#------------------------------------------------------------------------------
#$Date: 2023-12-07 12:52:16 +0100 (Thu, 07 Dec 2023) $
#$Revision: 288152 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022869.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_2022869
loop_
_publ_author_name
'Näther, Christian'
'Jess, Inke'
_publ_section_title
;
Synthesis, crystal structure and reactivity of
bis-(μ-2-methyl-pyridine
N-oxide-κ2O:O)bis-[di-bromido-(2-methyl-pyridine
N-oxide-κO)cobalt(II)] butanol monosolvate.
;
_journal_coeditor_code PK2697
_journal_issue 'Pt 11'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 972
_journal_page_last 976
_journal_paper_doi 10.1107/S2056989023008228
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '[Co2 Br4 (C6 H7 N1 O1)4], C4 H10 O'
_chemical_formula_moiety 'C24 H28 Br4 Co2 N4 O4, C4 H10 O'
_chemical_formula_sum 'C28 H38 Br4 Co2 N4 O5'
_chemical_formula_weight 948.12
_chemical_name_systematic
;
Bis(\m-2-methylpyridine
N-oxide-\k^2^O:O)bis[dibromido(2-methylpyridine
N-oxide-\kO)cobalt(II)] butanol monosolvate
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_cell_angle_alpha 70.2420(10)
_cell_angle_beta 76.0040(10)
_cell_angle_gamma 83.8600(10)
_cell_formula_units_Z 1
_cell_length_a 8.09000(10)
_cell_length_b 9.57720(10)
_cell_length_c 12.24000(10)
_cell_measurement_reflns_used 14929
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 79.8620
_cell_measurement_theta_min 3.9240
_cell_volume 865.693(17)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/4 (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 0.995
_diffrn_measured_fraction_theta_max 0.977
_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 CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0208
_diffrn_reflns_av_unetI/netI 0.0121
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 18480
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 80.199
_diffrn_reflns_theta_min 3.934
_exptl_absorpt_coefficient_mu 13.256
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.72139
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour 'dark blue'
_exptl_crystal_density_diffrn 1.819
_exptl_crystal_description block
_exptl_crystal_F_000 468
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.502
_refine_diff_density_min -0.590
_refine_ls_extinction_coef 0.00106(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.092
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 204
_refine_ls_number_reflns 3705
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.093
_refine_ls_R_factor_all 0.0245
_refine_ls_R_factor_gt 0.0244
_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^)+(0.0306P)^2^+1.2686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0648
_refine_ls_wR_factor_ref 0.0649
_reflns_number_gt 3686
_reflns_number_total 3705
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file pk2697sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2022869.cif.'
_cod_original_cell_volume 865.69(2)
_cod_database_code 2022869
_cod_database_fobs_code 2022869
_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 0.241
_shelx_estimated_absorpt_t_max 0.692
_shelx_hkl_file
;
0 0 -1 1660.66 21.40
0 0 -1 1651.86 21.32
0 0 -1 1651.43 21.12
0 0 -1 1676.48 21.31
0 0 2 68.00 1.80
0 0 2 65.84 1.62
0 0 -2 70.89 1.81
0 0 2 63.29 1.83
0 0 2 67.43 1.80
0 0 -2 77.06 1.74
0 0 -2 73.21 1.92
0 0 -2 74.99 1.49
0 0 -2 77.40 1.75
0 0 3 6038.36 80.31
0 0 3 6177.35 79.89
0 0 -3 6259.89 80.15
0 0 3 6166.02 80.64
0 0 3 6131.38 80.27
0 0 3 6058.40 79.46
0 0 -3 6380.33 79.91
0 0 -3 6061.41 79.34
0 0 -3 6422.75 80.54
0 0 -3 6288.92 79.98
0 0 4 1369.16 19.83
0 0 4 1349.61 19.16
0 0 -4 1309.40 19.41
0 0 4 1331.23 19.70
0 0 4 1383.74 20.18
0 0 4 1325.51 18.40
0 0 -4 1386.21 19.98
0 0 -4 1399.17 19.35
0 0 5 37.70 2.18
0 0 5 40.64 1.92
0 0 5 38.01 1.31
0 0 5 43.00 2.35
0 0 -5 40.68 2.08
0 0 5 38.73 2.44
0 0 -5 36.48 1.93
0 0 -5 35.96 2.18
0 0 6 8.96 1.63
0 0 6 7.13 1.76
0 0 -6 6.07 1.22
0 0 -6 7.77 1.67
0 0 -6 4.74 1.66
0 0 7 376.11 9.03
0 0 7 391.71 9.82
0 0 -7 390.60 9.26
0 0 -7 389.83 9.50
0 0 -8 435.60 10.85
0 0 -8 453.99 11.54
0 0 8 429.67 11.25
0 0 9 187.03 5.03
0 0 9 175.15 4.68
0 0 9 197.36 4.89
0 0 9 186.01 4.57
0 0 9 178.25 4.60
0 0 9 179.43 4.53
0 0 9 190.74 4.87
0 0 -9 165.71 6.91
0 0 -9 162.69 7.39
0 0 9 174.24 4.65
0 0 10 446.91 8.62
0 0 10 454.22 8.40
0 0 10 436.17 8.45
0 0 10 456.79 8.42
0 0 10 431.52 8.37
0 0 10 450.33 8.60
0 0 10 433.30 8.02
0 0 10 440.49 8.77
0 0 11 921.23 14.83
0 0 11 956.02 15.35
0 0 11 936.82 14.94
0 0 11 927.96 14.38
0 0 11 919.91 14.78
0 0 11 949.58 14.87
0 0 11 970.31 14.88
0 0 11 949.35 15.04
0 0 12 160.02 4.37
0 0 12 175.59 4.81
0 0 12 170.22 4.45
0 0 12 166.16 4.03
0 0 12 170.78 4.56
0 0 12 170.38 4.50
0 0 12 163.17 4.23
0 0 12 168.69 4.61
0 0 13 233.06 4.75
0 0 13 241.25 4.91
0 0 13 241.68 4.95
0 0 13 237.44 5.05
0 0 13 235.02 4.71
0 0 14 260.90 4.41
0 0 14 251.53 4.30
0 0 14 267.25 4.44
0 0 14 257.40 4.14
0 -1 13 23.40 1.37
0 -1 13 25.05 1.81
0 -1 13 25.69 1.70
0 -1 13 24.44 1.63
0 -1 12 376.91 6.98
0 -1 12 408.32 7.34
0 -1 12 399.49 7.29
0 -1 12 402.98 7.48
0 -1 12 409.50 7.75
0 -1 12 411.06 7.54
0 -1 12 397.21 7.40
0 -1 11 269.31 5.91
0 -1 11 277.95 6.31
0 -1 11 278.73 6.32
0 -1 11 280.72 6.16
0 -1 11 290.76 6.65
0 -1 11 273.30 6.05
0 -1 11 278.28 6.29
0 -1 11 289.12 6.47
0 -1 10 4.09 2.55
0 -1 10 5.73 1.75
0 -1 10 5.56 2.10
0 -1 10 4.41 2.38
0 -1 10 6.33 2.33
0 -1 10 6.76 2.25
0 -1 10 7.57 2.23
0 -1 10 6.22 2.41
0 -1 10 9.65 2.21
0 -1 10 4.05 2.18
0 -1 10 3.39 1.76
0 -1 10 4.64 1.56
0 -1 9 11.45 2.34
0 -1 9 6.59 1.94
0 -1 9 4.90 2.05
0 -1 9 5.89 2.04
0 -1 9 6.56 2.13
0 -1 9 8.84 2.03
0 -1 9 3.53 2.13
0 -1 9 7.63 1.51
0 -1 9 5.69 1.61
0 -1 9 4.25 2.04
0 1 -9 4.64 2.84
0 -1 9 5.25 2.11
0 1 -8 38.58 3.92
0 1 -8 38.45 3.42
0 -1 8 40.74 3.47
0 -1 8 44.06 2.53
0 1 -7 726.37 14.62
0 1 -7 721.17 15.40
0 -1 7 754.49 11.77
0 -1 7 773.19 14.95
0 1 -6 345.94 8.67
0 1 -6 329.90 8.03
0 -1 6 312.74 6.94
0 -1 6 332.75 6.00
0 -1 6 342.77 8.27
0 -1 6 348.27 8.03
0 -1 6 346.13 8.61
0 1 -5 27.99 1.82
0 1 -5 32.09 2.47
0 1 -5 27.16 2.16
0 -1 5 33.25 2.28
0 -1 5 32.11 1.85
0 -1 5 33.18 2.49
0 -1 5 27.52 2.08
0 1 -4 6222.19 81.07
0 1 -4 5925.84 80.43
0 1 -4 6040.01 79.83
0 -1 4 6118.34 79.79
0 -1 4 6049.00 80.72
0 -1 4 6089.16 80.98
0 -1 4 6275.48 80.53
0 -1 3 2927.81 39.67
0 1 -3 2962.20 38.42
0 -1 3 2894.27 38.47
0 1 -3 3083.18 40.67
0 1 -3 3021.45 40.17
0 1 -3 3100.86 39.82
0 -1 3 3024.36 40.46
0 -1 3 3043.81 40.40
0 -1 3 3036.77 40.13
0 1 -2 20.38 0.81
0 -1 2 18.94 0.85
0 1 -2 20.50 1.26
0 1 -2 18.50 1.08
0 -1 2 19.83 1.16
0 1 -1 2053.34 27.08
0 1 -1 2125.30 27.40
0 1 -1 2106.93 27.20
0 1 0 4187.91 55.03
0 1 0 4266.72 54.74
0 1 0 4362.98 55.11
0 1 0 4204.25 54.55
0 -1 -1 26.97 1.03
0 1 1 33.23 1.17
0 1 2 1918.61 25.77
0 -1 -2 1901.30 25.80
0 -1 -2 2011.91 26.35
0 -1 -2 2022.94 26.54
0 1 2 1952.94 26.34
0 1 3 187.08 3.13
0 -1 -3 185.84 3.96
0 -1 -3 179.78 4.12
0 1 3 187.27 3.85
0 1 3 197.28 4.04
0 -1 -4 2152.93 28.58
0 1 4 2186.16 28.45
0 1 4 2271.01 30.51
0 1 4 2338.44 31.10
0 1 4 2302.65 30.42
0 -1 -4 2286.20 31.06
0 -1 -4 2188.84 30.81
0 -1 -4 2211.02 30.34
0 1 5 468.40 8.67
0 -1 -5 479.02 9.05
0 1 5 477.90 8.25
0 1 5 481.67 9.27
0 -1 -5 436.43 8.65
0 -1 -5 435.03 8.33
0 -1 -5 448.06 9.26
0 1 6 295.63 7.04
0 1 6 318.95 7.74
0 1 6 307.70 6.12
0 -1 -6 312.04 7.37
0 -1 -6 301.66 7.61
0 -1 -6 293.45 6.63
0 1 7 485.00 8.28
0 -1 -7 494.86 10.63
0 1 7 502.43 11.44
0 -1 -7 520.62 11.28
0 -1 -7 513.97 11.44
0 -1 -7 507.18 9.99
0 1 8 817.81 13.02
0 1 8 850.60 17.17
0 -1 -8 855.69 16.89
0 -1 -8 833.91 16.76
0 1 9 138.50 4.14
0 -1 -9 126.83 6.20
0 1 9 139.06 6.60
0 1 10 1417.22 20.79
0 1 10 1390.71 20.40
0 1 10 1490.74 21.68
0 1 10 1417.31 21.11
0 1 10 1456.91 21.03
0 1 10 1457.49 21.19
0 1 10 1415.78 20.93
0 1 10 1374.37 20.70
0 1 10 1443.31 20.91
0 1 10 1473.81 21.32
0 1 10 1411.57 20.71
0 1 10 1432.91 20.94
0 -1 -10 1255.97 25.47
0 -1 -10 1309.50 26.58
0 1 10 1379.53 26.67
0 1 11 601.34 10.82
0 1 11 640.90 10.94
0 1 11 611.06 10.43
0 1 11 637.67 10.79
0 1 11 625.00 10.92
0 1 11 610.81 10.78
0 1 11 653.98 11.40
0 1 11 620.03 10.98
0 1 11 611.13 10.62
0 1 11 636.16 10.53
0 1 11 595.06 10.13
0 1 12 196.67 5.13
0 1 12 197.69 5.16
0 1 12 213.38 5.14
0 1 12 208.20 5.42
0 1 12 211.95 5.19
0 1 12 199.30 4.83
0 1 12 207.07 4.82
0 1 12 207.74 5.18
0 1 13 430.18 7.76
0 1 13 411.55 7.16
0 1 13 418.07 7.16
0 1 13 433.72 7.61
0 1 13 435.33 7.61
0 1 13 430.67 7.63
0 1 13 449.02 7.62
0 1 14 49.80 1.96
0 1 14 49.18 1.81
0 1 14 45.41 1.84
0 1 14 49.29 1.82
0 -2 13 36.42 1.40
0 -2 13 35.46 1.39
0 -2 12 226.02 4.58
0 -2 12 231.35 4.87
0 -2 12 230.07 4.78
0 -2 12 227.71 4.76
0 -2 12 213.53 4.05
0 -2 11 11.67 2.33
0 -2 11 11.12 2.10
0 -2 11 10.04 2.25
0 -2 11 10.81 1.70
0 -2 11 13.97 1.75
0 -2 11 11.80 2.42
0 -2 11 13.82 2.16
0 -2 10 103.65 3.40
0 -2 10 99.38 3.15
0 -2 10 109.55 3.62
0 -2 10 102.90 3.76
0 -2 10 108.85 3.96
0 -2 10 99.57 4.04
0 -2 10 99.44 3.76
0 -2 10 110.81 3.62
0 -2 10 106.42 3.98
0 -2 10 101.79 3.26
0 -2 10 105.73 4.13
0 -2 9 17.71 2.64
0 -2 9 17.40 2.31
0 -2 9 25.28 2.04
0 -2 9 18.58 2.39
0 -2 9 19.97 2.41
0 -2 9 18.55 2.45
0 -2 9 22.64 2.31
0 -2 9 20.85 2.04
0 -2 9 19.96 2.12
0 -2 9 17.07 2.50
0 -2 9 18.81 1.98
0 -2 8 307.41 6.50
0 -2 8 304.29 6.22
0 -2 8 298.13 6.08
0 -2 8 308.58 6.36
0 -2 8 319.43 6.58
0 -2 8 329.33 6.42
0 -2 8 297.02 6.12
0 -2 8 312.29 6.70
0 -2 8 312.41 6.36
0 -2 8 297.87 9.30
0 -2 8 311.89 6.83
0 2 -8 278.59 9.75
0 2 -7 1744.41 29.74
0 -2 7 1785.76 29.22
0 -2 7 1768.44 24.61
0 -2 7 1676.33 27.87
0 2 -6 143.30 5.93
0 -2 6 144.69 3.50
0 -2 6 149.16 5.73
0 -2 6 144.04 5.16
0 2 -5 2542.51 36.70
0 2 -5 2644.25 38.43
0 -2 5 2544.90 36.49
0 -2 5 2639.39 38.19
0 -2 5 2625.12 37.39
0 -2 4 5420.89 70.46
0 2 -4 5556.96 72.00
0 2 -4 5338.06 70.63
0 -2 4 5422.49 70.99
0 -2 4 5562.44 71.73
0 -2 3 529.64 8.53
0 2 -3 560.26 8.43
0 2 -3 537.66 9.94
0 2 -3 539.30 9.32
0 -2 3 551.58 9.53
0 -2 2 5716.10 72.14
0 2 -2 5692.68 71.99
0 2 -2 5861.65 72.95
0 2 -2 5751.04 72.53
0 -2 1 3729.34 47.35
0 2 -1 3673.12 47.25
0 -2 1 3705.12 48.10
0 2 -1 3461.23 45.70
0 2 -1 3667.77 47.36
0 -2 1 3436.91 45.67
0 2 -1 3592.63 46.17
0 2 0 50.70 1.97
0 -2 0 43.20 1.99
0 2 0 39.57 1.43
0 -2 0 41.26 1.49
0 2 0 51.21 1.71
0 2 1 335.52 6.36
0 -2 -1 372.68 6.59
0 2 1 348.96 5.94
0 2 1 350.35 6.25
0 2 1 365.81 6.35
0 -2 -1 339.72 6.12
0 -2 -2 2878.10 38.78
0 2 2 2895.87 38.82
0 2 3 3317.81 45.62
0 2 3 3309.52 44.87
0 -2 -3 3199.78 44.83
0 2 4 988.31 15.62
0 -2 -4 968.45 15.79
0 -2 -4 1066.02 16.20
0 -2 -4 1043.79 15.81
0 -2 -4 920.39 14.37
0 2 4 969.04 14.37
0 2 5 2.29 1.29
0 -2 -5 2.17 1.52
0 2 5 2.72 1.37
0 -2 -5 1.31 1.30
0 -2 -5 2.59 0.75
0 2 5 2.26 0.69
0 -2 -6 3671.69 52.52
0 -2 -6 3692.83 51.87
0 2 6 3712.33 50.85
0 -2 -6 3637.33 51.96
0 2 6 3734.77 52.11
0 2 7 3857.55 51.43
0 -2 -7 4009.07 56.36
0 -2 -7 3816.89 54.27
0 2 7 4101.38 56.09
0 2 7 3877.46 53.61
0 -2 -7 3920.77 55.65
0 2 8 711.09 11.36
0 -2 -8 700.68 15.48
0 2 8 741.31 15.55
0 -2 -8 718.59 15.01
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0 2 9 481.11 12.69
0 -2 -9 452.77 12.42
0 -2 -9 437.32 12.18
0 2 10 911.05 19.80
0 -2 -10 839.65 19.17
0 -2 -10 872.71 19.49
0 2 10 911.84 14.27
0 2 10 874.51 13.97
0 2 10 940.10 14.65
0 2 10 955.30 14.83
0 2 10 955.10 14.93
0 2 10 931.68 14.46
0 2 10 909.80 14.37
0 2 10 940.72 14.30
0 2 10 902.89 14.12
0 2 10 896.75 13.93
0 2 10 872.38 14.48
0 2 11 11.49 2.46
0 2 11 10.30 2.32
0 2 11 10.21 2.31
0 2 11 13.68 2.23
0 2 11 8.74 2.15
0 2 11 7.76 1.82
0 2 11 8.13 1.88
0 2 11 8.11 2.22
0 2 11 7.72 1.99
0 2 11 7.62 2.27
0 2 12 389.51 7.54
0 2 12 375.84 7.46
0 2 12 378.97 7.43
0 2 12 368.64 7.54
0 2 12 390.70 7.56
0 2 12 354.54 6.81
0 2 12 364.95 7.21
0 2 12 384.08 7.79
0 2 13 39.34 2.36
0 2 13 42.12 2.53
0 2 13 35.76 2.55
0 2 13 37.52 2.32
0 2 13 40.11 2.60
0 2 13 38.10 2.24
0 2 14 19.06 1.59
0 2 14 16.07 1.61
0 2 14 16.15 1.65
0 -3 12 107.50 2.58
0 -3 12 115.25 2.77
0 -3 12 109.51 2.75
0 -3 12 113.44 2.66
0 -3 11 157.86 3.93
0 -3 11 152.47 3.61
0 -3 11 152.50 3.91
0 -3 11 163.96 4.10
0 -3 11 148.64 3.57
0 -3 10 51.35 2.59
0 -3 10 50.46 2.39
0 -3 10 53.09 2.74
0 -3 10 54.89 2.95
0 -3 10 56.04 2.99
0 -3 10 53.15 2.47
0 -3 10 54.66 3.01
0 -3 10 56.10 2.76
0 -3 9 156.27 4.34
0 -3 9 150.27 3.99
0 -3 9 151.84 4.23
0 -3 9 158.07 4.92
0 -3 9 154.20 4.42
0 -3 9 158.38 4.61
0 -3 9 155.73 4.69
0 -3 9 160.00 4.14
0 -3 9 153.26 4.68
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8 6 5 132.61 3.90
8 6 6 7.70 1.20
8 6 6 7.30 1.61
8 6 6 7.63 1.93
8 6 7 11.52 1.25
8 6 7 9.64 1.68
8 6 7 11.08 1.87
8 6 8 29.99 2.09
8 6 8 30.17 1.46
8 6 8 33.53 2.03
8 6 8 32.70 1.81
8 6 8 30.27 2.17
8 6 9 37.07 1.59
8 6 9 40.61 2.00
8 6 9 42.70 2.14
8 6 9 41.37 2.07
8 6 9 39.29 1.73
8 6 10 87.33 2.51
8 6 10 81.55 2.48
8 6 10 83.11 2.35
8 6 11 9.52 1.04
8 6 11 6.86 1.09
8 6 11 8.12 0.91
8 7 0 10.46 0.67
-8 -7 0 13.37 0.80
-8 -7 -1 155.09 3.00
-8 -7 -2 75.21 2.13
-8 -7 -3 11.33 1.29
-8 -7 -3 11.54 1.25
8 7 3 12.65 1.58
8 7 3 13.17 1.37
-8 -7 -4 41.34 1.72
-8 -7 -4 38.03 1.74
8 7 4 43.11 2.13
8 7 4 42.33 1.90
-8 -7 -5 16.92 1.28
8 7 5 19.38 1.58
8 7 5 18.40 1.82
-8 -7 -5 20.08 1.36
8 7 6 7.70 1.43
8 7 6 8.51 1.62
8 7 6 6.81 1.07
8 7 7 4.27 1.30
8 7 7 5.47 1.10
8 7 7 5.93 1.29
8 7 7 6.15 1.58
8 7 7 4.01 1.53
8 7 8 48.86 1.86
8 7 8 52.02 1.85
8 7 8 54.00 1.88
8 7 8 52.85 2.10
8 7 8 49.40 2.17
8 7 9 127.87 2.69
8 7 9 132.77 3.05
8 7 9 128.34 2.94
8 7 10 87.00 2.11
8 7 10 89.89 1.89
8 7 11 25.65 0.94
8 8 2 0.74 0.49
-8 -8 -2 1.11 0.48
8 8 3 26.22 1.14
-8 -8 -3 23.98 1.02
-8 -8 -3 26.55 0.96
-8 -8 -4 4.02 0.64
8 8 4 5.28 0.95
8 8 5 8.84 0.98
8 8 5 6.08 0.60
8 8 5 9.31 1.11
8 8 6 32.76 1.49
8 8 6 34.55 1.46
8 8 7 7.24 1.06
8 8 7 6.45 1.03
8 8 7 7.00 0.96
8 8 8 213.56 3.62
8 8 8 208.72 3.58
8 8 8 205.80 3.54
8 8 9 151.26 2.60
8 8 9 153.01 2.56
-9 4 2 22.53 0.76
9 -4 -2 22.56 0.90
-9 4 1 19.95 0.81
9 -4 0 6.76 0.66
-9 4 0 6.52 0.58
9 -4 1 23.01 1.08
9 -4 1 22.98 1.27
9 -4 2 4.76 0.88
9 -4 2 5.43 0.97
9 -4 3 4.47 0.77
9 -4 3 4.83 0.88
9 -4 3 4.49 0.81
9 -4 4 4.33 0.74
9 -4 4 3.13 0.61
-9 3 3 24.98 0.93
9 -3 -3 23.47 0.94
-9 3 2 30.35 1.19
9 -3 -2 31.22 1.35
-9 3 1 66.17 1.72
9 -3 -1 62.71 2.00
-9 3 0 3.07 0.83
-9 3 0 2.93 0.77
9 -3 0 2.60 0.76
9 -3 0 3.18 1.26
-9 3 -1 40.16 1.30
9 -3 1 38.61 1.60
9 -3 2 36.10 1.65
9 -3 2 35.50 1.84
9 -3 3 8.67 1.29
9 -3 4 94.63 2.48
9 -3 4 86.59 2.42
9 -3 5 25.91 1.27
9 -3 5 26.55 1.40
9 -3 5 28.70 1.45
9 -3 6 15.71 0.95
9 -3 6 15.35 1.02
9 -2 -3 1.14 0.67
9 -2 -3 1.50 0.75
-9 2 3 1.29 0.80
9 -2 -2 8.94 1.17
-9 2 2 7.42 0.80
-9 2 2 7.09 1.04
-9 2 1 2.94 1.07
9 -2 -1 3.87 1.26
-9 2 1 3.31 0.83
9 -2 0 8.94 1.50
-9 2 0 8.31 1.22
9 -2 0 8.46 1.36
-9 2 -1 65.40 1.87
9 -2 1 64.41 2.49
9 -2 1 60.91 1.96
9 -2 1 65.49 2.28
9 -2 2 34.23 2.09
9 -2 2 36.51 1.76
9 -2 2 38.62 1.89
9 -2 3 16.04 1.83
9 -2 3 13.27 1.56
9 -2 3 15.02 1.50
9 -2 4 23.68 1.76
9 -2 4 27.53 1.59
9 -2 4 27.02 1.97
9 -2 4 24.99 1.74
9 -2 5 35.15 1.87
9 -2 5 33.93 1.87
9 -2 5 33.42 1.59
9 -2 5 35.85 1.92
9 -2 5 32.77 1.67
9 -2 6 83.79 2.43
9 -2 6 79.07 2.25
9 -2 7 8.35 1.06
9 -2 8 39.96 1.11
-9 1 4 12.13 0.71
9 -1 -4 10.77 0.78
-9 1 3 2.95 0.92
9 -1 -3 3.25 1.05
-9 1 2 41.14 1.64
9 -1 -2 38.92 1.80
9 -1 -2 37.89 1.46
9 -1 -1 6.34 1.17
9 -1 -1 4.71 1.24
-9 1 1 5.18 1.21
9 -1 0 86.75 2.56
9 -1 0 85.83 2.70
-9 1 0 89.22 2.42
9 -1 1 5.49 1.33
-9 1 -1 6.49 1.26
9 -1 1 5.55 1.61
9 -1 2 69.64 2.25
9 -1 2 75.35 2.73
9 -1 2 71.75 2.70
9 -1 2 71.90 2.44
9 -1 3 57.60 2.23
9 -1 3 55.28 2.19
9 -1 3 54.64 2.46
9 -1 3 53.65 2.52
9 -1 4 20.44 2.04
9 -1 4 18.79 1.53
9 -1 4 19.26 1.92
9 -1 4 18.74 1.72
9 -1 4 19.25 1.83
9 -1 5 158.24 3.81
9 -1 5 162.94 3.78
9 -1 5 160.20 3.94
9 -1 5 164.20 3.96
9 -1 6 61.92 2.37
9 -1 6 61.69 2.24
9 -1 6 62.30 2.42
9 -1 6 58.70 2.30
9 -1 6 60.60 2.42
9 -1 7 11.11 1.43
9 -1 7 10.39 1.27
9 -1 7 9.89 1.32
9 -1 7 10.61 1.22
9 -1 7 7.95 1.37
9 -1 8 47.51 1.71
9 -1 8 47.44 1.51
9 -1 8 45.73 1.74
9 -1 9 6.73 0.64
9 0 -4 2.88 0.64
-9 0 3 61.29 1.71
9 0 -3 57.52 1.96
9 0 -3 58.95 1.74
-9 0 2 11.61 1.19
-9 0 2 12.16 1.23
9 0 -2 10.90 1.46
9 0 -2 12.11 1.29
9 0 -1 46.68 1.68
9 0 -1 51.77 2.14
-9 0 1 51.33 1.96
-9 0 1 51.22 1.95
9 0 -1 48.91 2.26
9 0 0 59.37 2.18
9 0 0 73.15 2.59
9 0 0 69.05 2.18
-9 0 0 72.55 2.30
-9 0 0 74.00 2.27
9 0 0 61.16 2.51
9 0 1 49.30 2.32
-9 0 -1 47.37 1.89
9 0 1 48.29 2.14
9 0 2 108.36 3.24
9 0 2 105.20 3.34
-9 0 -2 95.51 2.51
9 0 2 102.36 3.08
9 0 3 5.43 1.65
9 0 3 6.74 1.85
9 0 3 5.65 1.81
9 0 3 6.02 1.70
9 0 4 189.08 4.28
9 0 4 177.69 4.01
9 0 4 182.11 4.33
9 0 4 188.31 4.52
9 0 5 34.83 2.06
9 0 5 32.81 1.99
9 0 5 32.47 2.17
9 0 5 34.79 2.37
9 0 6 46.40 2.23
9 0 6 50.82 2.18
9 0 6 50.12 2.49
9 0 6 48.23 2.32
9 0 7 117.94 3.25
9 0 7 119.10 3.16
9 0 7 116.81 2.92
9 0 7 114.41 3.16
9 0 7 112.87 3.22
9 0 8 11.13 1.38
9 0 8 11.28 1.42
9 0 8 11.70 1.12
9 0 8 12.05 1.40
9 0 8 10.27 1.38
9 0 8 11.06 1.31
9 0 9 15.70 1.18
9 0 9 13.75 1.11
9 0 9 14.80 1.09
-9 -1 2 29.34 1.46
9 1 -2 26.64 1.75
-9 -1 1 3.55 1.18
-9 -1 1 2.81 1.23
9 1 -1 1.66 1.49
9 1 -1 1.88 1.47
-9 -1 0 72.22 2.36
-9 -1 0 68.12 2.27
9 1 0 68.36 2.72
9 1 1 148.44 3.37
9 1 1 156.51 4.01
-9 -1 -1 146.38 3.43
-9 -1 -1 151.99 3.31
9 1 1 139.53 3.80
9 1 2 4.09 1.77
-9 -1 -2 4.39 1.25
-9 -1 -2 4.54 1.18
9 1 2 3.54 1.34
9 1 2 4.44 1.74
9 1 2 5.07 1.52
9 1 3 177.93 4.20
9 1 3 174.26 4.32
9 1 3 168.29 4.32
9 1 4 171.75 4.29
9 1 4 178.47 4.36
9 1 4 169.87 4.31
9 1 5 6.43 1.45
9 1 5 7.89 2.04
9 1 5 9.59 1.85
9 1 5 8.59 1.81
9 1 5 9.89 1.92
9 1 5 8.13 1.67
9 1 6 156.45 3.72
9 1 6 166.36 4.23
9 1 6 161.52 4.26
9 1 6 169.96 4.05
9 1 6 165.74 4.06
9 1 6 166.99 3.91
9 1 7 73.43 2.81
9 1 7 79.53 2.64
9 1 7 73.67 2.65
9 1 7 72.49 2.36
9 1 7 72.39 2.55
9 1 7 75.99 2.55
9 1 8 6.31 1.36
9 1 8 6.52 1.57
9 1 8 5.28 1.33
9 1 8 5.64 1.38
9 1 8 6.15 1.33
9 1 9 17.44 1.35
9 1 9 17.03 1.35
9 1 9 15.40 1.23
9 1 9 18.29 1.34
9 1 9 15.09 1.40
9 1 9 15.90 1.24
9 1 10 52.53 1.41
9 1 10 41.84 1.25
-9 -2 3 56.67 1.52
9 2 -3 59.09 1.53
-9 -2 2 57.18 1.71
9 2 -2 62.99 2.00
9 2 -1 70.04 2.38
9 2 -1 64.31 2.49
-9 -2 1 62.68 2.09
9 2 0 240.22 5.16
-9 -2 0 241.48 4.70
9 2 1 20.89 2.00
-9 -2 -1 21.96 1.60
9 2 1 19.57 2.01
-9 -2 -2 114.60 3.01
9 2 2 120.82 3.35
9 2 2 113.39 3.24
9 2 3 70.59 2.97
9 2 3 70.74 2.69
9 2 3 66.96 2.50
9 2 3 64.93 2.59
9 2 4 6.40 1.92
9 2 4 6.22 1.72
9 2 4 6.41 1.66
9 2 4 6.36 1.90
9 2 4 6.58 1.70
9 2 5 94.92 3.16
9 2 5 80.58 2.49
9 2 5 92.13 3.22
9 2 5 90.05 3.24
9 2 5 85.00 2.90
9 2 5 95.24 3.07
9 2 6 106.53 3.37
9 2 6 96.39 2.68
9 2 6 108.65 3.20
9 2 6 111.91 3.47
9 2 6 104.35 3.07
9 2 6 93.69 2.72
9 2 7 39.40 2.30
9 2 7 36.05 1.85
9 2 7 39.66 2.09
9 2 7 35.96 2.08
9 2 7 38.19 2.36
9 2 7 38.26 1.99
9 2 7 37.40 1.81
9 2 8 4.22 1.58
9 2 8 5.13 1.30
9 2 8 3.41 1.61
9 2 8 5.26 1.27
9 2 8 3.42 1.21
9 2 8 4.84 1.39
9 2 8 2.56 1.30
9 2 9 88.67 2.37
9 2 9 93.81 2.45
9 2 9 84.60 2.19
9 2 9 78.89 2.12
9 2 10 86.14 2.04
9 3 -2 33.08 1.22
-9 -3 2 27.60 1.03
-9 -3 1 179.11 3.46
9 3 -1 179.05 3.62
9 3 0 46.18 2.04
-9 -3 0 45.71 1.85
9 3 1 141.98 3.17
-9 -3 -1 147.50 3.39
9 3 2 210.66 4.59
9 3 2 189.52 3.88
9 3 2 191.21 4.02
-9 -3 -2 202.99 4.13
9 3 3 33.45 2.20
-9 -3 -3 31.24 1.66
9 3 3 28.87 1.82
9 3 3 30.21 2.17
9 3 3 30.77 1.84
9 3 4 91.20 3.09
9 3 4 87.40 2.65
9 3 4 80.27 2.75
9 3 4 77.98 2.94
9 3 4 83.02 2.66
9 3 5 88.71 2.91
9 3 5 88.00 2.98
9 3 5 89.19 3.07
9 3 5 91.12 2.79
9 3 6 131.53 3.59
9 3 6 128.90 3.54
9 3 6 127.98 3.56
9 3 6 124.52 3.52
9 3 6 125.17 3.28
9 3 7 129.88 3.47
9 3 7 132.22 3.55
9 3 7 128.07 3.52
9 3 7 125.90 3.42
9 3 7 120.60 3.18
9 3 7 126.14 3.46
9 3 8 8.57 1.49
9 3 8 7.44 1.62
9 3 8 5.93 1.58
9 3 8 6.91 1.50
9 3 8 6.00 1.27
9 3 8 6.02 1.43
9 3 9 164.02 3.64
9 3 9 161.45 3.43
9 3 9 164.83 3.48
9 3 9 163.13 3.28
9 3 9 156.49 3.37
9 3 10 172.20 3.18
9 3 10 181.43 3.43
9 3 10 178.67 3.26
9 4 -1 69.44 1.60
-9 -4 1 72.10 1.81
9 4 0 13.92 1.16
-9 -4 0 12.27 1.22
-9 -4 -1 92.64 2.52
9 4 1 96.39 2.56
-9 -4 -2 29.54 1.61
-9 -4 -2 34.70 1.84
9 4 2 34.73 1.82
-9 -4 -3 15.25 1.32
-9 -4 -3 21.70 1.64
9 4 3 20.09 1.71
9 4 3 18.73 1.95
9 4 4 15.90 1.89
9 4 4 15.87 1.54
9 4 4 15.42 1.23
-9 -4 -4 17.16 1.53
9 4 4 18.95 1.72
9 4 5 54.74 2.02
9 4 5 54.08 2.07
9 4 5 61.01 2.61
9 4 5 55.97 2.19
-9 -4 -5 64.67 1.99
9 4 5 62.92 2.40
9 4 5 56.64 1.89
9 4 5 63.23 2.53
9 4 6 117.46 2.82
9 4 6 142.20 3.57
9 4 6 123.29 3.18
9 4 6 127.90 3.21
9 4 6 137.03 3.38
9 4 6 127.64 3.27
9 4 6 132.11 3.19
9 4 6 140.51 3.60
9 4 7 33.79 1.82
9 4 7 35.05 2.06
9 4 7 33.95 1.81
9 4 7 36.91 1.89
9 4 7 35.59 1.80
9 4 7 31.72 1.52
9 4 7 34.91 2.04
9 4 8 49.22 1.89
9 4 8 47.54 1.62
9 4 8 49.27 2.02
9 4 9 272.40 4.46
9 4 9 263.99 4.31
9 4 9 262.63 4.57
9 4 10 43.82 1.36
9 4 10 41.68 1.46
-9 -5 0 80.85 1.66
-9 -5 -1 40.02 1.51
-9 -5 -1 36.92 1.30
9 5 2 14.42 1.00
-9 -5 -2 15.50 1.30
-9 -5 -2 13.49 1.02
9 5 3 8.38 1.21
-9 -5 -3 6.84 1.21
9 5 3 6.50 0.99
-9 -5 -3 4.73 0.94
9 5 3 7.43 1.05
9 5 4 33.66 2.02
9 5 4 33.83 1.77
9 5 4 31.88 1.54
-9 -5 -4 31.67 1.57
9 5 4 35.14 1.63
9 5 5 348.33 6.14
9 5 5 331.37 5.60
-9 -5 -5 323.05 5.30
9 5 5 339.94 5.85
9 5 5 344.16 5.84
9 5 6 171.55 3.82
9 5 6 161.92 3.64
9 5 6 161.48 3.32
9 5 6 166.51 3.61
9 5 7 36.10 1.73
9 5 7 35.87 1.89
9 5 7 33.49 1.48
9 5 7 32.20 1.76
9 5 7 35.68 1.79
9 5 8 409.07 6.48
9 5 8 395.70 5.99
9 5 8 392.65 6.24
9 5 8 417.03 6.31
9 5 8 431.49 6.51
9 5 9 164.08 3.23
9 5 9 239.83 3.90
9 5 9 207.03 3.57
9 5 9 224.84 3.71
9 5 9 194.77 3.32
9 5 9 245.88 3.96
9 5 10 1.04 0.64
9 5 10 0.97 0.54
9 6 2 131.87 2.47
-9 -6 -2 129.03 2.32
9 6 3 14.63 1.21
9 6 3 15.64 1.10
-9 -6 -3 17.15 0.99
9 6 4 65.88 2.02
9 6 4 69.38 1.94
9 6 5 380.94 5.57
9 6 5 371.38 5.57
9 6 6 23.31 1.14
9 6 6 22.83 1.42
9 6 6 22.51 1.42
9 6 6 23.28 1.44
9 6 7 151.25 2.98
9 6 7 155.37 3.14
9 6 7 154.42 3.16
9 6 7 163.15 3.21
9 6 8 341.72 5.34
9 6 8 341.63 5.36
9 6 8 339.76 5.34
9 6 8 330.68 5.25
9 6 9 8.17 0.70
9 6 9 7.99 0.72
9 6 9 8.44 0.73
9 7 5 34.23 1.11
9 7 6 77.06 1.70
9 7 7 233.19 3.64
10 -1 1 4.54 0.61
10 -1 1 4.40 0.69
10 -1 2 110.11 2.15
10 -1 2 119.12 2.34
10 -1 3 104.27 2.05
10 -1 3 108.89 2.14
10 -1 4 84.00 1.73
10 -1 4 80.67 1.84
10 -1 4 86.25 1.90
10 -1 5 5.34 0.65
10 0 0 8.57 0.63
10 0 1 56.01 1.48
10 0 1 45.25 1.40
10 0 2 91.33 2.17
10 0 2 89.38 2.18
10 0 3 32.64 1.35
10 0 3 29.66 1.45
10 0 3 28.68 1.22
10 0 4 6.36 0.66
10 0 4 8.47 1.04
10 0 4 7.89 0.95
10 0 5 12.60 0.75
10 0 5 17.47 1.08
10 0 6 112.49 2.27
10 0 6 124.86 2.38
10 1 1 13.92 0.90
10 1 1 16.69 0.92
10 1 2 48.34 1.57
10 1 2 46.30 1.50
10 1 2 51.74 1.57
10 1 3 99.67 2.22
10 1 3 93.26 2.23
10 1 3 97.51 2.19
10 1 4 1.06 0.88
10 1 4 1.62 0.88
10 1 4 1.52 0.97
10 1 4 1.86 0.93
10 1 4 1.84 0.84
10 1 5 69.96 1.94
10 1 5 69.18 1.78
10 1 5 80.52 2.08
10 1 5 71.58 1.85
10 1 5 78.23 1.96
10 1 6 272.68 4.27
10 1 6 268.72 4.40
10 1 6 259.71 4.34
10 1 7 44.27 1.19
-10 -2 -1 23.15 0.94
10 2 1 20.75 0.97
10 2 2 102.92 2.03
10 2 3 70.95 1.72
10 2 3 59.67 1.57
10 2 4 84.11 2.01
10 2 4 87.78 2.04
10 2 5 315.26 5.20
10 2 5 302.68 4.95
10 2 6 157.26 2.97
10 2 6 154.45 2.80
10 2 6 151.12 2.85
10 2 6 148.95 2.85
10 2 7 12.19 0.74
10 2 7 14.85 0.90
10 3 2 139.94 2.51
-10 -3 -2 146.69 2.55
10 3 3 1.77 0.78
-10 -3 -3 2.16 0.62
10 3 3 2.20 0.82
10 3 4 253.99 4.15
10 3 4 232.06 4.10
10 3 5 370.92 5.82
10 3 5 373.71 5.76
10 3 6 8.55 0.88
10 3 7 60.56 1.46
10 3 7 65.79 1.52
10 4 5 78.02 1.64
10 4 5 64.52 1.49
10 4 6 15.66 0.82
TITL ij1027_auto in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184 8.090030 9.577204 12.239978 70.2419 76.0038 83.8605
ZERR 1.00 0.000095 0.000082 0.000083 0.0007 0.0009 0.0008
LATT 1
SFAC C H N O Co Br
UNIT 28.00 37.00 4.00 5.00 2.00 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 57699
_shelx_res_file
;
TITL ij1027_a.res in P-1
ij1027.res
created by SHELXL-2016/6 at 13:23:11 on 23-Jun-2023
REM Old TITL ij1027_auto in P-1 #2
REM SHELXT solution in P-1
REM R1 0.084, Rweak 0.010, Alpha 0.073, Orientation as input
REM Formula found by SHELXT: C15 Br2 Co N2 O2
CELL 1.54184 8.09 9.5772 12.24 70.242 76.004 83.86
ZERR 1 0.0001 0.0001 0.0001 0.001 0.001 0.001
LATT 1
SFAC C H Br Co N O
UNIT 28 38 4 2 4 5
EQIV $1 1-X,1-Y,1-Z
EQIV $2 1+X,+Y,+Z
EQIV $3 1-X,-Y,1-Z
EQIV $4 2-X,1-Y,-Z
EQIV $5 1-X,1-Y,-Z
DFIX 1.45 0.001 C21 O21
L.S. 10
PLAN 5
SIZE 0.03 0.03 0.15
TEMP -173.15(10)
HTAB C5 Br1_$2
HTAB C5 Br1_$1
HTAB C6 O11_$1
HTAB C6 Br2_$3
HTAB C6 Br1
HTAB C12 Br2_$4
HTAB C12 O21_$4
HTAB C14 Br1_$5
HTAB C16 Br1_$2
HTAB O21 Br2
CONF
BOND $H
HTAB
MORE -1
fmap 2
acta
REM
REM
REM
WGHT 0.030600 1.268600
EXTI 0.001060
FVAR 0.61183
CO1 4 0.522095 0.469471 0.367343 11.00000 0.02026 0.01482 =
0.01137 -0.00463 -0.00241 -0.00042
BR1 3 0.244346 0.416560 0.349436 11.00000 0.02518 0.02280 =
0.02382 -0.00991 -0.01136 0.00051
BR2 3 0.712032 0.288925 0.280694 11.00000 0.03810 0.01941 =
0.02232 -0.01123 0.00953 -0.00291
O1 6 0.576114 0.381056 0.527999 11.00000 0.01947 0.01433 =
0.01613 -0.00700 -0.00526 0.00580
N1 5 0.671287 0.255523 0.564047 11.00000 0.01963 0.01344 =
0.01594 -0.00605 -0.00580 0.00508
C1 1 0.594542 0.122698 0.605054 11.00000 0.02497 0.01772 =
0.01216 -0.00571 -0.00294 -0.00074
C2 1 0.694428 -0.004579 0.643167 11.00000 0.03139 0.01868 =
0.01997 -0.00636 -0.00551 0.00449
AFIX 43
H2 2 0.644348 -0.099275 0.673735 11.00000 -1.20000
AFIX 0
C3 1 0.865991 0.006001 0.636802 11.00000 0.03344 0.02645 =
0.02352 -0.00851 -0.01067 0.01167
AFIX 43
H3 2 0.933382 -0.081032 0.663242 11.00000 -1.20000
AFIX 0
C4 1 0.938824 0.143844 0.591779 11.00000 0.02243 0.02910 =
0.03049 -0.01356 -0.00871 0.00697
AFIX 43
H4 2 1.056708 0.152377 0.586252 11.00000 -1.20000
AFIX 0
C5 1 0.838175 0.268900 0.554962 11.00000 0.02011 0.02229 =
0.02353 -0.01188 -0.00342 0.00134
AFIX 43
H5 2 0.886759 0.364257 0.523258 11.00000 -1.20000
AFIX 0
C6 1 0.412525 0.121101 0.603156 11.00000 0.02471 0.01732 =
0.02149 -0.00618 -0.00475 -0.00261
AFIX 137
H6A 2 0.345495 0.183462 0.647998 11.00000 -1.50000
H6B 2 0.372568 0.019130 0.639542 11.00000 -1.50000
H6C 2 0.398996 0.159651 0.520671 11.00000 -1.50000
AFIX 0
O11 6 0.614695 0.653877 0.243966 11.00000 0.03826 0.01933 =
0.01192 -0.00633 0.00460 -0.00586
N11 5 0.694577 0.652259 0.134231 11.00000 0.03734 0.01584 =
0.01388 -0.00537 0.00298 -0.00486
C11 1 0.863399 0.674169 0.098551 11.00000 0.03477 0.01730 =
0.01986 -0.00563 -0.00096 0.00494
C12 1 0.941091 0.678135 -0.016938 11.00000 0.04142 0.02496 =
0.02102 -0.00665 0.00421 0.00472
AFIX 43
H12 2 1.059812 0.694910 -0.045090 11.00000 -1.20000
AFIX 0
C13 1 0.848511 0.658091 -0.091381 11.00000 0.05887 0.02389 =
0.01610 -0.00847 0.00554 -0.00583
AFIX 43
H13 2 0.903094 0.660251 -0.169909 11.00000 -1.20000
AFIX 0
C14 1 0.677368 0.635096 -0.050806 11.00000 0.06261 0.02941 =
0.01996 -0.01120 -0.00006 -0.01739
AFIX 43
H14 2 0.611936 0.621342 -0.101029 11.00000 -1.20000
AFIX 0
C15 1 0.600352 0.632018 0.063768 11.00000 0.04615 0.02816 =
0.02403 -0.01189 -0.00097 -0.01527
AFIX 43
H15 2 0.481643 0.615737 0.092873 11.00000 -1.20000
AFIX 0
C16 1 0.954584 0.691669 0.184683 11.00000 0.02950 0.04413 =
0.02574 -0.00724 -0.00783 0.01019
AFIX 137
H16A 2 0.911410 0.781415 0.204957 11.00000 -1.50000
H16B 2 1.076871 0.700157 0.148968 11.00000 -1.50000
H16C 2 0.935641 0.604983 0.256956 11.00000 -1.50000
AFIX 0
PART 1
O21 6 0.656751 0.198443 0.059679 10.50000 0.05266 0.04358 =
0.04445 -0.02178 -0.02661 0.00650
AFIX 147
H21 2 0.673583 0.200477 0.124200 10.50000 -1.50000
AFIX 0
PART 0
C21 1 0.691173 0.049246 0.052958 11.00000 0.07873 0.05287 =
0.03780 -0.01772 -0.02553 0.03450
PART 1
AFIX 23
H21A 2 0.658475 -0.023433 0.133764 10.50000 -1.20000
H21B 2 0.814941 0.035705 0.023128 10.50000 -1.20000
AFIX 137
PART 2
H21C 2 0.665943 -0.027068 0.131402 10.50000 -1.20000
H21D 2 0.656102 0.147024 0.061153 10.50000 -1.20000
H21E 2 0.813823 0.047438 0.018754 10.50000 -1.20000
AFIX 0
PART 0
C22 1 0.593247 0.018372 -0.029399 11.00000 0.08071 0.03390 =
0.02705 -0.01212 -0.01274 0.02416
AFIX 23
H22A 2 0.598140 0.106639 -0.101445 11.00000 -1.20000
H22B 2 0.650354 -0.065663 -0.054982 11.00000 -1.20000
AFIX 0
HKLF 4
REM ij1027_a.res in P-1
REM R1 = 0.0244 for 3686 Fo > 4sig(Fo) and 0.0245 for all 3705 data
REM 204 parameters refined using 1 restraints
END
WGHT 0.0306 1.2689
REM Instructions for potential hydrogen bonds
HTAB C5 Br1_$2
HTAB C5 Br1_$1
HTAB C6 O11_$1
HTAB C6 Br2_$3
HTAB C6 Br1
HTAB C12 Br2_$4
HTAB C12 O21_$4
HTAB C14 Br1_$5
HTAB C16 Br1_$2
HTAB O21 Br2
REM Highest difference peak 0.502, deepest hole -0.590, 1-sigma level 0.078
Q1 1 0.3675 0.4346 0.3799 11.00000 0.05 0.50
Q2 1 0.5808 0.5852 0.2920 11.00000 0.05 0.42
Q3 1 0.3917 0.4785 0.3216 11.00000 0.05 0.40
Q4 1 0.3047 0.3355 0.4317 11.00000 0.05 0.37
Q5 1 0.7143 0.3219 0.2019 11.00000 0.05 0.36
;
_shelx_res_checksum 50571
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.52210(5) 0.46947(4) 0.36734(3) 0.01558(10) Uani d 1 . .
Br Br1 0.24435(3) 0.41656(3) 0.34944(2) 0.02233(8) Uani d 1 . .
Br Br2 0.71203(4) 0.28893(3) 0.28069(2) 0.02820(9) Uani d 1 . .
O O1 0.5761(2) 0.38106(17) 0.52800(14) 0.0163(3) Uani d 1 . .
N N1 0.6713(2) 0.2555(2) 0.56405(17) 0.0161(4) Uani d 1 . .
C C1 0.5945(3) 0.1227(3) 0.60505(19) 0.0183(4) Uani d 1 . .
C C2 0.6944(3) -0.0046(3) 0.6432(2) 0.0238(5) Uani d 1 . .
H H2 0.644348 -0.099275 0.673735 0.029 Uiso calc 1 . .
C C3 0.8660(4) 0.0060(3) 0.6368(2) 0.0279(5) Uani d 1 . .
H H3 0.933382 -0.081032 0.663242 0.033 Uiso calc 1 . .
C C4 0.9388(3) 0.1438(3) 0.5918(2) 0.0264(5) Uani d 1 . .
H H4 1.056708 0.152377 0.586252 0.032 Uiso calc 1 . .
C C5 0.8382(3) 0.2689(3) 0.5550(2) 0.0212(5) Uani d 1 . .
H H5 0.886759 0.364257 0.523258 0.025 Uiso calc 1 . .
C C6 0.4125(3) 0.1211(3) 0.6032(2) 0.0211(5) Uani d 1 . .
H H6A 0.345495 0.183462 0.647998 0.032 Uiso calc 1 . .
H H6B 0.372568 0.019130 0.639542 0.032 Uiso calc 1 . .
H H6C 0.398996 0.159651 0.520671 0.032 Uiso calc 1 . .
O O11 0.6147(2) 0.65388(19) 0.24397(14) 0.0243(4) Uani d 1 . .
N N11 0.6946(3) 0.6523(2) 0.13423(17) 0.0234(4) Uani d 1 . .
C C11 0.8634(3) 0.6742(3) 0.0986(2) 0.0254(5) Uani d 1 . .
C C12 0.9411(4) 0.6781(3) -0.0169(2) 0.0318(6) Uani d 1 . .
H H12 1.059812 0.694910 -0.045090 0.038 Uiso calc 1 . .
C C13 0.8485(4) 0.6581(3) -0.0914(2) 0.0346(7) Uani d 1 . .
H H13 0.903094 0.660251 -0.169909 0.041 Uiso calc 1 . .
C C14 0.6774(4) 0.6351(3) -0.0508(2) 0.0369(7) Uani d 1 . .
H H14 0.611936 0.621342 -0.101029 0.044 Uiso calc 1 . .
C C15 0.6004(4) 0.6320(3) 0.0638(2) 0.0320(6) Uani d 1 . .
H H15 0.481643 0.615737 0.092873 0.038 Uiso calc 1 . .
C C16 0.9546(4) 0.6917(4) 0.1847(3) 0.0347(6) Uani d 1 . .
H H16A 0.911410 0.781415 0.204957 0.052 Uiso calc 1 . .
H H16B 1.076871 0.700157 0.148968 0.052 Uiso calc 1 . .
H H16C 0.935641 0.604983 0.256956 0.052 Uiso calc 1 . .
O O21 0.6568(6) 0.1984(4) 0.0597(4) 0.0427(10) Uani d 0.5 A 1
H H21 0.673583 0.200477 0.124200 0.064 Uiso calc 0.5 A 1
C C21 0.6912(6) 0.0492(4) 0.0530(3) 0.0562(10) Uani d 1 . .
H H21A 0.658475 -0.023433 0.133764 0.067 Uiso calc 0.5 A 1
H H21B 0.814941 0.035705 0.023128 0.067 Uiso calc 0.5 A 1
H H21C 0.665943 -0.027068 0.131402 0.067 Uiso calc 0.5 A 2
H H21D 0.656102 0.147024 0.061153 0.067 Uiso calc 0.5 A 2
H H21E 0.813823 0.047438 0.018754 0.067 Uiso calc 0.5 A 2
C C22 0.5932(5) 0.0184(4) -0.0294(3) 0.0485(9) Uani d 1 . .
H H22A 0.598140 0.106639 -0.101445 0.058 Uiso calc 1 . .
H H22B 0.650354 -0.065663 -0.054982 0.058 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 0.02026(19) 0.01482(18) 0.01137(18) -0.00042(13) -0.00241(14) -0.00463(13)
Br1 0.02518(13) 0.02280(13) 0.02382(14) 0.00051(9) -0.01136(10) -0.00991(10)
Br2 0.03810(16) 0.01941(13) 0.02232(14) -0.00291(10) 0.00953(10) -0.01123(10)
O1 0.0195(7) 0.0143(7) 0.0161(7) 0.0058(6) -0.0053(6) -0.0070(6)
N1 0.0196(9) 0.0134(8) 0.0159(9) 0.0051(7) -0.0058(7) -0.0061(7)
C1 0.0250(11) 0.0177(10) 0.0122(10) -0.0007(8) -0.0029(8) -0.0057(8)
C2 0.0314(13) 0.0187(11) 0.0200(11) 0.0045(9) -0.0055(10) -0.0064(9)
C3 0.0334(13) 0.0264(12) 0.0235(12) 0.0117(10) -0.0107(10) -0.0085(10)
C4 0.0224(11) 0.0291(13) 0.0305(13) 0.0070(10) -0.0087(10) -0.0136(11)
C5 0.0201(11) 0.0223(11) 0.0235(12) 0.0013(9) -0.0034(9) -0.0119(9)
C6 0.0247(11) 0.0173(11) 0.0215(11) -0.0026(9) -0.0048(9) -0.0062(9)
O11 0.0383(10) 0.0193(8) 0.0119(7) -0.0059(7) 0.0046(7) -0.0063(6)
N11 0.0373(12) 0.0158(9) 0.0139(9) -0.0049(8) 0.0030(8) -0.0054(7)
C11 0.0348(13) 0.0173(11) 0.0199(12) 0.0049(9) -0.0010(10) -0.0056(9)
C12 0.0414(15) 0.0250(13) 0.0210(12) 0.0047(11) 0.0042(11) -0.0067(10)
C13 0.0589(19) 0.0239(12) 0.0161(11) -0.0058(12) 0.0055(12) -0.0085(10)
C14 0.063(2) 0.0294(14) 0.0200(13) -0.0174(13) -0.0001(13) -0.0112(11)
C15 0.0461(16) 0.0282(13) 0.0240(13) -0.0153(12) -0.0010(12) -0.0119(11)
C16 0.0295(13) 0.0441(16) 0.0257(13) 0.0102(12) -0.0078(11) -0.0072(12)
O21 0.053(3) 0.044(2) 0.044(3) 0.006(2) -0.027(2) -0.022(2)
C21 0.079(3) 0.053(2) 0.0378(18) 0.035(2) -0.0255(18) -0.0177(16)
C22 0.081(3) 0.0339(16) 0.0270(15) 0.0242(17) -0.0127(15) -0.0121(13)
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'
Br Br -0.6763 1.2805 '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'
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
Br1 Co1 Br2 . . 101.355(16) y
O1 Co1 Br1 . . 116.56(5) y
O1 Co1 Br1 2_666 . 95.39(4) y
O1 Co1 Br2 . . 94.52(4) y
O1 Co1 Br2 2_666 . 161.54(4) y
O1 Co1 O1 . 2_666 70.82(7) y
O11 Co1 Br1 . . 112.08(6) y
O11 Co1 Br2 . . 97.54(5) y
O11 Co1 O1 . 2_666 83.12(6) y
O11 Co1 O1 . . 126.08(7) y
Co1 O1 Co1 . 2_666 109.18(7) y
N1 O1 Co1 . . 125.78(12) y
N1 O1 Co1 . 2_666 124.80(12) y
O1 N1 C1 . . 118.60(18) ?
C5 N1 O1 . . 118.18(19) ?
C5 N1 C1 . . 123.2(2) ?
N1 C1 C2 . . 117.5(2) ?
N1 C1 C6 . . 118.4(2) ?
C2 C1 C6 . . 124.0(2) ?
C1 C2 H2 . . 119.8 ?
C3 C2 C1 . . 120.5(2) ?
C3 C2 H2 . . 119.8 ?
C2 C3 H3 . . 120.2 ?
C4 C3 C2 . . 119.7(2) ?
C4 C3 H3 . . 120.2 ?
C3 C4 H4 . . 120.4 ?
C5 C4 C3 . . 119.2(2) ?
C5 C4 H4 . . 120.4 ?
N1 C5 C4 . . 119.9(2) ?
N1 C5 H5 . . 120.1 ?
C4 C5 H5 . . 120.1 ?
C1 C6 H6A . . 109.5 ?
C1 C6 H6B . . 109.5 ?
C1 C6 H6C . . 109.5 ?
H6A C6 H6B . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
N11 O11 Co1 . . 120.09(13) ?
O11 N11 C15 . . 118.3(2) ?
C11 N11 O11 . . 118.8(2) ?
C11 N11 C15 . . 122.9(2) ?
N11 C11 C12 . . 117.5(3) ?
N11 C11 C16 . . 118.2(2) ?
C12 C11 C16 . . 124.3(3) ?
C11 C12 H12 . . 119.5 ?
C13 C12 C11 . . 121.1(3) ?
C13 C12 H12 . . 119.5 ?
C12 C13 H13 . . 120.4 ?
C14 C13 C12 . . 119.3(2) ?
C14 C13 H13 . . 120.4 ?
C13 C14 H14 . . 120.2 ?
C13 C14 C15 . . 119.5(3) ?
C15 C14 H14 . . 120.2 ?
N11 C15 C14 . . 119.7(3) ?
N11 C15 H15 . . 120.1 ?
C14 C15 H15 . . 120.1 ?
C11 C16 H16A . . 109.5 ?
C11 C16 H16B . . 109.5 ?
C11 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C21 O21 H21 . . 109.5 ?
O21 C21 H21A . . 109.2 ?
O21 C21 H21B . . 109.2 ?
O21 C21 C22 . . 112.1(3) ?
H21A C21 H21B . . 107.9 ?
H21C C21 H21D . . 109.5 ?
H21C C21 H21E . . 109.5 ?
H21D C21 H21E . . 109.5 ?
C22 C21 H21A . . 109.2 ?
C22 C21 H21B . . 109.2 ?
C22 C21 H21C . . 109.5 ?
C22 C21 H21D . . 109.5 ?
C22 C21 H21E . . 109.5 ?
C21 C22 H22A . . 108.9 ?
C21 C22 H22B . . 108.9 ?
C22 C22 C21 2_655 . 113.3(3) ?
C22 C22 H22A 2_655 . 108.9 ?
C22 C22 H22B 2_655 . 108.9 ?
H22A C22 H22B . . 107.7 ?
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 Br1 . 2.4312(4) y
Co1 Br2 . 2.5217(4) y
Co1 O1 . 1.9964(16) y
Co1 O1 2_666 2.1968(15) y
Co1 O11 . 1.9732(17) y
O1 N1 . 1.357(2) ?
N1 C1 . 1.357(3) ?
N1 C5 . 1.344(3) ?
C1 C2 . 1.394(3) ?
C1 C6 . 1.480(3) ?
C2 H2 . 0.9500 ?
C2 C3 . 1.384(4) ?
C3 H3 . 0.9500 ?
C3 C4 . 1.382(4) ?
C4 H4 . 0.9500 ?
C4 C5 . 1.380(3) ?
C5 H5 . 0.9500 ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
O11 N11 . 1.347(2) ?
N11 C11 . 1.346(4) ?
N11 C15 . 1.351(4) ?
C11 C12 . 1.391(3) ?
C11 C16 . 1.485(4) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.381(4) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.368(5) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.382(4) ?
C15 H15 . 0.9500 ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
O21 H21 . 0.8400 ?
O21 C21 . 1.4524(10) ?
C21 H21A . 0.9900 ?
C21 H21B . 0.9900 ?
C21 H21C . 0.9800 ?
C21 H21D . 0.9800 ?
C21 H21E . 0.9800 ?
C21 C22 . 1.539(5) ?
C22 C22 2_655 1.528(8) ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
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
C5 H5 Br1 1_655 0.95 3.12 3.704(2) 121.0
C5 H5 Br1 2_666 0.95 2.98 3.531(2) 118.1
C6 H6A O11 2_666 0.98 2.45 3.259(3) 140.0
C6 H6B Br2 2_656 0.98 2.88 3.852(2) 172.1
C6 H6C Br1 . 0.98 3.02 3.845(2) 142.3
C12 H12 Br2 2_765 0.95 2.99 3.676(3) 130.4
C12 H12 O21 2_765 0.95 2.55 3.441(6) 155.8
C14 H14 Br1 2_665 0.95 3.11 3.747(3) 125.9
C16 H16C Br1 1_655 0.98 3.13 3.725(3) 120.6
O21 H21 Br2 . 0.84 2.43 3.244(4) 162.1
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 N1 C1 2_666 . . . 102.20(19) ?
Co1 O1 N1 C1 . . . . -84.0(2) ?
Co1 O1 N1 C5 2_666 . . . -79.2(2) ?
Co1 O1 N1 C5 . . . . 94.6(2) ?
Co1 O11 N11 C11 . . . . -111.6(2) ?
Co1 O11 N11 C15 . . . . 69.9(3) ?
O1 N1 C1 C2 . . . . -179.10(19) ?
O1 N1 C1 C6 . . . . 2.8(3) ?
O1 N1 C5 C4 . . . . 179.4(2) ?
N1 C1 C2 C3 . . . . -1.1(3) ?
C1 N1 C5 C4 . . . . -2.1(4) ?
C1 C2 C3 C4 . . . . -0.3(4) ?
C2 C3 C4 C5 . . . . 0.6(4) ?
C3 C4 C5 N1 . . . . 0.5(4) ?
C5 N1 C1 C2 . . . . 2.3(3) ?
C5 N1 C1 C6 . . . . -175.8(2) ?
C6 C1 C2 C3 . . . . 176.9(2) ?
O11 N11 C11 C12 . . . . -177.4(2) ?
O11 N11 C11 C16 . . . . 3.0(3) ?
O11 N11 C15 C14 . . . . 177.7(2) ?
N11 C11 C12 C13 . . . . -0.9(4) ?
C11 N11 C15 C14 . . . . -0.7(4) ?
C11 C12 C13 C14 . . . . 0.5(4) ?
C12 C13 C14 C15 . . . . -0.1(4) ?
C13 C14 C15 N11 . . . . 0.2(4) ?
C15 N11 C11 C12 . . . . 1.1(4) ?
C15 N11 C11 C16 . . . . -178.6(2) ?
C16 C11 C12 C13 . . . . 178.7(3) ?
O21 C21 C22 C22 . . . 2_655 -79.5(5) ?