#------------------------------------------------------------------------------
#$Date: 2023-10-06 03:52:34 +0200 (Fri, 06 Oct 2023) $
#$Revision: 286819 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022871.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_2022871
loop_
_publ_author_name
'Sirenko, Valerii Y.'
'Kuzevanova, Iryna S.'
'Vynohradov, Oleksandr S.'
'Naumova, Dina D.'
'Shova, Sergiu'
_publ_section_title
;
Carbon dioxide capture from air leading to
bis[N-(5-methyl-1H-pyrazol-3-yl-\kN 2)carbamato-\kO]copper(II)
tetrahydrate
;
_journal_coeditor_code TX2076
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023008575
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '[Cu (C5 H6 N3 O2)2], 4H2 O'
_chemical_formula_moiety 'C10 H12 Cu N6 O4, 4(H2 O)'
_chemical_formula_sum 'C10 H20 Cu N6 O8'
_chemical_formula_weight 415.86
_chemical_name_systematic
'Bis[N-(5-methyl-1H-pyrazol-3-yl-\kN^2^)carbamato-\kO]copper(II) tetrahydrate'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha 90
_cell_angle_beta 98.786(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.4623(2)
_cell_length_b 5.64870(16)
_cell_length_c 17.4536(4)
_cell_measurement_reflns_used 2285
_cell_measurement_temperature 199.99(11)
_cell_measurement_theta_max 72.2760
_cell_measurement_theta_min 5.1080
_cell_volume 824.51(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015a)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015b)
;
_diffrn_ambient_temperature 199.99(11)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0416
_diffrn_reflns_av_unetI/netI 0.0383
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 5223
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.771
_diffrn_reflns_theta_min 5.128
_exptl_absorpt_coefficient_mu 2.390
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.63767
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour 'clear light violet'
_exptl_crystal_density_diffrn 1.675
_exptl_crystal_description block
_exptl_crystal_F_000 430
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.453
_refine_diff_density_min -0.569
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.048
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 116
_refine_ls_number_reflns 1634
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.047
_refine_ls_R_factor_all 0.0487
_refine_ls_R_factor_gt 0.0413
_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^)+(0.0636P)^2^+0.4306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1100
_refine_ls_wR_factor_ref 0.1184
_reflns_number_gt 1401
_reflns_number_total 1634
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file tx2076sup1.cif
_cod_data_source_block I
_cod_database_code 2022871
_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 0.716
_shelx_estimated_absorpt_t_max 0.716
_shelx_hkl_file
;
0 0 1 0.38 0.16
0 0 -1 0.32 0.11
0 0 -2 1899.81 65.22
0 0 2 1887.62 65.48
0 0 3 1.46 0.51
0 0 -3 0.17 0.25
0 0 4 1854.91 62.68
0 0 -4 1743.85 62.18
0 0 -5 0.51 0.44
0 0 5 0.28 0.43
0 0 6 418.78 16.73
0 0 7 0.83 0.61
0 0 8 106.90 6.37
0 0 9 0.86 0.85
0 0 9 -0.60 0.78
0 0 10 564.30 23.55
0 0 10 534.47 23.11
0 0 11 0.80 0.68
0 0 11 0.96 0.94
0 0 11 -0.38 0.65
0 0 12 89.08 7.43
0 0 12 105.10 7.56
0 0 12 99.79 7.67
0 0 12 97.47 8.12
0 0 13 0.47 0.94
0 0 13 -0.60 1.18
0 0 13 2.54 1.22
0 0 13 1.49 1.29
0 0 14 511.40 23.95
0 0 14 496.65 23.78
0 0 14 507.05 23.66
0 0 15 1.63 1.07
0 0 15 -0.55 0.94
0 0 15 -0.57 1.12
0 0 16 158.84 10.83
0 0 16 151.20 10.20
0 0 16 138.37 10.14
0 0 17 0.49 0.83
0 0 17 -0.47 1.04
0 0 18 191.97 11.22
0 0 19 0.35 0.68
0 0 20 140.07 8.98
0 0 21 0.27 0.59
0 -1 0 -0.08 0.32
0 -1 1 24.13 1.15
0 -1 1 23.68 1.52
0 1 1 24.31 1.17
0 -1 2 335.75 12.33
0 1 2 342.78 12.38
0 1 3 412.92 14.81
0 -1 3 383.53 14.68
0 1 4 134.11 6.07
0 -1 -4 137.50 6.70
0 -1 4 134.71 6.03
0 1 5 1434.92 49.69
0 -1 5 1365.72 49.51
0 -1 -5 1373.43 50.26
0 -1 -6 521.18 21.12
0 -1 6 524.79 20.46
0 1 6 545.35 20.68
0 -1 7 325.82 13.87
0 1 7 329.06 13.98
0 -1 8 98.83 5.98
0 1 8 100.91 6.14
0 1 8 102.56 6.51
0 -1 9 2262.45 82.20
0 1 9 2342.83 82.57
0 -1 9 2221.93 82.25
0 1 9 2372.54 83.02
0 -1 9 2292.57 82.51
0 1 9 2266.52 82.70
0 1 10 19.29 2.86
0 -1 10 21.62 2.88
0 1 10 18.28 2.70
0 -1 10 23.18 3.03
0 -1 11 850.43 33.30
0 1 11 843.71 33.26
0 1 11 875.68 33.91
0 -1 11 807.39 34.22
0 -1 11 751.06 33.99
0 1 11 837.45 34.60
0 -1 11 810.45 34.36
0 -1 11 784.22 33.24
0 1 12 99.82 7.32
0 -1 12 72.11 6.45
0 1 12 78.13 6.46
0 -1 12 82.98 6.56
0 -1 12 84.81 7.47
0 -1 12 75.02 7.08
0 1 12 66.19 6.91
0 -1 12 75.21 7.08
0 -1 13 90.99 7.63
0 -1 13 98.82 8.52
0 1 13 113.32 8.22
0 -1 13 110.43 8.94
0 -1 13 112.95 8.11
0 1 13 93.48 7.82
0 -1 13 104.07 7.34
0 -1 14 471.22 20.99
0 1 14 482.37 22.56
0 -1 14 403.49 22.44
0 1 14 451.53 21.82
0 -1 14 483.31 22.54
0 -1 14 455.11 21.82
0 -1 15 27.79 3.72
0 -1 15 23.60 3.78
0 -1 15 34.35 4.66
0 1 15 27.40 4.24
0 -1 15 33.61 4.95
0 1 15 29.58 4.29
0 -1 16 12.77 2.48
0 -1 16 15.16 3.33
0 -1 17 173.03 12.15
0 -1 17 187.94 10.60
0 -1 17 187.47 12.36
0 -1 18 68.41 6.70
0 -1 18 66.96 6.50
0 1 18 71.20 6.33
0 -1 19 105.09 8.65
0 -1 19 115.51 7.87
0 -1 19 115.36 8.19
0 1 19 107.38 7.52
0 -1 20 -0.42 1.01
0 -1 20 0.26 0.57
0 1 20 1.15 0.89
0 -1 20 -0.31 0.61
0 -1 21 29.19 3.11
0 -2 0 131.04 6.55
0 -2 -1 13.56 1.80
0 -2 -2 821.51 31.09
0 -2 3 2.48 0.49
0 2 3 2.17 0.49
0 2 4 64.01 3.35
0 -2 4 52.99 3.06
0 -2 -4 55.19 4.48
0 2 5 388.92 14.71
0 -2 5 354.99 14.37
0 -2 -5 361.83 16.46
0 -2 6 177.49 8.33
0 2 6 192.44 8.69
0 -2 7 28.47 2.67
0 2 7 29.50 2.82
0 -2 8 266.01 12.75
0 2 8 280.42 13.12
0 -2 8 284.89 12.70
0 2 8 296.96 13.06
0 -2 9 63.17 5.11
0 2 9 67.81 5.37
0 2 9 75.87 5.45
0 -2 9 75.64 5.28
0 -2 -9 74.27 6.17
0 -2 10 246.99 9.34
0 -2 10 225.75 8.60
0 -2 10 242.14 11.66
0 2 10 256.64 9.44
0 2 10 258.57 9.91
0 -2 11 -0.47 0.08
0 -2 11 0.58 2.07
0 -2 11 99.23 7.32
0 -2 11 109.49 8.15
0 -2 11 110.15 6.67
0 -2 11 95.73 6.00
0 2 11 101.29 6.57
0 2 11 113.30 6.67
0 2 12 26.72 3.78
0 -2 12 35.26 5.12
0 -2 12 31.50 4.49
0 -2 12 31.12 4.71
0 2 12 29.45 4.11
0 -2 12 33.37 4.09
0 -2 12 42.23 5.04
0 -2 12 34.58 4.37
0 -2 13 0.67 0.93
0 -2 13 0.72 1.41
0 -2 13 1.73 1.04
0 -2 13 0.62 0.87
0 -2 13 -0.58 1.27
0 2 13 0.92 0.91
0 -2 13 0.55 1.08
0 -2 14 1.82 1.34
0 -2 14 1.79 1.44
0 -2 14 3.39 1.58
0 -2 14 2.76 1.67
0 -2 14 2.23 1.47
0 -2 15 67.78 7.79
0 -2 15 75.98 7.23
0 -2 15 86.68 8.38
0 -2 16 142.72 11.01
0 -2 16 146.71 10.19
0 -2 16 130.80 10.96
0 -2 17 251.58 14.50
0 -2 17 211.29 12.62
0 -2 17 214.21 14.17
0 2 18 85.00 6.78
0 -2 18 81.11 7.49
0 -2 18 98.87 7.91
0 -2 19 13.69 2.57
0 2 19 15.70 2.45
0 -2 19 15.44 2.68
0 -2 20 21.51 2.76
0 -2 20 33.71 3.18
0 -3 0 1.92 1.07
0 -3 0 0.71 0.79
0 -3 -1 1200.19 47.15
0 -3 1 1258.26 47.28
0 -3 -1 1275.25 47.80
0 -3 1 1197.98 46.70
0 -3 2 0.72 0.80
0 -3 -3 563.77 24.75
0 -3 3 569.77 24.02
0 -3 -3 562.32 24.96
0 -3 -4 41.09 4.51
0 -3 -4 28.44 3.95
0 -3 -5 5.80 1.91
0 -3 -6 35.67 4.63
0 -3 6 42.20 5.12
0 -3 7 486.68 23.67
0 -3 7 478.49 22.53
0 -3 7 507.07 22.62
0 -3 -7 451.56 22.69
0 -3 8 31.28 4.23
0 -3 8 26.44 3.87
0 -3 -8 32.11 4.47
0 -3 9 181.96 10.36
0 -3 9 162.37 10.64
0 -3 9 157.76 9.83
0 -3 -9 168.86 10.19
0 -3 -10 32.51 4.78
0 -3 10 38.10 4.57
0 -3 10 28.66 4.67
0 -3 10 41.93 5.39
0 -3 10 35.30 5.34
0 -3 11 180.44 13.06
0 -3 11 219.32 14.57
0 -3 11 228.99 14.01
0 -3 -11 206.88 13.27
0 -3 11 177.14 11.86
0 -3 12 4.16 1.70
0 -3 12 4.06 2.11
0 -3 12 4.07 2.01
0 -3 12 3.72 2.08
0 -3 13 18.30 3.92
0 -3 13 14.39 3.55
0 -3 13 15.56 3.51
0 -3 13 16.07 3.20
0 -3 14 28.40 4.72
0 -3 14 21.00 3.54
0 -3 14 22.74 4.21
0 -3 15 180.89 12.37
0 -3 16 5.39 2.07
0 -3 16 7.46 2.47
0 3 17 59.68 5.35
0 -3 17 67.75 6.42
0 -3 18 0.38 0.83
0 3 18 0.60 0.66
0 -3 18 1.55 1.01
0 -3 19 55.37 4.39
0 -3 19 72.75 5.08
0 -4 0 16.28 3.29
0 -4 1 11.63 2.92
0 -4 1 11.86 2.98
0 -4 1 14.68 3.00
0 -4 1 9.05 2.59
0 -4 -1 10.18 2.73
0 -4 -1 16.61 3.47
0 -4 2 213.41 13.84
0 -4 2 213.13 13.29
0 -4 -2 221.77 14.29
0 -4 -2 232.26 14.23
0 -4 2 206.51 13.39
0 -4 2 232.73 14.08
0 -4 3 6.36 2.18
0 -4 3 13.06 3.06
0 -4 3 13.75 3.19
0 -4 3 15.86 3.24
0 -4 3 12.10 2.79
0 -4 -3 7.92 2.46
0 -4 3 11.66 3.04
0 -4 -4 98.69 8.92
0 -4 4 71.54 7.32
0 -4 4 69.28 7.28
0 -4 4 85.58 7.93
0 -4 4 73.72 7.67
0 -4 -4 101.72 8.94
0 -4 4 88.93 7.54
0 -4 5 0.67 1.15
0 -4 -5 2.05 1.50
0 -4 5 0.61 1.21
0 -4 -5 1.37 1.35
0 -4 5 1.20 1.18
0 -4 5 -0.58 0.98
0 -4 6 145.76 11.19
0 -4 6 151.63 10.92
0 -4 6 162.92 12.32
0 -4 -6 158.56 12.09
0 -4 -6 161.70 12.09
0 -4 6 172.20 10.71
0 -4 7 21.64 4.46
0 -4 -7 18.88 3.97
0 -4 7 14.38 3.41
0 -4 7 23.79 3.72
0 -4 8 293.14 17.10
0 -4 8 262.34 17.41
0 -4 -8 287.78 17.50
0 -4 8 258.55 15.39
0 -4 9 -0.68 1.17
0 -4 -9 0.74 1.94
0 -4 9 -0.80 1.76
0 -4 9 0.58 1.27
0 -4 10 666.92 31.69
0 -4 -10 655.17 32.02
0 -4 10 708.24 31.17
0 -4 11 8.10 2.83
0 -4 11 8.46 2.60
0 -4 11 4.77 2.36
0 -4 -11 6.26 2.39
0 -4 12 147.55 11.16
0 -4 12 118.80 10.87
0 -4 12 164.56 11.25
0 -4 -12 141.03 10.86
0 -4 13 13.56 3.03
0 -4 13 15.61 3.38
0 -4 13 11.26 3.13
0 -4 14 35.20 4.59
0 -4 14 25.61 4.03
0 -4 15 -0.90 1.09
0 -4 15 0.45 0.88
0 4 15 -0.31 0.62
0 -4 16 56.27 5.01
0 4 16 51.05 4.18
0 -5 0 -0.77 1.07
0 -5 0 -0.74 1.45
0 -5 0 0.77 1.52
0 -5 1 306.75 18.80
0 -5 1 298.35 18.04
0 -5 -1 289.92 18.29
0 -5 -1 317.23 19.24
0 -5 -2 3.88 2.17
0 -5 2 7.45 2.85
0 -5 -2 6.28 2.57
0 -5 2 4.45 1.99
0 -5 -2 6.68 2.73
0 -5 2 2.01 1.62
0 -5 -3 67.99 8.07
0 -5 -3 95.12 9.41
0 -5 3 81.70 8.45
0 -5 3 74.98 7.86
0 -5 3 72.37 7.35
0 -5 4 145.19 11.66
0 -5 4 151.31 11.92
0 -5 -4 171.64 13.14
0 -5 -5 31.00 5.41
0 -5 5 38.54 5.39
0 -5 5 29.38 5.04
0 -5 -5 33.02 5.67
0 -5 6 2.25 1.81
0 -5 -6 0.80 1.58
0 -5 -6 -0.76 1.06
0 -5 -7 19.74 4.11
0 -5 7 12.13 3.47
0 -5 -7 16.54 3.99
0 -5 8 -0.75 1.28
0 -5 -8 0.76 1.50
0 -5 -8 -0.69 1.36
0 -5 9 9.00 2.57
0 -5 9 15.37 3.70
0 -5 -9 12.20 3.26
0 -5 -9 12.59 3.25
0 -5 10 0.70 1.19
0 -5 -10 1.64 1.62
0 -5 10 2.59 1.53
0 -5 11 0.64 1.09
0 -5 11 3.68 1.57
0 -5 -12 11.27 2.85
0 -5 -13 7.22 2.17
0 -6 0 9.22 2.92
0 -6 1 7.68 2.71
0 -6 -1 12.57 2.98
0 -6 -2 -0.63 1.08
0 -6 2 -0.61 1.34
0 -6 -3 -0.65 1.29
0 -6 -3 -0.65 1.11
0 -6 -4 -0.65 1.44
0 -6 -4 -0.63 1.39
0 -6 -5 35.42 5.21
0 -6 -5 32.42 4.83
0 -6 -6 28.95 4.41
0 -6 -6 24.39 4.23
0 -6 -7 16.00 3.31
0 -6 -7 15.38 3.24
0 -6 -8 94.04 7.34
0 -6 -9 0.33 0.93
0 -6 -10 3.70 1.41
-1 0 22 10.20 1.51
-1 0 21 -0.31 0.69
-1 0 21 0.35 0.84
-1 0 20 64.23 6.26
-1 0 20 77.92 6.50
-1 0 19 0.68 0.82
-1 0 18 204.00 11.67
-1 0 17 -0.57 0.97
-1 0 16 3.99 1.64
-1 0 16 1.75 1.63
-1 0 16 3.92 1.91
-1 0 15 -0.55 0.94
-1 0 15 -0.51 0.87
-1 0 15 -0.57 1.26
-1 0 14 452.60 21.91
-1 0 14 456.98 22.16
-1 0 14 486.15 22.79
-1 0 13 0.47 1.04
-1 0 13 -0.48 0.95
-1 0 13 -0.50 0.99
-1 0 12 513.75 22.98
-1 0 12 555.23 23.52
-1 0 11 0.77 0.85
-1 0 10 565.50 23.85
-1 0 9 -0.29 0.57
-1 0 8 1775.64 64.23
-1 0 7 1.31 0.78
-1 0 6 1663.59 59.52
-1 0 5 -0.16 0.54
-1 0 4 153.87 6.98
-1 0 3 0.35 0.44
-1 0 2 2361.77 81.84
-1 0 1 1.78 0.54
-1 0 0 5463.16 187.67
-1 0 -1 3.64 0.57
-1 0 -2 635.44 22.71
1 0 3 0.53 0.50
1 0 4 133.21 6.19
-1 0 -5 0.25 0.46
1 0 5 0.32 0.49
1 0 6 440.51 17.49
-1 0 -6 430.22 16.88
1 0 7 0.22 0.58
-1 0 -7 0.17 0.37
-1 0 -8 4004.70 139.90
1 0 8 4040.95 141.07
1 0 8 3996.77 140.72
1 0 9 0.30 0.72
-1 0 -9 -0.22 0.49
1 0 9 0.32 0.55
1 0 10 80.23 6.03
1 0 10 87.55 6.40
1 0 11 0.39 0.77
1 0 11 -0.41 0.58
1 0 11 -0.52 0.89
1 0 11 1.57 1.26
1 0 12 652.70 27.65
1 0 12 574.87 28.29
1 0 12 659.87 29.06
1 0 12 621.02 27.05
1 0 13 -0.49 0.68
1 0 13 -0.64 1.27
1 0 14 124.06 9.04
1 0 14 129.65 10.53
1 0 14 122.55 9.63
1 0 15 0.51 1.00
1 0 15 -0.71 1.72
1 0 15 -0.59 1.17
1 0 16 291.03 16.27
1 0 16 282.84 15.46
1 0 17 1.51 1.40
1 0 17 -0.47 0.92
1 0 18 555.76 24.28
1 0 18 560.17 24.42
1 0 19 -0.33 0.73
1 0 20 79.86 5.77
1 0 20 65.02 4.72
1 0 21 0.24 0.47
-1 -1 21 27.33 3.18
-1 -1 21 29.07 2.92
-1 1 21 28.69 3.26
-1 1 21 36.32 3.54
-1 -1 20 48.27 5.09
-1 1 20 30.96 3.46
-1 1 20 41.88 4.57
-1 -1 20 48.19 4.59
-1 -1 19 242.95 14.53
-1 1 19 233.95 12.69
-1 -1 19 252.99 13.87
-1 -1 19 232.32 12.72
-1 -1 18 0.49 0.84
-1 -1 18 -0.58 1.14
-1 -1 18 0.68 1.49
-1 1 17 161.69 10.82
-1 -1 17 134.31 8.66
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-7 2 -3 115.48 8.66
-7 -2 -3 124.91 9.43
7 -2 3 129.24 9.57
7 -2 3 110.15 9.18
7 2 3 105.75 9.25
-7 -2 -3 111.51 8.37
7 -2 4 23.38 4.30
7 2 4 21.54 4.14
-7 -2 -4 22.63 4.11
-7 2 -4 31.20 4.67
7 -2 4 25.41 4.34
7 -2 5 53.03 6.36
7 2 5 55.79 6.59
-7 -2 -5 50.06 5.88
-7 2 -5 49.80 5.99
7 -2 5 47.56 6.05
7 -2 6 111.47 9.13
7 2 6 72.34 7.71
-7 -2 -6 81.25 7.69
-7 2 -6 91.63 8.08
7 -2 6 114.82 9.02
7 -2 7 5.71 2.18
7 2 7 4.16 1.86
-7 -2 -7 3.70 1.74
-7 2 -7 4.95 2.03
7 -2 7 5.71 2.26
7 -2 8 27.84 4.22
7 2 8 19.87 3.84
-7 -2 -8 25.28 3.81
-7 2 -8 27.94 4.04
7 -2 8 28.21 4.11
-7 -2 -9 15.53 2.75
-7 2 -9 14.95 2.88
7 -2 9 20.38 3.31
7 2 10 2.74 1.29
-7 2 -10 6.15 1.78
7 -2 10 4.31 1.50
7 2 11 12.55 2.16
7 -2 11 10.88 2.05
7 -2 12 23.67 2.85
-7 -3 15 13.88 2.11
-7 -3 14 3.62 1.34
-7 -3 13 73.12 6.12
-7 -3 12 2.55 1.59
-7 -3 12 5.28 2.01
-7 -3 11 111.25 8.99
-7 -3 11 111.23 9.05
7 -3 -11 113.97 8.55
7 -3 -10 10.67 2.68
-7 -3 10 11.05 2.99
-7 -3 9 27.89 4.74
-7 -3 9 34.36 5.06
7 -3 -9 35.64 5.05
-7 -3 8 23.55 4.26
-7 -3 8 21.25 4.10
-7 -3 7 13.04 3.19
-7 -3 7 8.85 2.87
-7 -3 6 23.52 4.46
-7 -3 6 33.05 5.16
-7 -3 5 174.49 12.82
-7 -3 4 6.79 2.42
-7 -3 3 30.45 4.86
-7 -3 2 -0.64 1.08
-7 -3 1 15.74 3.64
-7 -3 0 4.19 2.18
7 -3 1 54.25 6.68
-7 -3 -1 47.24 6.12
7 -3 2 13.46 3.33
-7 -3 -2 6.45 2.31
7 -3 3 107.87 9.41
-7 -3 -3 104.36 8.98
-7 -3 -4 13.96 3.02
7 -3 4 3.77 1.87
-7 -3 -5 28.40 4.05
7 -3 5 30.36 4.61
7 -3 6 14.87 3.25
7 -3 7 85.57 7.38
7 -3 8 0.87 1.06
7 -3 9 21.32 3.05
7 -3 10 0.87 0.76
7 -3 11 24.92 2.45
-7 -4 13 3.87 1.02
7 -4 -10 29.17 3.62
7 -4 -9 11.15 2.54
-7 -4 9 11.47 2.55
-7 -4 9 6.04 1.96
7 -4 -8 15.44 3.09
-7 -4 8 10.37 2.49
7 -4 -7 6.43 2.05
-7 -4 7 1.96 1.28
-7 -4 6 69.84 6.65
7 -4 -6 78.76 7.35
7 -4 -5 25.44 4.20
-7 -4 5 25.79 3.92
-7 -4 4 20.28 3.47
7 -4 -3 9.26 2.58
-7 -4 3 11.91 2.62
-7 -4 2 71.45 6.32
7 -4 -2 100.33 8.29
7 -4 -1 1.61 1.40
7 -4 0 55.81 6.19
-7 -4 0 40.93 5.44
7 -4 0 49.13 5.46
7 -4 1 0.45 0.89
7 -4 1 1.67 1.46
-7 -4 -1 2.80 1.56
7 -4 2 63.12 6.32
-7 -4 -2 45.92 5.41
-7 -4 -3 2.92 1.44
7 -4 3 1.01 1.41
-7 -4 -4 60.54 5.63
7 -4 4 64.25 6.11
-7 -4 -4 60.02 5.68
-7 -4 -5 0.32 0.63
-7 -4 -5 0.37 0.63
7 -4 5 0.42 0.93
7 -4 6 41.94 4.41
7 -4 7 2.81 1.16
7 -4 8 17.85 2.28
-7 -5 5 22.24 2.75
7 -5 -4 3.84 1.39
-7 -5 4 8.01 1.78
-7 -5 3 24.10 3.24
7 -5 -3 30.15 3.45
7 -5 -2 5.59 1.66
7 -5 -1 12.60 2.26
-7 -5 1 15.11 2.50
-7 -5 0 0.32 0.55
7 -5 0 0.31 0.61
-7 -5 -1 -0.29 0.75
7 -5 1 0.58 0.76
-7 -5 -2 0.24 0.63
7 -5 2 2.64 1.04
7 -5 3 6.86 1.37
-8 0 15 0.30 0.58
-8 0 14 78.82 6.07
-8 0 13 -0.40 0.69
-8 0 12 78.55 6.72
-8 0 11 0.50 0.99
-8 0 10 2.70 1.41
-8 0 9 -0.57 1.58
-8 0 8 24.81 4.36
-8 0 7 -1.22 1.47
-8 0 6 11.87 3.10
-8 0 5 -1.49 2.07
-8 0 5 -0.64 2.08
-8 0 5 0.64 0.89
-8 0 4 225.27 15.78
-8 0 4 232.69 15.06
-8 0 3 -2.57 2.37
-8 0 3 -0.64 0.63
-8 0 2 105.04 9.19
-8 0 2 102.46 9.01
8 0 -1 -1.73 2.08
-8 0 1 -0.65 2.23
-8 0 1 -0.62 1.22
8 0 0 112.40 10.71
8 0 0 122.56 11.41
8 0 1 -0.84 1.17
8 0 2 122.53 11.08
-8 0 -2 119.47 10.14
8 0 3 -0.80 1.76
-8 0 -3 -0.67 1.32
8 0 4 234.87 15.76
-8 0 -4 223.16 14.66
8 0 5 0.73 1.60
-8 0 -5 0.63 1.39
8 0 6 11.56 3.11
-8 0 -6 17.86 3.51
8 0 7 -0.62 1.50
-8 0 -7 -0.55 1.34
8 0 8 -0.55 1.44
-8 0 -8 -0.50 0.86
8 0 9 -0.48 1.15
-8 0 -9 -0.88 1.50
8 0 10 53.05 5.14
-8 0 -10 60.30 5.23
8 0 11 -0.30 0.58
-8 -1 16 4.89 1.28
-8 -1 15 8.40 1.58
-8 1 15 12.72 1.92
-8 -1 14 8.58 1.79
-8 1 14 7.45 1.67
-8 -1 13 23.58 3.19
-8 1 13 18.54 2.82
-8 -1 12 0.88 0.97
-8 -1 12 -1.23 1.40
-8 1 12 -0.41 1.28
-8 -1 11 8.34 2.31
-8 -1 11 4.12 1.57
-8 1 11 5.04 1.70
-8 -1 10 -0.50 2.02
-8 1 10 -0.50 1.84
-8 -1 9 50.79 5.62
-8 1 9 46.12 5.38
-8 -1 8 2.76 1.72
-8 1 8 1.66 1.73
-8 -1 7 121.88 9.63
-8 1 7 128.98 9.89
-8 -1 6 1.18 1.30
-8 1 6 0.59 1.16
-8 -1 5 99.95 8.73
-8 1 5 97.15 8.59
-8 -1 5 88.34 7.93
-8 -1 4 -0.61 2.10
-8 1 4 -1.85 2.27
-8 -1 3 44.70 5.77
-8 1 3 57.92 6.55
8 -1 -2 12.26 3.53
8 1 -2 9.24 3.33
8 -1 -1 38.82 5.98
8 1 -1 31.53 5.55
8 -1 0 -0.80 1.57
8 1 0 2.45 2.13
8 -1 1 10.99 3.20
8 1 1 4.02 2.25
8 -1 2 8.43 2.85
8 1 2 14.88 3.72
8 -1 3 33.25 5.37
8 1 3 37.72 5.77
-8 -1 -3 32.54 4.91
-8 1 -3 30.37 4.76
8 -1 4 1.41 1.55
8 1 4 3.59 2.00
-8 -1 -4 3.64 1.98
-8 1 -4 2.46 1.71
8 -1 5 188.14 12.87
8 1 5 174.25 12.57
-8 -1 -5 176.93 11.98
-8 1 -5 156.58 11.49
8 -1 6 0.62 1.22
8 1 6 1.26 1.52
-8 -1 -6 1.09 1.07
-8 1 -6 0.55 1.34
8 -1 7 49.02 5.73
8 1 7 50.57 5.79
-8 -1 -7 36.02 4.64
-8 1 -7 31.61 4.42
8 -1 8 52.69 5.57
8 1 8 50.31 5.48
-8 -1 -8 55.81 5.53
-8 1 -8 46.99 5.21
-8 -1 -9 74.02 6.07
-8 1 -9 77.79 6.25
8 -1 10 3.21 1.19
8 1 10 5.32 1.51
-8 -1 -10 3.42 1.23
-8 1 -10 3.83 1.26
8 -1 11 33.40 3.06
8 1 11 34.62 3.18
-8 -2 15 4.51 1.19
-8 -2 14 18.59 2.69
-8 -2 13 18.84 3.01
-8 -2 13 21.89 2.91
-8 -2 12 42.26 3.92
-8 2 12 34.10 3.44
-8 -2 12 46.29 4.80
-8 -2 12 50.02 5.17
-8 -2 11 0.51 1.00
-8 2 11 0.62 0.68
-8 -2 11 0.48 0.96
-8 -2 10 31.46 4.44
-8 -2 10 33.24 4.59
-8 -2 10 27.57 3.42
-8 2 10 22.41 3.12
-8 -2 9 35.13 4.10
-8 2 9 37.85 4.24
-8 -2 9 41.97 5.25
-8 -2 8 3.48 1.72
-8 -2 8 5.10 1.74
-8 2 8 6.00 1.80
-8 -2 7 1.75 1.41
-8 -2 7 1.34 1.08
-8 2 7 1.36 1.26
-8 2 6 75.24 6.68
-8 -2 6 74.99 6.69
-8 -2 6 77.14 7.41
-8 -2 5 15.06 3.26
-8 -2 5 19.71 3.31
-8 2 5 20.40 3.41
-8 -2 4 2.12 1.38
-8 -2 4 2.46 1.46
-8 2 4 0.50 1.30
8 -2 -4 5.94 2.35
8 2 -4 1.41 1.71
-8 -2 3 2.50 1.64
-8 2 3 1.52 1.58
8 -2 -3 5.27 2.16
8 2 -3 1.41 1.55
8 -2 -2 9.69 2.59
-8 -2 2 8.65 2.38
-8 2 2 12.88 2.89
8 -2 -2 11.13 2.91
8 2 -2 13.22 3.31
8 -2 -1 2.04 1.43
-8 -2 1 2.54 1.51
-8 2 1 3.10 1.76
8 -2 -1 1.94 1.81
8 2 -1 2.74 1.66
8 -2 0 15.75 3.14
8 -2 0 15.86 3.53
8 2 0 24.13 4.32
8 -2 1 1.23 1.36
8 2 1 5.20 2.13
8 -2 1 4.01 1.71
8 -2 2 24.76 4.07
8 2 2 16.75 3.46
8 -2 2 16.10 3.07
8 -2 3 2.24 1.35
8 2 3 3.53 1.64
8 -2 3 1.40 1.13
8 -2 4 68.70 6.71
8 2 4 71.13 6.87
8 -2 4 63.10 5.99
8 -2 5 6.72 1.96
8 2 5 8.08 2.24
8 -2 5 5.22 1.69
8 -2 6 4.25 1.57
8 2 6 2.24 1.25
8 -2 6 2.85 1.22
8 2 7 4.21 1.57
8 -2 7 6.63 1.58
8 2 8 -0.31 0.91
8 -2 8 1.63 0.79
8 2 9 3.25 0.99
8 -2 10 0.58 0.47
-8 -3 13 13.25 1.98
-8 -3 12 6.64 1.61
-8 -3 12 6.80 1.61
-8 -3 11 40.76 4.31
8 -3 -10 7.72 1.87
-8 -3 10 3.74 1.54
8 -3 -9 2.27 1.35
-8 -3 9 2.25 1.26
-8 -3 9 4.17 1.65
-8 -3 8 67.66 6.71
-8 -3 8 66.42 6.27
8 -3 -8 75.90 6.93
-8 -3 7 16.62 3.19
-8 -3 7 23.45 3.73
-8 -3 6 21.94 3.82
-8 -3 6 27.59 3.97
-8 -3 5 105.67 8.41
-8 -3 5 82.07 7.27
-8 -3 4 11.20 2.76
-8 -3 3 40.91 5.04
8 -3 -2 30.62 4.32
-8 -3 2 23.61 3.77
-8 -3 1 40.44 4.72
8 -3 -1 43.85 5.07
8 -3 0 17.61 3.22
-8 -3 0 8.87 2.21
8 -3 1 28.46 4.06
8 -3 2 2.26 1.26
8 -3 3 109.16 7.92
8 -3 4 5.40 1.67
8 -3 5 22.84 3.05
8 -3 6 -0.29 0.57
8 -3 7 33.62 3.09
8 -4 -7 18.57 2.71
-8 -4 7 12.25 2.15
-8 -4 6 74.56 5.59
8 -4 -6 85.86 6.44
8 -4 -5 8.94 1.92
-8 -4 5 7.38 1.72
-8 -4 4 34.20 3.43
8 -4 -4 29.75 3.55
8 -4 -4 39.23 4.27
8 -4 -3 5.02 1.53
8 -4 -3 2.12 1.26
-8 -4 3 2.69 1.03
8 -4 -2 24.85 3.29
8 -4 -2 30.96 3.68
8 -4 -1 -0.35 0.91
8 -4 -1 0.34 0.58
8 -4 0 3.71 1.38
8 -4 1 3.19 1.26
-8 -4 -2 12.81 2.12
8 -4 2 7.28 1.65
-8 -4 -3 2.04 0.87
8 -4 3 5.64 1.36
8 -4 4 4.05 1.06
-9 0 13 -0.24 0.48
-9 0 11 -0.33 0.66
-9 0 10 27.74 3.50
-9 0 9 -0.42 0.92
-9 0 8 2.24 1.40
-9 0 7 -0.47 1.47
-9 0 6 0.49 0.97
-9 0 5 0.51 1.12
9 0 -4 56.14 6.82
-9 0 4 44.39 5.38
-9 0 3 -0.53 1.65
9 0 -3 -0.72 2.00
-9 0 1 -0.53 1.48
9 0 0 56.66 6.83
9 0 1 -0.66 1.30
9 0 2 92.73 8.56
9 0 3 0.58 1.41
9 0 4 284.86 15.88
9 0 5 -0.49 1.17
9 0 6 15.70 2.79
9 0 7 -0.36 0.70
-9 -1 13 14.04 2.00
-9 -1 12 4.26 1.26
-9 -1 12 4.15 1.18
-9 -1 11 6.11 1.53
-9 -1 11 3.56 1.43
-9 -1 11 4.07 1.22
-9 1 11 4.36 1.26
-9 -1 10 11.80 2.18
-9 -1 10 7.11 1.89
-9 -1 10 8.01 1.82
-9 1 10 6.02 1.60
-9 -1 9 56.86 5.12
-9 1 9 55.84 5.05
-9 -1 9 52.61 4.88
-9 -1 8 3.96 1.47
-9 -1 8 2.42 1.32
-9 1 8 6.87 1.87
-9 -1 7 51.80 5.27
-9 1 7 53.62 5.26
-9 -1 6 0.90 1.08
-9 1 6 2.25 1.40
9 -1 -5 102.78 9.29
9 1 -5 116.71 9.92
-9 -1 5 114.43 8.40
-9 1 5 109.17 8.29
-9 -1 4 -1.91 2.30
-9 1 4 0.96 1.83
9 -1 -4 -2.59 2.86
9 1 -4 0.67 2.29
-9 -1 3 36.33 4.63
-9 1 3 35.50 4.57
9 -1 -3 45.39 5.85
9 1 -3 33.52 5.23
-9 -1 2 -2.44 2.26
9 1 -2 -1.33 2.36
-9 -1 1 15.07 3.25
-9 1 1 15.16 3.27
9 -1 -1 12.65 3.50
9 1 -1 13.69 3.72
-9 -1 0 19.12 3.39
-9 1 0 12.99 2.95
9 -1 0 19.66 3.88
9 -1 1 13.52 3.14
9 1 1 7.86 2.41
9 -1 2 75.35 7.23
9 1 2 69.47 7.02
9 -1 3 5.15 1.91
9 1 3 6.35 2.10
9 -1 4 -0.47 0.93
9 1 4 0.48 1.17
9 -1 5 27.20 3.64
9 1 5 27.09 3.69
9 -1 6 -0.36 0.61
9 1 6 0.73 0.89
9 -1 8 4.02 1.06
9 1 8 6.42 1.29
-9 -2 12 12.43 1.81
-9 -2 12 19.34 2.08
-9 -2 11 0.25 0.43
-9 -2 11 0.27 0.61
-9 -2 10 2.28 0.94
-9 -2 10 2.70 1.16
9 2 -10 1.82 0.95
-9 -2 9 11.35 2.12
9 2 -9 14.79 2.48
-9 -2 8 3.47 1.29
-9 2 8 5.97 1.41
-9 -2 7 0.62 0.69
-9 2 7 -0.58 0.70
9 2 -7 -0.44 0.96
-9 -2 6 22.76 2.85
-9 2 6 19.24 2.64
9 -2 -6 16.08 2.84
9 2 -6 18.94 3.22
-9 -2 5 2.26 1.19
-9 2 5 2.61 1.20
9 -2 -5 0.44 1.37
9 2 -5 3.82 1.70
-9 -2 4 18.35 2.67
-9 2 4 16.52 2.59
9 -2 -4 18.86 3.22
9 2 -4 24.30 3.79
-9 -2 3 0.34 1.11
-9 2 3 -1.03 1.27
9 -2 -3 0.45 1.41
9 2 -3 -0.97 1.66
-9 -2 2 8.54 1.99
-9 2 2 9.69 2.08
9 -2 -2 13.39 2.77
9 2 -2 13.45 2.94
-9 -2 1 4.39 1.60
-9 2 1 2.74 1.48
9 -2 -1 7.36 2.14
9 2 -1 4.65 1.89
-9 -2 0 14.79 2.40
-9 2 0 12.36 2.18
9 -2 0 10.73 2.31
9 2 0 16.37 2.93
-9 -2 -1 21.99 2.86
-9 2 -1 19.46 2.75
9 2 2 38.16 4.16
-9 2 -2 33.07 3.46
9 2 3 3.73 1.34
-9 2 -3 2.70 1.03
9 2 4 5.15 1.36
-9 -3 9 0.24 0.59
-9 -3 8 9.72 1.85
-9 -3 7 18.69 2.65
9 -3 -7 21.87 2.90
-9 -3 6 3.78 1.40
9 -3 -6 6.42 1.69
-9 -3 5 27.68 3.32
9 -3 -5 25.86 3.41
-9 -3 4 10.85 2.06
-9 -3 3 27.31 3.08
9 -3 -3 25.20 3.31
-9 -3 2 0.26 0.62
9 -3 -2 0.36 0.79
9 -3 -1 4.96 1.47
10 0 -10 14.54 2.17
10 0 -9 0.65 0.78
10 0 -8 22.51 3.09
-10 0 8 18.71 2.33
-10 0 7 -0.27 0.60
10 0 -7 -0.39 0.87
-10 0 6 5.81 1.48
10 0 -6 9.16 2.14
-10 0 5 -0.61 0.67
10 0 -5 -0.43 1.12
-10 0 4 13.50 2.29
10 0 -4 20.18 3.28
-10 0 3 -1.59 1.13
10 0 -3 -0.88 1.50
-10 0 2 19.36 2.72
10 0 -2 15.10 2.85
-10 0 1 -0.31 0.75
10 0 -1 -0.41 0.82
-10 0 0 0.90 0.78
10 0 0 2.35 1.16
-10 0 -1 -0.28 0.56
10 0 1 -0.36 0.72
10 0 2 19.75 2.78
10 0 3 0.57 0.69
10 0 4 53.84 4.08
-10 -1 9 4.75 1.08
10 -1 -9 2.68 0.94
10 1 -9 4.14 1.17
-10 -1 8 3.34 1.11
10 -1 -8 4.88 1.30
10 1 -8 4.54 1.40
10 -1 -7 7.35 1.72
10 1 -7 10.07 2.03
-10 -1 6 19.32 2.33
-10 1 6 13.48 2.00
10 -1 -6 17.85 2.70
10 1 -6 16.55 2.66
-10 -1 5 10.36 1.83
-10 1 5 7.01 1.54
10 -1 -5 7.89 1.99
10 1 -5 7.88 1.91
-10 -1 4 6.69 1.61
-10 1 4 4.30 1.28
10 -1 -4 4.04 1.54
10 1 -4 3.45 1.47
-10 -1 3 11.13 1.95
-10 1 3 12.26 2.01
10 -1 -3 11.40 2.32
10 1 -3 11.49 2.42
-10 -1 2 1.35 0.96
-10 1 2 2.44 1.10
10 -1 -2 2.87 1.42
10 1 -2 1.12 1.04
-10 -1 1 15.28 2.18
-10 1 1 15.63 2.24
10 -1 -1 20.64 2.91
10 1 -1 16.45 2.63
10 -1 0 0.97 0.84
10 1 0 1.34 0.93
10 -1 1 13.57 2.16
10 1 1 12.26 2.10
10 -1 2 0.52 0.62
10 1 2 2.42 0.96
10 -1 3 20.51 2.26
10 1 3 18.79 2.23
-10 -2 7 3.09 0.96
-10 -2 6 42.18 3.49
-10 -2 5 3.51 1.04
-10 -2 4 18.11 2.26
-10 -2 3 4.80 1.15
-10 -2 2 1.52 0.70
0 0 0 0.00 0.00
TITL shS_162_IlGu_auto in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 8.462297 5.648705 17.453620 90.0000 98.7859 90.0000
ZERR 4.00 0.000228 0.000159 0.000355 0.0000 0.0022 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N Cu
UNIT 40.00 8.00 8.00 4.00
REM CrysAlisPro recorded range (K): Min=199.9; max=200.1; aver:200.0
TEMP -73
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 46561
_shelx_res_file
;
TITL shs_162_ilgu_auto_a.res in P2(1)/c
shs_162_ilgu_auto.res
created by SHELXL-2018/3 at 14:37:38 on 07-Sep-2023
REM Old TITL shS_162_IlGu_auto in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.409, Rweak 0.109, Alpha 0.016
REM 0.553 for 92 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 O4 Cu
CELL 1.54184 8.462297 5.648705 17.45362 90 98.7859 90
ZERR 2 0.000228 0.000159 0.000355 0 0.0022 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cu N O
UNIT 20 40 2 12 16
EQIV $1 1-X,0.5+Y,0.5-Z
EQIV $2 1-X,-0.5+Y,0.5-Z
EQIV $3 -1+X,0.5-Y,-0.5+Z
EQIV $4 -X,0.5+Y,0.5-Z
DANG 1.796 H4d_$1 O3
DANG 2.15 H4d_$1 H3a
L.S. 20
PLAN 5
SIZE 0.15 0.15 0.15
TEMP -73.16(11)
CONF
HTAB O4 O3_$2
HTAB O4 O1_$1
HTAB O4 O2_$1
HTAB N2 O4_$3
HTAB N3 O2_$4
HTAB O3 O2
HTAB O3 O4
HTAB C2 O3_$4
MORE -1
BOND $H
HTAB
fmap 2
acta
REM
REM
REM
WGHT 0.063600 0.430600
FVAR 0.62392
CU1 3 0.000000 0.000000 0.000000 10.50000 0.03785 0.04045 =
0.01822 -0.00083 -0.00118 0.00345
O4 5 0.660127 0.282928 0.295166 11.00000 0.05772 0.05861 =
0.03548 -0.00305 -0.00424 -0.00589
AFIX 3
H4D 2 0.663197 0.160498 0.265176 11.00000 -1.50000
H4E 2 0.733747 0.377068 0.282986 11.00000 -1.50000
AFIX 0
N2 4 -0.233795 0.379774 -0.050182 11.00000 0.04033 0.04091 =
0.02282 0.00301 -0.00203 0.00148
AFIX 43
H2 2 -0.253149 0.326001 -0.098018 11.00000 -1.20000
AFIX 0
N1 4 -0.134801 0.271564 0.008697 11.00000 0.03629 0.04169 =
0.02001 0.00164 -0.00030 0.00324
N3 4 -0.050720 0.354993 0.142350 11.00000 0.04423 0.04380 =
0.01955 -0.00312 0.00164 0.00150
AFIX 43
H3 2 -0.059104 0.455034 0.180169 11.00000 -1.20000
AFIX 0
O3 5 0.351307 0.431250 0.307188 11.00000 0.06176 0.06275 =
0.04184 0.00078 -0.00364 -0.00982
AFIX 3
H3A 2 0.280457 0.334940 0.282998 11.00000 -1.50000
H3B 2 0.442727 0.365820 0.303128 11.00000 -1.50000
AFIX 0
C1 1 -0.137571 0.409033 0.070522 11.00000 0.03412 0.03919 =
0.02451 -0.00014 0.00357 -0.00396
C2 1 -0.236528 0.604705 0.051562 11.00000 0.03930 0.04122 =
0.02965 -0.00086 0.00459 0.00041
AFIX 43
H2A 2 -0.257394 0.729896 0.084961 11.00000 -1.20000
AFIX 0
C4 1 -0.411156 0.726462 -0.079305 11.00000 0.04186 0.04912 =
0.04348 0.00851 -0.00035 0.00323
AFIX 137
H4A 2 -0.388986 0.707721 -0.132463 11.00000 -1.50000
H4B 2 -0.398069 0.893005 -0.063909 11.00000 -1.50000
H4C 2 -0.521048 0.676241 -0.076675 11.00000 -1.50000
AFIX 0
C3 1 -0.297698 0.578119 -0.025898 11.00000 0.03524 0.03911 =
0.03361 0.00409 0.00480 -0.00268
C5 1 0.046175 0.164169 0.160877 11.00000 0.04090 0.04171 =
0.01868 -0.00003 0.00314 -0.00635
O1 5 0.067740 0.013010 0.109679 11.00000 0.04784 0.04654 =
0.02052 -0.00088 -0.00280 0.00651
O2 5 0.115226 0.145582 0.229735 11.00000 0.04908 0.05005 =
0.01832 0.00224 -0.00264 -0.00390
HKLF 4
REM shs_162_ilgu_auto_a.res in P2(1)/c
REM wR2 = 0.1184, GooF = S = 1.048, Restrained GooF = 1.047 for all data
REM R1 = 0.0413 for 1401 Fo > 4sig(Fo) and 0.0487 for all 1634 data
REM 116 parameters refined using 2 restraints
END
WGHT 0.0636 0.4306
REM Instructions for potential hydrogen bonds
HTAB O4 O3_$2
HTAB O4 O1_$1
HTAB O4 O2_$1
HTAB N2 O4_$3
HTAB N3 O2_$4
HTAB O3 O2
HTAB O3 O4
HTAB C2 O3_$4
REM Highest difference peak 0.453, deepest hole -0.569, 1-sigma level 0.078
Q1 1 -0.0657 0.1734 0.0032 11.00000 0.05 0.45
Q2 1 -0.2773 0.4564 -0.0354 11.00000 0.05 0.33
Q3 1 -0.4721 0.5991 -0.1184 11.00000 0.05 0.29
Q4 1 -0.2621 0.6040 0.0177 11.00000 0.05 0.28
Q5 1 -0.3431 0.8464 -0.1034 11.00000 0.05 0.28
;
_shelx_res_checksum 71933
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.000000 0.000000 0.000000 0.0327(2) Uani d 1 . .
O O4 0.6601(3) 0.2829(4) 0.29517(11) 0.0518(6) Uani d 1 . .
H H4D 0.663197 0.160498 0.265176 0.078 Uiso d 1 . .
H H4E 0.733747 0.377068 0.282986 0.078 Uiso d 1 . .
N N2 -0.2338(3) 0.3798(4) -0.05018(12) 0.0354(5) Uani d 1 . .
H H2 -0.253149 0.326001 -0.098018 0.042 Uiso calc 1 . .
N N1 -0.1348(2) 0.2716(4) 0.00870(11) 0.0331(5) Uani d 1 . .
N N3 -0.0507(3) 0.3550(4) 0.14235(11) 0.0362(5) Uani d 1 . .
H H3 -0.059104 0.455034 0.180169 0.043 Uiso calc 1 . .
O O3 0.3513(3) 0.4313(5) 0.30719(12) 0.0567(6) Uani d 1 . .
H H3A 0.280457 0.334940 0.282998 0.085 Uiso d 1 . .
H H3B 0.442727 0.365820 0.303128 0.085 Uiso d 1 . .
C C1 -0.1376(3) 0.4090(5) 0.07052(14) 0.0327(5) Uani d 1 . .
C C2 -0.2365(3) 0.6047(5) 0.05156(15) 0.0368(6) Uani d 1 . .
H H2A -0.257394 0.729896 0.084961 0.044 Uiso calc 1 . .
C C4 -0.4112(3) 0.7265(6) -0.07931(17) 0.0455(7) Uani d 1 . .
H H4A -0.388986 0.707721 -0.132463 0.068 Uiso calc 1 . .
H H4B -0.398069 0.893005 -0.063909 0.068 Uiso calc 1 . .
H H4C -0.521048 0.676241 -0.076675 0.068 Uiso calc 1 . .
C C3 -0.2977(3) 0.5781(5) -0.02590(15) 0.0360(6) Uani d 1 . .
C C5 0.0462(3) 0.1642(5) 0.16088(13) 0.0339(6) Uani d 1 . .
O O1 0.0677(2) 0.0130(3) 0.10968(10) 0.0391(5) Uani d 1 . .
O O2 0.1152(2) 0.1456(4) 0.22973(9) 0.0400(5) Uani 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
Cu1 0.0378(3) 0.0405(4) 0.0182(3) 0.0035(2) -0.0012(2) -0.0008(2)
O4 0.0577(12) 0.0586(14) 0.0355(10) -0.0059(11) -0.0042(9) -0.0031(9)
N2 0.0403(11) 0.0409(13) 0.0228(10) 0.0015(10) -0.0020(8) 0.0030(9)
N1 0.0363(11) 0.0417(12) 0.0200(9) 0.0032(9) -0.0003(8) 0.0016(9)
N3 0.0442(12) 0.0438(13) 0.0196(9) 0.0015(10) 0.0016(8) -0.0031(9)
O3 0.0618(14) 0.0628(14) 0.0418(12) -0.0098(12) -0.0036(10) 0.0008(11)
C1 0.0341(12) 0.0392(14) 0.0245(11) -0.0040(11) 0.0036(9) -0.0001(11)
C2 0.0393(13) 0.0412(15) 0.0296(12) 0.0004(12) 0.0046(10) -0.0009(11)
C4 0.0419(14) 0.0491(18) 0.0435(15) 0.0032(13) -0.0004(12) 0.0085(13)
C3 0.0352(12) 0.0391(14) 0.0336(13) -0.0027(11) 0.0048(10) 0.0041(12)
C5 0.0409(13) 0.0417(14) 0.0187(11) -0.0064(12) 0.0031(9) 0.0000(10)
O1 0.0478(11) 0.0465(12) 0.0205(9) 0.0065(8) -0.0028(8) -0.0009(7)
O2 0.0491(10) 0.0501(11) 0.0183(8) -0.0039(9) -0.0026(7) 0.0022(8)
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'
Cu Cu -1.9646 0.5888 '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
N1 Cu1 N1 3 . 180.0 ?
O1 Cu1 N1 3 3 88.92(8) ?
O1 Cu1 N1 3 . 91.08(8) ?
O1 Cu1 N1 . . 88.92(8) ?
O1 Cu1 N1 . 3 91.08(8) ?
O1 Cu1 O1 . 3 180.0 ?
H4D O4 H4E . . 104.5 ?
N1 N2 H2 . . 124.3 ?
C3 N2 H2 . . 124.3 ?
C3 N2 N1 . . 111.5(2) ?
N2 N1 Cu1 . . 126.70(16) ?
C1 N1 Cu1 . . 127.60(17) ?
C1 N1 N2 . . 105.3(2) ?
C1 N3 H3 . . 116.4 ?
C5 N3 H3 . . 116.4 ?
C5 N3 C1 . . 127.2(2) ?
H3A O3 H3B . . 104.5 ?
N1 C1 N3 . . 122.1(2) ?
N1 C1 C2 . . 110.7(2) ?
N3 C1 C2 . . 127.2(2) ?
C1 C2 H2A . . 127.2 ?
C3 C2 C1 . . 105.5(2) ?
C3 C2 H2A . . 127.2 ?
H4A C4 H4B . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
N2 C3 C2 . . 107.0(2) ?
N2 C3 C4 . . 121.7(2) ?
C2 C3 C4 . . 131.4(3) ?
O1 C5 N3 . . 120.7(2) ?
O2 C5 N3 . . 117.9(2) ?
O2 C5 O1 . . 121.4(3) ?
C5 O1 Cu1 . . 132.59(17) ?
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
Cu1 N1 . 1.931(2) ?
Cu1 N1 3 1.931(2) ?
Cu1 O1 . 1.9140(17) ?
Cu1 O1 3 1.9140(17) ?
O4 H4D . 0.8701 ?
O4 H4E . 0.8698 ?
N2 H2 . 0.8800 ?
N2 N1 . 1.367(3) ?
N2 C3 . 1.341(4) ?
N1 C1 . 1.333(3) ?
N3 H3 . 0.8800 ?
N3 C1 . 1.387(3) ?
N3 C5 . 1.363(4) ?
O3 H3A . 0.8697 ?
O3 H3B . 0.8700 ?
C1 C2 . 1.396(4) ?
C2 H2A . 0.9500 ?
C2 C3 . 1.380(4) ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C4 H4C . 0.9800 ?
C4 C3 . 1.490(4) ?
C5 O1 . 1.269(3) ?
C5 O2 . 1.258(3) ?
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
O4 H4D O3 2_645 0.87 1.80 2.664(3) 171.4 yes
O4 H4E O1 2_655 0.87 2.44 2.930(3) 116.1 yes
O4 H4E O2 2_655 0.87 2.02 2.873(3) 167.4 yes
N2 H2 O4 4_465 0.88 1.99 2.863(3) 169.2 yes
N3 H3 O2 2 0.88 2.02 2.889(3) 168.8 yes
O3 H3A O2 . 0.87 1.89 2.756(3) 175.5 yes
O3 H3B O4 . 0.87 1.92 2.783(3) 168.9 yes
C2 H2A O3 2 0.95 2.43 3.340(4) 159.3 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cu1 N1 C1 N3 . . . . -7.3(4) ?
Cu1 N1 C1 C2 . . . . 172.53(18) ?
N2 N1 C1 N3 . . . . 179.7(2) ?
N2 N1 C1 C2 . . . . -0.4(3) ?
N1 N2 C3 C2 . . . . 1.1(3) ?
N1 N2 C3 C4 . . . . -179.4(2) ?
N1 C1 C2 C3 . . . . 1.1(3) ?
N3 C1 C2 C3 . . . . -179.1(3) ?
N3 C5 O1 Cu1 . . . . 5.3(4) ?
C1 N3 C5 O1 . . . . 1.3(4) ?
C1 N3 C5 O2 . . . . -179.9(2) ?
C1 C2 C3 N2 . . . . -1.3(3) ?
C1 C2 C3 C4 . . . . 179.3(3) ?
C3 N2 N1 Cu1 . . . . -173.46(18) ?
C3 N2 N1 C1 . . . . -0.5(3) ?
C5 N3 C1 N1 . . . . 0.0(4) ?
C5 N3 C1 C2 . . . . -179.9(3) ?
O2 C5 O1 Cu1 . . . . -173.44(18) ?
_cod_database_fobs_code 2022871