
-1 1 -4 37.09 2.23
1 -1 -4 38.98 2.27
1 1 -4 38.03 1.57
1 1 4 37.61 1.22
1 -1 4 36.33 1.57
3 -1 4 12.20 1.62
3 1 4 12.70 1.66
3 1 -4 16.85 1.91
3 -1 4 16.11 1.97
5 1 -4 65.45 6.08
5 -1 4 66.77 4.58
5 1 -4 58.82 3.92
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2 -6 -8 31.76 3.95
2 -6 -8 26.67 3.25
2 -6 8 30.87 3.95
4 -6 -8 872.05 19.28
4 -6 -8 838.96 18.90
4 -6 8 887.08 19.67
4 -6 8 874.54 19.65
-3 6 -9 47.12 3.05
-3 6 -9 44.34 3.39
-1 -6 9 12.39 3.37
-1 -6 9 8.29 2.52
-1 6 -9 9.43 3.07
-1 -6 9 9.71 2.76
-1 -6 -9 7.45 2.93
1 -6 -9 9.02 2.83
1 -6 9 8.28 2.87
1 -6 9 8.02 2.70
1 -6 9 9.47 2.87
1 -6 -9 8.32 2.89
3 6 -9 45.06 3.10
3 -6 -9 42.62 3.18
3 -6 9 46.63 3.29
-2 6 -10 25.65 2.79
-2 -6 10 24.11 2.90
0 -6 10 323.31 9.73
0 6 -10 315.81 9.73
0 -6 -10 315.35 9.17
0 -6 10 306.20 9.24
0 6 -10 324.61 9.96
0 -6 10 288.30 8.58
0 -6 -10 327.54 9.57
0 -6 10 327.92 9.98
2 -6 10 26.46 2.41
2 6 -10 25.58 2.94
2 -6 -10 23.61 2.50
2 -6 -10 27.29 2.86
2 -6 10 26.65 2.83
2 6 -10 26.61 2.81
2 -6 10 21.88 2.36
2 -6 10 22.11 2.94
-1 6 -11 314.70 8.32
-1 -6 11 321.47 8.32
-1 -6 11 342.63 9.08
1 6 -11 340.66 9.33
1 -6 -11 347.57 9.04
1 -6 11 329.97 9.03
1 -6 11 354.01 9.49
3 -6 11 29.06 1.56
0 6 -12 483.06 10.71
0 -6 12 459.48 10.51
-5 -7 0 2.16 1.23
-5 7 0 0.37 1.34
-3 -7 0 -0.10 2.30
-3 7 0 -0.30 2.13
-3 -7 0 0.84 2.99
-1 -7 0 -0.69 2.66
-1 -7 0 0.31 2.97
1 -7 0 2.11 3.19
1 -7 0 0.49 3.36
1 -7 0 -0.91 2.53
1 -7 0 0.93 3.12
3 -7 0 3.06 2.85
3 -7 0 -0.29 3.16
3 -7 0 -0.10 2.11
5 -7 0 0.75 1.59
-4 -7 -1 42.13 3.01
-4 -7 1 42.41 3.27
-4 7 -1 46.26 3.23
-4 7 1 48.47 3.20
-4 -7 -1 47.67 3.75
-2 -7 1 1338.80 30.22
-2 -7 -1 1354.08 30.48
-2 -7 1 1338.44 31.07
0 -7 -1 27.21 4.26
0 -7 1 28.38 4.39
0 -7 -1 23.65 3.18
0 -7 1 23.85 3.70
0 -7 1 24.09 3.95
0 -7 -1 29.22 4.20
2 -7 -1 1352.72 29.67
2 -7 -1 1305.10 29.99
2 -7 -1 1307.95 30.17
2 -7 1 1283.70 30.25
2 -7 1 1293.48 29.29
2 -7 1 1257.22 29.20
4 -7 -1 48.84 3.54
4 -7 -1 41.53 3.75
4 -7 1 44.28 3.81
4 -7 1 41.30 2.88
-5 -7 2 118.54 4.07
-5 7 -2 123.97 3.93
-5 7 2 119.16 3.77
-3 -7 2 167.64 6.64
-3 7 -2 167.31 6.19
-3 7 2 174.22 6.13
-3 7 -2 169.01 6.27
-3 -7 -2 176.92 6.92
-1 -7 2 265.96 9.71
-1 -7 2 247.13 9.43
-1 -7 -2 252.56 8.67
1 -7 -2 266.58 9.62
1 -7 2 272.18 9.83
1 -7 -2 253.36 9.60
1 -7 2 257.88 9.81
1 -7 2 254.36 9.35
3 -7 -2 168.59 6.60
3 -7 -2 180.24 7.39
3 -7 -2 172.59 7.28
3 -7 2 172.48 7.38
3 -7 2 162.88 6.80
5 -7 -2 117.15 3.76
5 -7 -2 122.81 4.09
5 -7 2 123.32 4.23
-4 -7 3 57.34 3.53
-4 7 -3 59.40 3.26
-4 7 3 58.21 3.14
-4 7 -3 53.98 3.17
-4 -7 3 55.36 4.06
-2 -7 3 649.60 16.42
-2 7 -3 627.29 16.17
-2 -7 -3 618.90 15.69
0 -7 3 53.78 5.05
0 -7 -3 52.88 4.84
0 -7 -3 52.76 4.66
0 -7 3 56.89 4.92
0 7 -3 53.17 4.16
0 -7 3 59.87 4.94
2 -7 -3 658.19 17.02
2 -7 3 661.06 16.66
2 -7 -3 653.79 17.23
2 -7 -3 644.17 16.86
2 -7 3 618.61 16.95
2 -7 3 613.52 16.85
4 -7 -3 53.87 2.88
4 -7 -3 58.25 3.77
4 -7 -3 53.87 3.47
4 -7 3 56.99 3.70
4 -7 3 52.46 3.50
-3 7 -4 403.00 10.59
-3 7 -4 403.29 11.35
-3 -7 4 429.07 12.31
-1 -7 4 458.07 13.27
-1 7 -4 436.42 12.55
-1 -7 4 417.16 12.00
1 -7 4 465.79 13.26
1 -7 -4 443.35 13.14
1 7 -4 430.98 12.51
1 -7 -4 426.52 12.43
1 -7 4 436.44 12.78
1 -7 4 425.54 13.05
1 -7 4 415.70 11.84
3 -7 -4 409.03 11.46
3 7 -4 387.84 10.79
3 -7 -4 413.24 11.92
3 -7 -4 405.57 11.14
3 -7 4 422.57 11.56
3 -7 4 413.83 11.87
5 -7 -4 199.68 5.10
-4 -7 5 439.69 10.94
-4 7 -5 461.52 10.39
-4 -7 5 459.13 10.99
-2 -7 5 158.76 6.34
-2 7 -5 170.89 6.79
-2 -7 5 153.90 6.30
0 -7 5 471.24 13.58
0 -7 -5 442.89 12.98
0 7 -5 449.49 12.98
0 -7 5 459.02 13.41
0 -7 5 420.49 12.27
2 -7 5 158.84 6.38
2 -7 -5 164.30 6.87
2 -7 -5 160.52 6.84
2 7 -5 157.11 6.45
2 -7 -5 149.19 5.84
2 -7 5 163.31 6.37
2 -7 5 149.46 6.01
4 -7 -5 436.54 10.08
4 -7 5 459.82 10.91
-3 7 -6 208.35 7.01
-3 -7 6 216.35 7.07
-1 -7 6 174.76 7.03
-1 7 -6 180.89 7.17
-1 -7 6 182.05 7.51
-1 -7 6 174.34 6.84
1 -7 6 188.80 7.29
1 7 -6 182.69 7.25
1 -7 6 178.40 7.39
1 -7 6 169.23 6.73
3 -7 -6 204.87 6.83
3 7 -6 197.15 6.59
3 -7 -6 207.81 6.84
3 -7 6 192.34 6.21
-4 -7 7 481.15 10.58
-2 -7 7 43.40 3.07
-2 7 -7 49.61 3.55
-2 -7 7 52.26 3.68
-2 -7 7 53.54 3.55
0 -7 7 1074.31 23.95
0 -7 -7 1003.51 23.14
0 7 -7 1048.31 23.87
0 -7 7 1009.00 23.71
0 -7 7 1005.87 23.27
2 -7 7 42.44 3.10
2 7 -7 47.52 3.42
2 -7 7 48.63 3.73
2 -7 7 50.62 3.38
4 -7 -7 493.21 10.70
4 -7 7 522.68 11.22
-1 -7 8 10.85 2.40
-1 7 -8 10.74 2.42
-1 -7 8 10.92 2.24
1 -7 8 10.66 2.28
1 -7 -8 14.11 2.44
1 7 -8 6.17 2.20
1 -7 8 11.64 2.55
1 -7 8 13.48 2.36
3 -7 8 19.23 1.92
3 -7 8 17.46 1.65
0 -7 9 1258.67 26.77
0 7 -9 1282.41 26.93
0 -7 9 1232.44 26.59
2 7 -9 27.46 1.98
2 -7 -9 29.56 2.02
2 -7 9 24.32 1.88
2 -7 9 26.63 2.11
1 7 -10 23.62 1.81
1 -7 10 23.28 1.75
-2 -8 0 31.56 2.84
0 -8 0 1497.86 31.48
2 -8 0 34.82 3.33
-3 -8 -1 80.63 3.42
-3 -8 1 85.11 3.79
-1 -8 -1 18.80 2.41
-1 -8 1 17.65 2.73
-1 -8 1 17.03 2.78
1 -8 1 19.39 2.42
1 -8 1 22.47 2.87
1 -8 -1 19.94 3.15
1 -8 1 21.25 3.15
3 -8 -1 86.78 3.89
3 -8 1 80.66 3.86
-2 -8 2 41.41 3.30
0 -8 2 225.24 7.43
0 -8 2 250.07 8.20
2 -8 -2 39.63 3.19
2 -8 2 38.13 3.23
2 -8 2 40.41 2.80
4 -8 2 346.38 7.66
-3 -8 3 40.06 2.68
-1 -8 3 77.75 4.13
1 -8 3 81.16 4.23
1 -8 3 70.76 4.00
3 -8 -3 39.68 2.34
3 -8 3 39.31 2.45
3 -8 3 36.01 2.18
-2 -8 4 299.17 8.43
0 -8 4 171.93 6.20
0 -8 4 156.84 5.94
2 -8 4 281.18 7.86
-3 -8 5 68.90 2.58
-1 -8 5 246.79 7.25
1 -8 5 254.39 7.30
1 -8 5 233.53 7.26
3 -8 5 66.25 2.53
-2 -8 6 191.45 5.37
0 -8 6 156.55 5.30
2 8 -6 125.83 3.48
-1 -8 7 6.86 1.34
1 8 -7 7.34 1.42
1 -8 7 8.96 1.49
TITL ico3a_auto in Ima2
REM Ima2 (#46, found as I2mb in bca setting)
CELL 1.54184 7.202366 12.798316 6.693553 90.0000 90.0000 90.0000
ZERR 4.00 0.000129 0.000220 0.000117 0.0000 0.0000 0.0000
LATT -2
SYMM -x,-y, z
SYMM x+1/2,-y, z
SYMM -x+1/2, y, z
SFAC C H N Cl Co
UNIT 16.00 16.00 8.00 8.00 4.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 43075
_shelx_res_file
;
TITL ico3a_auto_a.res in Imma
ico3a.res
created by SHELXL-2016/6 at 08:20:22 on 07-Jul-2023
REM Old TITL ico3a_auto in Ima2
REM SHELXT solution in Imma
REM R1 0.053, Rweak 0.016, Alpha 0.030, Orientation a'=c, b'=a, c'=b
REM Formula found by SHELXT: C4 N2 Cl2 Co
CELL 1.54184 6.6935 7.2024 12.7978 90 90 90
ZERR 4 0.0001 0.0001 0.0002 0 0 0
LATT 2
SYMM -X,0.5-Y,+Z
SYMM -X,0.5+Y,-Z
SYMM +X,-Y,-Z
SFAC C H Cl Co N
UNIT 16 16 8 4 8
L.S. 10
PLAN 5
TEMP -173
fmap 2
acta
BOND $H
HTAB
EQIV $4 x-1/2, y-1/2, z+1/2
HTAB C2 Cl1_$4
EQIV $5 -x+1/2, -y+1, z+1/2
HTAB C2 Cl1_$5
REM
REM
REM
WGHT 0.039000 0.961800
EXTI 0.001641
FVAR 0.51709
CO1 4 0.250000 0.250000 0.250000 10.25000 0.00364 0.01106 =
0.00616 0.00000 -0.00030 0.00000
CL1 3 0.500000 0.478038 0.191177 10.50000 0.00600 0.01080 =
0.00986 0.00073 0.00000 0.00000
N1 5 0.399124 0.250000 0.396865 10.50000 0.00521 0.01069 =
0.00867 0.00000 0.00005 0.00000
C1 1 0.302513 0.250000 0.487654 10.50000 0.00757 0.01836 =
0.01185 0.00000 0.00202 0.00000
AFIX 43
H1 2 0.160605 0.250000 0.486369 10.50000 -1.20000
AFIX 0
C2 1 0.397346 0.250000 0.584522 10.50000 0.01032 0.01422 =
0.00901 0.00000 -0.00046 0.00000
AFIX 43
H2 2 0.323309 0.250000 0.647854 10.50000 -1.20000
AFIX 0
HKLF 4
REM ico3a_auto_a.res in Imma
REM R1 = 0.0203 for 386 Fo > 4sig(Fo) and 0.0206 for all 395 data
REM 30 parameters refined using 0 restraints
END
WGHT 0.0390 0.9618
REM Instructions for potential hydrogen bonds
HTAB C2 Cl1_$4
HTAB C2 Cl1_$5
REM Highest difference peak 0.638, deepest hole -0.338, 1-sigma level 0.091
Q1 1 0.1312 0.2500 0.2401 10.50000 0.05 0.64
Q2 1 0.6167 0.4733 0.1907 11.00000 0.05 0.40
Q3 1 0.6236 0.3822 0.2160 11.00000 0.05 0.39
Q4 1 0.5000 0.2500 0.5887 10.25000 0.05 0.39
Q5 1 0.5000 0.2500 0.3950 10.25000 0.05 0.31
;
_shelx_res_checksum 53006
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, 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 0.250000 0.250000 0.250000 0.0069(2) Uani d 1 . .
Cl Cl1 0.500000 0.47804(8) 0.19118(4) 0.0089(2) Uani d 1 . .
N N1 0.3991(3) 0.250000 0.39687(15) 0.0082(4) Uani d 1 . .
C C1 0.3025(4) 0.250000 0.48765(19) 0.0126(5) Uani d 1 . .
H H1 0.160605 0.250000 0.486369 0.015 Uiso calc 1 . .
C C2 0.3973(4) 0.250000 0.58452(17) 0.0112(5) Uani d 1 . .
H H2 0.323309 0.250000 0.647854 0.013 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 0.0036(3) 0.0111(3) 0.0062(3) 0.000 -0.00030(17) 0.000
Cl1 0.0060(3) 0.0108(3) 0.0099(3) 0.000 0.000 0.00073(17)
N1 0.0052(9) 0.0107(9) 0.0087(8) 0.000 0.0001(7) 0.000
C1 0.0076(11) 0.0184(12) 0.0118(11) 0.000 0.0020(10) 0.000
C2 0.0103(12) 0.0142(11) 0.0090(11) 0.000 -0.0005(9) 0.000
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'
Cl Cl 0.3639 0.7018 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Co1 N1 . 13 180.0 y
N1 Co1 Cl1 . . 87.21(4) y
N1 Co1 Cl1 13 . 92.79(4) y
N1 Co1 Cl1 . 13 92.79(4) ?
N1 Co1 Cl1 13 13 87.21(4) ?
Cl1 Co1 Cl1 . 13 180.0 y
N1 Co1 Cl1 . 2_655 87.21(4) ?
N1 Co1 Cl1 13 2_655 92.79(4) n
Cl1 Co1 Cl1 . 2_655 83.66(2) y
Cl1 Co1 Cl1 13 2_655 96.34(2) y
N1 Co1 Cl1 . 14_455 92.79(4) ?
N1 Co1 Cl1 13 14_455 87.21(4) ?
Cl1 Co1 Cl1 . 14_455 96.34(2) ?
Cl1 Co1 Cl1 13 14_455 83.66(2) ?
Cl1 Co1 Cl1 2_655 14_455 180.0 ?
Co1 Cl1 Co1 . 2_655 85.611(17) ?
C1 N1 N1 . 2_655 119.10(15) ?
C1 N1 Co1 . . 122.93(17) ?
N1 N1 Co1 2_655 . 117.97(5) ?
N1 C1 C2 . . 123.8(3) ?
N1 C1 H1 . . 118.1 ?
C2 C1 H1 . . 118.1 ?
C2 C2 C1 2_655 . 117.11(16) ?
C2 C2 H2 2_655 . 121.4 ?
C1 C2 H2 . . 121.4 ?
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 N1 . 2.1282(19) y
Co1 N1 13 2.1282(19) ?
Co1 Cl1 . 2.4626(4) y
Co1 Cl1 13 2.4626(4) ?
Co1 Cl1 2_655 2.4626(4) ?
Co1 Cl1 14_455 2.4626(4) ?
N1 C1 . 1.330(3) ?
N1 N1 2_655 1.350(4) ?
C1 C2 . 1.393(3) ?
C1 H1 . 0.9500 ?
C2 C2 2_655 1.374(5) ?
C2 H2 . 0.9500 ?
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
C2 H2 Cl1 5_445 0.95 2.97 3.574(2) 123
_cod_database_fobs_code 2022856