#------------------------------------------------------------------------------
#$Date: 2024-05-15 04:59:16 +0300 (Wed, 15 May 2024) $
#$Revision: 291858 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023128.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_2023128
loop_
_publ_author_name
'Breen, Olivia D.'
'Keene, Tony D.'
_publ_section_title
;
Crystal structure and Hirshfeld surface of a pentaaminecopper(II) complex
with urea and chloride
;
_journal_coeditor_code OO2003
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024004298
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Cu (N H3)5] Cl2, C1 H4 N2 O1'
_chemical_formula_moiety 'H15 Cu N5 2+, 2(Cl -), C1 H4 N2 O1'
_chemical_formula_sum 'C H19 Cl2 Cu N7 O'
_chemical_formula_weight 279.67
_chemical_name_common 'pentaaminecopper(II) chloride urea'
_chemical_name_systematic
;
Pentaaminecopper(II) dichloride--urea (1/1)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha 90
_cell_angle_beta 94.511(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.2214(2)
_cell_length_b 7.02300(10)
_cell_length_c 13.0537(3)
_cell_measurement_reflns_used 8370
_cell_measurement_temperature 100
_cell_measurement_theta_max 66.5890
_cell_measurement_theta_min 4.7490
_cell_volume 1116.94(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)
;
_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, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas'
_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 0.0588
_diffrn_reflns_av_unetI/netI 0.0262
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 12732
_diffrn_reflns_theta_full 66.567
_diffrn_reflns_theta_max 66.567
_diffrn_reflns_theta_min 4.773
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 7.007
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.22922
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.663
_exptl_crystal_description block
_exptl_crystal_F_000 580
_exptl_crystal_size_max 0.453
_exptl_crystal_size_mid 0.217
_exptl_crystal_size_min 0.118
_refine_diff_density_max 0.674
_refine_diff_density_min -0.799
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.078
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 130
_refine_ls_number_reflns 1977
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.078
_refine_ls_R_factor_all 0.0350
_refine_ls_R_factor_gt 0.0332
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+1.0977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0903
_refine_ls_wR_factor_ref 0.0920
_reflns_number_gt 1835
_reflns_number_total 1977
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file oo2003.cif
_cod_data_source_block I
_cod_database_code 2023128
_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 0.143
_shelx_estimated_absorpt_t_max 0.492
_shelx_hkl_file
;
0 0 -1 0.08 0.08
0 0 1 0.05 0.06
0 0 1 0.27 0.10
0 0 -1 0.04 0.07
0 0 1 0.07 0.07
0 0 2 1755.84 9.24
0 0 -2 1945.17 11.16
0 0 2 1866.45 10.34
0 0 -2 1976.31 11.47
0 0 2 1675.65 9.64
0 0 -3 -0.07 0.24
0 0 3 0.02 0.16
0 0 3 -0.04 0.23
0 0 -3 0.15 0.26
0 0 3 -0.16 0.28
0 0 4 8.48 1.01
0 0 -4 9.83 1.15
0 0 4 8.84 0.96
0 0 -4 8.34 1.09
0 0 -4 8.34 1.06
0 0 -5 0.18 0.30
0 0 5 -0.15 0.30
0 0 -5 -0.17 0.47
0 0 5 0.11 0.34
0 0 5 0.02 0.34
0 0 -5 0.54 0.47
0 0 6 660.71 10.99
0 0 6 668.88 10.22
0 0 -6 655.92 12.13
0 0 7 -0.64 0.50
0 0 7 0.10 0.47
0 0 -7 0.25 0.84
0 0 -7 -0.02 0.38
0 0 8 12.30 1.81
0 0 8 13.87 2.03
0 0 -8 11.00 1.92
0 0 9 -0.88 0.64
0 0 9 -0.49 0.66
0 0 10 80.98 5.49
0 0 10 77.08 4.91
0 0 -10 76.02 5.55
0 0 -10 85.21 5.80
0 0 11 -0.01 0.60
0 0 -11 2.30 1.39
0 0 -11 -0.23 0.94
0 0 -11 1.50 1.49
0 0 11 0.77 0.61
0 0 11 0.38 0.73
0 0 -12 723.08 17.64
0 0 -12 711.95 18.04
0 0 12 743.09 16.95
0 0 12 755.19 15.76
0 0 13 -1.29 0.73
0 0 13 0.67 0.76
0 0 -13 0.17 1.36
0 0 14 65.59 3.91
0 0 14 65.46 4.42
0 0 -14 70.03 5.35
0 0 -14 65.15 4.85
0 0 15 -0.35 0.36
0 0 15 -1.09 0.60
0 0 -15 -0.26 0.64
0 -1 0 0.77 0.20
0 1 0 0.15 0.14
0 1 0 0.28 0.23
0 1 0 0.18 0.14
0 1 0 1.04 0.44
0 -1 1 2.47 0.27
0 -1 -1 3.14 0.54
0 1 -1 2.68 0.57
0 1 -1 2.46 0.39
0 1 1 2.82 0.48
0 1 -1 2.72 0.52
0 -1 1 2.38 0.42
0 1 1 3.15 0.51
0 1 -1 2.60 0.29
0 -1 -1 2.45 0.28
0 1 1 3.12 0.32
0 -1 1 3.42 0.32
0 -1 2 100.34 2.02
0 1 -2 113.34 2.60
0 1 2 111.10 3.53
0 1 -2 79.52 3.70
0 1 -2 85.80 2.03
0 1 -2 103.44 3.74
0 -1 -2 105.41 2.90
0 -1 2 96.66 2.96
0 1 -2 103.19 2.53
0 -1 -2 99.02 2.44
0 -1 2 96.83 2.36
0 1 2 94.27 2.41
0 -1 3 47.80 1.69
0 1 3 49.50 2.20
0 1 -3 41.94 2.13
0 1 -3 43.59 1.19
0 1 -3 49.75 2.25
0 -1 -3 48.99 2.20
0 -1 3 46.60 2.00
0 1 3 48.33 2.09
0 1 3 53.10 1.73
0 -1 -3 53.97 2.28
0 -1 3 47.65 2.40
0 -1 4 704.23 7.49
0 -1 -4 673.85 9.96
0 1 4 710.89 9.51
0 1 -4 754.47 10.17
0 -1 -4 759.61 9.94
0 -1 4 762.74 9.47
0 1 4 755.58 9.66
0 -1 4 679.66 9.84
0 -1 -4 781.87 9.54
0 1 4 796.87 8.39
0 1 -5 11.07 1.61
0 -1 5 15.72 1.30
0 -1 -5 16.60 1.80
0 1 -5 19.44 1.95
0 -1 -5 18.95 1.88
0 -1 5 11.65 1.36
0 1 5 12.79 1.44
0 -1 -5 19.51 1.70
0 1 5 19.42 1.59
0 -1 5 16.78 1.78
0 -1 6 473.18 7.93
0 -1 -6 454.89 10.19
0 1 -6 408.30 10.85
0 -1 -6 485.19 10.48
0 1 -6 479.75 10.73
0 1 6 456.32 9.43
0 -1 6 462.50 9.26
0 1 6 548.98 9.55
0 -1 6 473.08 10.12
0 -1 -6 499.93 9.32
0 -1 -7 6.37 1.22
0 -1 7 6.76 1.42
0 1 7 8.46 1.39
0 1 -7 4.67 1.40
0 -1 -7 4.93 1.40
0 -1 7 3.30 0.91
0 1 7 2.73 0.92
0 -1 -7 5.65 1.30
0 1 -7 4.15 1.31
0 -1 7 4.76 0.93
0 -1 8 2605.97 27.97
0 -1 -8 2593.81 24.86
0 1 8 2469.49 26.75
0 -1 8 2566.93 26.56
0 -1 -8 2484.36 28.43
0 -1 9 7.98 1.70
0 1 -9 8.07 2.75
0 -1 -9 10.89 2.00
0 -1 9 7.17 1.54
0 1 9 7.89 1.70
0 1 -10 145.71 7.79
0 -1 -10 157.47 7.90
0 -1 10 197.25 8.59
0 1 10 195.61 8.39
0 -1 10 171.03 7.04
0 1 10 172.66 7.76
0 1 10 165.83 7.99
0 -1 10 181.87 8.12
0 1 10 163.14 7.02
0 1 10 162.66 8.13
0 -1 10 163.19 8.04
0 -1 10 165.34 7.98
0 1 -10 105.87 8.83
0 1 -10 155.69 7.76
0 -1 -10 163.67 8.50
0 1 -10 197.25 10.86
0 -1 -11 4.76 1.89
0 1 -11 4.35 1.85
0 1 11 6.34 1.72
0 -1 11 5.51 1.30
0 -1 11 4.59 1.41
0 1 11 4.82 1.43
0 1 11 5.46 1.36
0 1 11 3.37 1.17
0 -1 11 2.56 1.30
0 1 -11 2.44 1.95
0 -1 11 6.49 1.60
0 -1 -11 5.35 1.74
0 1 -11 3.36 1.37
0 1 -11 4.46 2.20
0 -1 -12 18.82 3.02
0 1 -12 19.89 3.13
0 -1 12 24.47 2.70
0 1 12 21.34 2.78
0 -1 12 21.59 2.85
0 1 12 23.91 3.11
0 1 -12 18.76 2.98
0 -1 -12 22.02 3.48
0 1 -12 20.73 3.82
0 1 12 28.30 2.95
0 -1 -13 6.78 1.91
0 1 -13 6.95 2.06
0 1 13 10.29 1.94
0 -1 13 8.83 1.83
0 1 13 7.46 1.58
0 -1 13 9.07 1.55
0 1 -13 8.57 2.08
0 1 -13 7.62 2.09
0 -1 -13 16.21 3.16
0 1 13 10.24 1.68
0 1 14 136.75 6.30
0 -1 14 128.41 6.09
0 1 14 130.28 5.77
0 1 -14 115.73 6.69
0 -1 -14 128.51 7.11
0 -1 -14 115.26 6.15
0 1 -14 114.76 6.26
0 -1 15 3.33 0.92
0 1 15 3.08 0.79
0 1 15 3.52 0.91
0 -1 -15 2.33 0.93
0 1 -15 3.05 0.97
0 1 -15 2.74 1.02
0 -1 -15 3.04 1.04
0 2 0 4694.66 25.03
0 -2 0 4782.62 18.64
0 2 0 4714.89 26.13
0 2 0 4524.75 32.22
0 2 0 4594.88 22.70
0 2 1 87.42 3.47
0 -2 -1 82.63 1.77
0 -2 1 84.30 2.96
0 2 -1 90.39 3.79
0 2 1 89.44 3.88
0 2 -1 86.99 4.45
0 2 1 96.58 4.96
0 2 1 88.73 3.36
0 2 -1 84.53 3.36
0 2 -1 96.99 3.42
0 -2 1 75.21 1.17
0 2 1 86.05 1.33
0 -2 -1 100.67 3.96
0 -2 1 102.72 2.27
0 -2 2 40.12 2.29
0 2 -2 40.25 2.79
0 2 -2 44.93 2.45
0 2 -2 35.82 2.90
0 2 2 41.90 2.61
0 2 -2 35.92 2.03
0 2 2 43.82 2.90
0 2 2 34.59 1.49
0 -2 2 33.03 1.38
0 -2 -2 41.38 2.38
0 -2 2 41.61 1.28
0 -2 3 20.28 0.99
0 2 -3 17.32 2.24
0 2 -3 19.19 1.36
0 -2 -3 22.12 1.75
0 -2 3 21.36 1.86
0 2 -3 24.30 2.55
0 2 -3 23.47 1.61
0 -2 -3 22.14 1.52
0 -2 3 24.48 1.50
0 2 3 25.35 1.58
0 -2 4 187.21 3.54
0 2 -4 171.24 3.46
0 -2 -4 195.66 5.26
0 2 -4 193.36 8.07
0 -2 4 182.13 5.91
0 2 -4 207.70 5.77
0 -2 -4 201.32 5.48
0 -2 4 189.18 4.80
0 2 4 187.21 5.06
0 2 -5 71.54 3.01
0 -2 5 69.48 2.51
0 2 -5 57.89 4.88
0 -2 5 72.20 4.10
0 2 -5 65.54 5.25
0 -2 -5 70.40 3.30
0 -2 -5 80.44 3.91
0 2 -5 76.55 4.02
0 -2 5 84.32 3.65
0 2 5 83.82 3.84
0 -2 -6 658.35 10.75
0 2 -6 616.27 17.98
0 -2 6 660.29 13.13
0 2 -6 514.41 16.07
0 2 6 808.63 13.34
0 -2 6 836.48 12.94
0 -2 -6 632.53 13.03
0 -2 6 701.93 9.08
0 -2 -7 10.30 1.48
0 2 -7 8.95 2.57
0 -2 7 8.33 1.68
0 -2 7 14.55 1.92
0 2 7 15.36 2.07
0 -2 -7 10.13 1.79
0 2 -8 0.29 1.54
0 -2 8 0.31 0.63
0 -2 -8 0.23 0.46
0 -2 -8 0.63 0.58
0 -2 8 2.04 0.90
0 2 8 0.27 0.67
0 2 9 3.70 1.29
0 -2 -9 3.10 1.14
0 2 9 2.13 0.85
0 2 -9 3.29 1.84
0 -2 9 1.26 0.82
0 -2 -9 2.41 0.85
0 -2 -9 1.16 1.22
0 2 9 2.47 1.07
0 -2 9 2.20 1.03
0 -2 -10 8.42 2.08
0 2 -10 9.77 2.25
0 -2 10 7.70 1.80
0 2 10 7.84 1.94
0 2 10 9.72 2.10
0 2 10 9.62 1.97
0 -2 -10 5.65 1.64
0 -2 10 7.50 1.89
0 2 -10 -0.29 1.32
0 2 -10 16.68 2.56
0 -2 -10 6.05 1.80
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0 2 -11 4.55 1.75
0 -2 -11 3.63 1.41
0 2 11 4.40 1.47
0 -2 11 5.17 1.39
0 2 11 5.31 1.59
0 2 -11 4.71 1.52
0 2 -11 4.59 1.76
0 2 11 5.02 1.37
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0 2 -12 413.08 13.40
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0 2 12 427.14 12.52
0 2 12 446.79 13.35
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0 2 -12 439.93 15.73
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0 -2 -13 1.77 1.03
0 2 -13 2.49 1.27
0 2 13 2.61 1.05
0 -2 13 3.79 1.16
0 2 13 3.90 1.21
0 2 -13 1.34 1.02
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0 2 13 5.29 1.31
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0 2 14 0.35 0.46
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0 2 15 0.25 0.23
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0 -2 -15 2.01 0.70
0 2 -15 1.59 0.63
0 -2 -15 0.56 0.73
0 -3 0 0.44 0.73
0 -3 0 0.19 0.27
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0 3 0 0.67 0.53
0 3 0 0.23 0.64
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0 -3 -1 4.64 0.54
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0 -3 1 4.88 0.92
0 3 -1 6.15 1.23
0 3 1 5.56 1.17
0 3 -1 6.26 1.20
0 3 -1 7.68 1.78
0 3 1 5.90 1.25
0 -3 -1 6.81 1.36
0 -3 2 612.33 10.47
0 3 -2 648.04 13.81
0 3 2 664.11 12.55
0 3 -2 602.91 14.48
0 3 -2 673.12 11.44
0 3 -2 585.17 10.99
0 -3 -2 651.99 11.48
0 -3 3 28.42 2.51
0 3 -3 31.23 3.37
0 3 -3 30.71 3.40
0 3 -3 26.52 2.21
0 3 3 30.39 2.98
0 -3 -3 28.57 2.36
0 -3 4 109.59 5.31
0 3 -4 104.77 6.59
0 -3 -4 114.18 4.59
0 3 4 123.22 6.69
0 3 -4 101.45 6.22
0 3 4 134.37 4.69
0 -3 5 23.93 2.65
0 -3 -5 23.28 2.09
0 3 -5 21.67 3.38
0 -3 5 30.04 2.41
0 3 5 28.28 2.49
0 3 5 30.75 3.76
0 -3 6 12.61 2.12
0 3 -6 13.90 2.96
0 3 6 15.20 2.96
0 3 6 15.44 2.07
0 -3 6 17.42 2.08
0 -3 -6 12.16 2.07
0 3 -7 30.28 4.82
0 -3 7 37.39 3.78
0 -3 -7 35.53 2.82
0 3 7 41.41 5.23
0 -3 -7 32.54 3.57
0 3 -8 1446.86 34.58
0 -3 -8 1777.23 20.78
0 -3 8 1924.56 28.56
0 3 8 2046.35 39.27
0 3 8 1975.69 25.08
0 3 8 2117.00 28.08
0 -3 -8 1699.57 26.78
0 -3 -9 40.50 4.31
0 3 9 59.41 7.10
0 3 9 49.12 4.11
0 -3 9 50.46 4.85
0 3 -9 32.25 5.37
0 3 9 53.48 4.67
0 3 -9 54.92 5.54
0 3 10 328.94 10.81
0 3 10 332.12 11.80
0 3 -10 334.20 13.19
0 3 11 0.81 0.94
0 -3 11 0.32 0.57
0 3 -11 1.18 1.16
0 3 11 -0.32 1.02
0 3 12 0.53 0.74
0 -3 12 3.37 1.10
0 -3 -12 -1.05 1.23
0 3 -12 -0.76 1.42
0 3 -12 1.92 1.15
0 3 12 0.72 0.83
0 -3 -13 1.85 0.82
0 3 13 2.99 1.06
0 -3 13 2.32 0.88
0 3 13 3.97 1.25
0 3 14 22.36 2.03
0 -3 14 23.05 2.20
0 -3 -14 22.50 2.67
0 4 0 6111.15 43.56
0 -4 0 6005.56 49.64
0 4 -1 104.19 6.51
0 -4 1 103.69 4.50
0 4 1 108.55 6.20
0 4 -1 109.75 5.70
0 4 -1 103.39 7.21
0 4 1 108.19 5.95
0 -4 1 107.72 7.26
0 -4 -1 107.43 6.05
0 -4 2 405.53 9.99
0 4 -2 377.73 12.86
0 4 -2 372.51 13.39
0 4 -2 426.21 11.11
0 4 2 409.94 11.86
0 -4 -2 394.76 10.68
0 -4 3 0.30 0.51
0 -4 -3 1.53 0.69
0 4 -3 0.34 0.58
0 4 -3 0.11 0.51
0 4 3 -0.34 0.62
0 -4 4 209.51 8.35
0 -4 -4 194.68 6.82
0 4 -4 203.58 10.85
0 -4 -5 5.11 1.14
0 -4 5 5.48 1.51
0 4 -5 6.41 1.99
0 4 5 5.58 1.96
0 -4 -5 4.76 1.46
0 -4 6 156.05 8.12
0 4 -6 128.72 10.00
0 4 6 167.74 10.45
0 -4 -6 138.66 7.83
0 -4 -7 22.73 3.24
0 4 7 30.59 4.70
0 4 7 26.40 3.01
0 4 -7 20.66 4.17
0 4 -7 26.81 3.65
0 -4 7 27.28 3.63
0 4 7 26.52 3.34
0 4 -7 30.87 4.40
0 -4 -8 54.16 5.30
0 4 -8 42.37 6.47
0 4 -8 64.19 5.48
0 -4 8 63.00 5.62
0 4 8 57.66 5.09
0 4 -8 60.83 6.34
0 4 8 61.85 7.12
0 4 8 60.37 4.65
0 4 9 23.84 3.31
0 4 -9 16.79 2.77
0 4 9 19.46 2.67
0 4 -9 18.50 3.60
0 4 10 27.18 3.17
0 4 -10 19.77 3.68
0 4 10 27.97 3.61
0 4 11 75.34 5.05
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-12 1 0 164.70 7.66
12 1 0 153.27 6.42
-12 1 0 144.90 7.22
-12 -1 0 138.86 6.89
12 1 1 0.57 0.60
12 -1 1 0.43 0.60
12 1 1 -1.37 0.77
-12 1 -1 -0.68 0.97
-12 -1 -1 -2.35 1.05
-12 1 -1 1.81 0.87
-12 -1 -1 0.04 0.55
12 1 2 317.85 9.82
12 -1 2 315.58 9.01
-12 1 -2 318.14 10.50
-12 -1 -2 314.21 10.16
-12 -1 -2 340.58 10.01
12 1 3 0.43 0.72
12 -1 3 0.72 0.46
12 1 3 0.65 0.52
-12 1 -3 0.21 0.51
-12 -1 -3 1.22 0.82
-12 -1 -3 0.72 0.59
12 1 4 14.09 2.05
12 -1 4 12.84 1.80
12 1 4 13.88 1.75
-12 1 -4 11.70 2.01
-12 -1 -4 13.23 2.05
-12 -1 -4 14.13 1.94
12 1 5 7.81 1.46
12 -1 5 9.36 1.50
12 1 5 10.59 1.41
-12 1 -5 9.26 1.70
-12 -1 -5 8.03 1.50
-12 -1 -5 7.42 1.34
12 1 6 44.35 3.21
12 -1 6 42.77 2.98
12 1 6 50.39 2.86
-12 1 -6 38.84 3.20
-12 -1 -6 35.06 2.98
-12 -1 -6 43.82 2.90
-12 -1 -7 -0.02 0.12
12 1 7 0.37 0.47
12 -1 7 0.23 0.37
12 1 7 0.31 0.42
-12 1 -7 0.13 0.48
-12 -1 -7 -0.31 0.46
-12 -2 8 7.58 1.04
-12 -2 8 6.60 1.14
-12 2 8 10.41 1.71
12 2 -8 8.26 1.37
-12 2 8 12.50 1.54
-12 -2 8 12.46 1.50
12 -2 -8 12.22 1.63
12 2 -8 13.56 1.66
-12 -2 7 2.78 0.83
-12 2 7 1.24 0.73
-12 -2 7 1.33 0.49
12 2 -7 1.92 0.78
12 -2 -7 1.70 0.72
12 2 -7 2.17 0.86
-12 2 7 1.81 0.69
-12 -2 7 2.70 0.84
-12 2 6 182.74 6.95
-12 -2 6 172.63 6.58
12 -2 -6 186.87 7.03
12 2 -6 185.51 6.83
-12 -2 6 161.85 6.41
-12 -2 6 146.97 5.16
-12 2 6 173.87 8.07
12 2 -6 173.32 6.59
12 2 -6 161.44 6.84
-12 2 5 0.11 0.47
-12 -2 5 0.20 0.56
12 2 -5 0.63 0.91
12 2 -5 0.38 0.63
-12 2 5 0.40 0.58
-12 -2 5 0.15 0.42
-12 -2 5 -0.18 0.28
-12 2 4 39.97 3.59
-12 -2 4 39.80 3.46
-12 2 4 41.90 3.70
-12 -2 4 35.27 3.23
12 2 -4 38.81 3.30
12 2 -4 46.65 4.58
12 2 -3 0.63 0.66
-12 2 3 -1.72 0.91
-12 -2 3 -1.97 0.98
-12 2 3 0.90 0.66
-12 -2 3 -0.06 0.55
-12 -2 2 247.76 8.64
12 2 -2 254.76 8.44
-12 2 2 256.20 9.34
-12 -2 2 239.01 8.72
12 2 -1 1.25 0.71
-12 2 1 0.85 0.70
-12 -2 1 1.53 0.79
-12 -2 1 1.13 0.72
12 2 0 567.77 12.26
-12 2 0 612.54 14.55
-12 -2 0 606.55 13.84
12 2 1 -0.69 0.87
12 2 1 -0.42 0.63
-12 2 -1 -1.25 0.84
-12 -2 -1 -0.24 0.75
-12 -2 -1 -0.12 0.66
12 2 2 183.15 7.54
12 2 2 196.43 6.95
-12 2 -2 201.69 8.17
-12 -2 -2 193.13 7.59
-12 -2 -2 179.41 6.93
12 2 3 8.51 1.64
12 2 3 7.86 1.40
-12 2 -3 10.40 1.85
-12 -2 -3 9.93 1.72
-12 -2 -3 7.65 1.44
12 2 4 191.69 7.28
12 2 4 200.08 6.56
-12 2 -4 197.74 7.63
-12 -2 -4 182.08 7.00
-12 -2 -4 184.29 6.54
-12 2 -5 1.69 0.73
-12 -2 -5 1.42 0.65
12 2 5 2.01 0.90
12 -2 5 1.38 0.61
12 2 5 2.18 0.75
12 2 5 1.77 1.05
-12 -2 -5 2.36 0.81
-12 2 -6 55.86 3.58
-12 -2 -6 54.81 3.37
-12 -2 -6 50.37 3.01
12 2 6 55.56 3.51
12 -2 6 57.17 3.04
12 2 6 61.50 3.17
12 2 6 48.00 3.70
12 3 -7 14.46 1.72
-12 3 7 13.14 1.92
-12 -3 7 11.61 1.31
-12 -3 7 12.15 1.41
-12 3 6 128.20 6.49
-12 -3 6 124.19 4.96
12 3 -6 136.19 5.46
12 3 -6 125.01 5.59
-12 3 5 58.62 4.69
-12 -3 5 55.37 3.54
-12 -3 5 49.82 2.96
12 3 -5 61.13 3.84
12 3 -5 62.64 4.59
-12 -3 4 177.86 6.33
-12 3 4 162.15 8.12
12 3 -4 165.34 6.47
12 3 -4 169.09 8.21
-12 -3 4 157.23 5.33
-12 -3 4 155.86 6.15
-12 -3 3 25.74 2.50
12 3 -3 22.94 2.50
12 3 -3 28.09 3.65
-12 -3 3 24.27 2.53
-12 -3 3 21.23 2.00
-12 -3 2 51.85 3.65
-12 -3 2 43.47 3.39
12 3 -2 49.38 3.64
12 3 -2 56.86 4.57
12 3 -2 55.20 5.33
-12 -3 1 7.92 1.52
12 3 -1 11.35 2.32
12 3 -1 11.03 2.66
12 3 -1 7.48 1.46
-12 -3 1 10.79 1.72
-12 -3 0 323.93 9.06
12 3 0 419.35 14.72
12 3 0 418.91 13.81
12 3 0 334.77 9.21
-12 -3 0 411.94 10.34
-12 -3 -1 2.04 0.83
12 3 1 3.86 1.69
12 3 1 3.25 1.68
12 3 1 2.79 0.94
-12 -3 -1 1.81 0.75
12 3 2 252.14 10.72
12 3 2 233.89 10.29
12 3 2 216.79 7.10
-12 -3 -2 245.37 7.67
-12 -3 -2 209.82 7.03
-12 -3 -3 29.85 2.57
-12 -3 -3 24.97 2.37
-12 3 -3 24.59 2.89
12 3 3 28.98 2.54
12 3 3 31.68 3.75
12 3 3 25.36 3.15
12 3 3 27.58 2.74
-12 -3 -4 34.85 2.65
-12 3 -4 27.91 2.99
12 3 4 39.58 2.81
12 3 4 33.58 3.58
12 3 4 27.52 2.81
12 3 4 35.15 2.95
-12 -3 -5 8.38 1.27
12 3 5 8.19 1.38
12 3 5 7.99 1.22
-12 3 -5 5.20 1.24
12 3 5 7.44 1.61
12 4 -5 8.02 1.29
-12 -4 5 6.28 0.94
-12 -4 5 7.32 0.99
-12 4 5 7.76 1.45
12 4 -5 6.49 1.34
12 4 -4 11.57 1.61
-12 -4 4 10.15 1.33
-12 -4 4 10.91 1.26
12 4 -4 9.92 1.83
-12 4 4 13.00 1.89
12 4 -3 5.72 1.19
-12 -4 3 5.92 0.97
-12 -4 3 7.20 1.23
-12 4 3 6.24 1.41
12 4 -3 6.43 1.67
-12 4 2 176.15 7.05
12 4 -2 175.27 6.25
12 4 -2 184.87 6.75
12 4 -2 186.93 8.64
-12 -4 2 163.30 5.76
-12 4 1 100.30 5.58
12 4 -1 103.74 4.86
12 4 -1 109.24 5.75
12 4 -1 102.23 6.52
-12 -4 1 96.26 4.45
-12 4 0 282.09 9.53
12 4 0 286.93 7.98
12 4 0 313.22 10.26
12 4 0 308.83 11.21
-12 -4 0 259.21 7.27
-12 4 -1 36.07 3.50
12 4 1 42.72 3.03
12 4 1 43.78 3.97
12 4 1 39.91 3.92
-12 -4 -1 38.37 2.80
12 4 2 32.21 3.35
12 4 2 25.52 2.90
-12 -4 -2 24.75 2.21
-12 4 -2 23.84 2.82
12 4 2 29.31 2.44
12 4 3 17.66 2.11
12 4 3 26.02 2.93
-12 4 -3 22.63 2.63
12 4 3 25.34 2.17
-12 -4 -3 23.37 2.05
-13 0 8 0.11 0.22
-13 0 8 -1.17 0.52
-13 0 7 140.38 5.52
-13 0 7 152.31 5.50
13 0 -7 156.45 5.62
-13 0 7 154.09 5.69
13 0 -6 0.14 0.64
-13 0 6 0.14 0.55
-13 0 6 0.47 0.54
-13 0 5 109.79 5.39
-13 0 5 103.11 5.23
-13 0 4 -0.51 0.61
-13 0 4 0.37 0.65
-13 0 3 15.93 2.24
-13 0 3 18.23 2.32
-13 0 2 0.01 0.59
-13 0 2 1.36 0.76
-13 0 1 46.58 3.80
-13 0 1 48.09 3.80
-13 0 0 0.43 0.63
-13 0 0 -1.23 0.68
13 0 1 5.88 1.24
-13 0 -1 5.40 1.44
-13 0 -1 5.28 1.25
13 0 2 -0.16 0.48
-13 0 -2 0.29 0.57
-13 0 -2 0.69 0.49
-13 0 -3 33.98 2.73
13 0 3 31.75 2.69
-13 0 -3 33.59 3.08
13 0 4 0.00 0.45
-13 0 -4 -0.50 0.52
13 0 5 381.70 8.40
-13 0 -5 386.88 9.14
-13 -1 7 50.62 3.13
-13 1 7 50.85 3.47
13 1 -7 54.48 2.98
-13 1 7 54.59 3.22
-13 -1 7 54.54 3.16
13 -1 -7 58.83 3.39
13 1 -7 58.37 3.31
-13 1 6 -0.14 0.43
13 1 -6 0.63 0.50
13 -1 -6 0.36 0.63
13 1 -6 -0.30 0.63
-13 1 6 -0.16 0.43
-13 -1 6 0.42 0.51
-13 1 6 -1.20 0.64
-13 -1 6 -0.02 0.39
-13 1 5 49.52 3.53
-13 -1 5 49.74 3.48
-13 -1 5 43.34 3.29
-13 1 5 51.70 3.65
13 1 -5 44.76 3.05
13 1 -5 52.73 3.81
13 1 -4 0.01 0.42
-13 1 4 -1.07 0.68
-13 -1 4 0.08 0.48
-13 1 4 0.33 0.42
-13 -1 4 0.02 0.61
13 1 -3 452.69 10.13
-13 1 3 440.82 11.41
-13 -1 3 442.13 11.18
-13 1 3 446.70 11.26
-13 -1 3 421.81 10.72
13 1 -2 -0.87 0.60
-13 -1 2 -1.27 0.74
-13 1 2 -2.56 1.02
-13 -1 2 -1.40 0.86
13 1 -1 12.30 1.71
-13 1 1 10.79 1.78
-13 -1 1 10.01 1.75
-13 1 1 13.44 1.91
-13 -1 1 11.14 1.81
13 1 0 6.07 1.21
-13 1 0 4.18 1.13
-13 -1 0 4.93 1.18
-13 1 0 2.84 0.96
-13 -1 0 3.48 1.13
-13 1 -1 114.84 5.84
-13 -1 -1 120.44 5.80
-13 -1 -1 128.48 5.75
13 -1 1 115.00 4.89
13 1 1 113.78 5.36
-13 -1 -2 0.58 0.58
13 1 2 0.05 0.46
-13 1 -2 -0.52 0.58
-13 -1 -2 0.23 0.53
13 1 2 0.36 0.55
13 -1 2 -0.35 0.46
13 1 3 437.14 8.58
-13 1 -3 397.72 10.25
-13 -1 -3 389.33 9.83
-13 -1 -3 396.07 9.34
13 1 3 360.25 9.18
13 -1 3 354.57 8.40
13 1 4 5.03 1.10
13 -1 4 6.21 1.11
-13 -1 -4 5.02 1.01
-13 1 -4 4.96 1.17
-13 -1 -4 5.15 1.14
13 1 5 -0.68 0.40
13 1 5 1.91 0.69
13 -1 5 1.31 0.61
-13 1 -5 0.64 0.43
-13 -1 -5 2.10 0.74
-13 -1 -5 0.11 0.22
-13 2 6 2.36 0.86
13 -2 -6 3.28 0.86
13 2 -6 3.42 0.87
-13 2 6 3.39 0.87
-13 -2 6 3.42 0.82
13 2 -6 3.30 0.85
-13 -2 6 2.86 0.81
-13 2 5 232.13 7.01
-13 -2 5 224.99 6.70
13 -2 -5 249.30 7.23
13 2 -5 254.21 7.06
-13 -2 5 208.37 6.66
-13 2 5 207.84 8.02
13 2 -5 209.88 6.42
13 2 -5 205.89 7.23
13 2 -4 0.41 0.85
13 2 -4 0.07 0.49
-13 2 4 0.15 0.37
-13 -2 4 -1.09 0.60
-13 -2 4 0.58 0.56
-13 2 3 40.95 3.26
-13 -2 3 37.46 3.02
13 2 -3 42.10 3.07
13 2 -3 46.34 4.18
-13 -2 3 38.60 3.09
-13 -2 2 7.59 1.51
-13 2 2 5.67 1.33
-13 -2 2 6.00 1.31
13 2 -2 7.84 1.37
-13 -2 1 139.53 5.89
13 2 -1 154.89 5.85
-13 2 1 155.67 6.53
-13 -2 1 152.68 6.22
13 2 0 5.56 1.13
-13 2 0 2.59 1.01
-13 -2 0 4.63 1.21
-13 -2 0 4.04 1.03
-13 -2 -1 146.21 5.80
13 2 1 157.87 5.71
-13 2 -1 159.53 6.56
-13 -2 -1 157.55 6.20
13 2 2 0.11 0.41
-13 2 -2 0.67 0.53
-13 -2 -2 -0.29 0.52
-13 -2 -2 0.97 0.65
-13 2 -3 103.50 4.91
-13 -2 -3 95.53 4.51
-13 -2 -3 84.09 4.09
13 2 3 86.14 4.38
13 2 3 97.51 4.08
13 2 3 105.20 5.79
-13 2 -4 1.87 0.81
-13 -2 -4 2.47 0.73
-13 -2 -4 1.55 0.59
13 2 4 1.93 0.70
13 2 4 2.46 0.69
13 2 4 3.41 1.15
13 2 4 2.21 0.82
-13 -3 5 127.93 4.48
-13 3 5 141.65 5.86
13 3 -5 141.89 4.92
13 3 -5 133.52 5.23
-13 3 4 0.72 0.42
13 3 -4 1.04 0.80
13 3 -4 0.99 0.59
-13 -3 4 -0.13 0.38
-13 -3 3 190.67 6.13
13 3 -3 201.89 6.31
13 3 -3 211.05 8.12
-13 3 3 199.99 7.66
-13 -3 2 12.79 1.66
-13 3 2 13.70 2.02
13 3 -2 13.55 1.71
13 3 -2 14.26 2.36
13 3 -2 12.03 1.68
13 3 -1 7.65 1.88
13 3 -1 4.59 1.17
13 3 -1 6.21 1.19
-13 -3 1 4.17 1.00
-13 -3 0 10.67 1.49
13 3 0 10.79 1.51
13 3 0 15.06 2.18
13 3 0 10.75 2.06
-13 -3 -1 107.43 4.55
13 3 1 113.79 6.21
13 3 1 118.94 6.05
13 3 1 113.34 4.58
-13 -3 -2 45.12 2.87
13 3 2 44.33 3.61
13 3 2 50.20 3.89
13 3 2 47.23 2.85
-13 -3 -3 189.78 5.61
13 3 3 210.27 5.66
13 3 3 208.92 7.48
13 3 3 177.93 6.31
14 0 -5 -0.24 0.56
-14 0 5 0.06 0.28
-14 0 4 36.39 2.68
-14 0 4 32.28 2.53
-14 0 3 -0.31 0.43
-14 0 3 1.29 0.60
-14 0 2 2.75 0.80
-14 0 2 2.67 0.85
-14 0 1 -1.16 0.68
-14 0 1 0.16 0.37
-14 0 0 196.77 6.63
-14 0 0 196.75 6.21
-14 0 -1 -0.37 0.58
-14 0 -1 -0.43 0.34
-14 0 -2 56.91 3.42
-14 0 -2 -0.41 0.30
-14 0 -3 -0.74 0.47
-14 1 4 192.45 5.99
-14 -1 4 188.94 5.85
14 1 -4 196.65 6.45
-14 -1 4 182.57 5.84
-14 1 4 190.66 5.72
-14 1 3 -0.04 0.53
-14 -1 3 -0.69 0.53
-14 1 3 1.08 0.52
-14 -1 3 1.19 0.56
-14 1 2 172.18 6.10
-14 -1 2 172.42 5.97
-14 -1 2 156.86 5.65
-14 1 2 158.85 5.30
-14 1 1 1.79 0.74
-14 -1 1 2.09 0.70
-14 -1 0 33.60 2.59
-14 1 0 33.33 2.71
-14 -1 0 33.34 2.66
-14 -1 -1 23.72 2.11
-14 1 -1 27.66 2.43
-14 -1 -1 26.28 2.32
-14 -1 -2 219.58 6.03
-14 1 -2 221.95 6.59
-14 -1 -2 219.28 6.42
-14 2 3 1.94 0.74
14 2 -3 1.35 0.73
14 2 -3 2.27 0.62
14 -2 -3 1.98 0.62
14 2 -3 1.62 0.56
-14 2 3 1.21 0.49
-14 -2 3 1.82 0.57
-14 -2 3 1.70 0.60
-14 2 2 28.88 2.24
-14 -2 2 26.81 2.09
-14 -2 2 19.76 1.88
14 2 -2 24.18 1.89
14 2 -2 22.10 1.94
14 2 -2 25.87 2.66
-14 -2 1 3.96 0.88
14 2 -1 4.02 1.22
14 2 -1 3.68 0.76
-14 2 1 3.21 0.79
-14 -2 1 3.30 0.78
14 2 -1 4.28 0.99
-14 2 0 240.51 6.50
-14 -2 0 228.30 6.13
-14 -2 0 216.23 6.12
14 2 0 239.95 5.78
14 2 0 244.38 8.13
14 2 0 240.47 7.41
0 0 0 0.00 0.00
TITL exp_1764_OB-2-46b in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 12.221375 7.023007 13.053698 90.0000 94.5113 90.0000
ZERR 4.00 0.000226 0.000145 0.000254 0.0000 0.0017 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC H N O Cu
UNIT 92.00 20.00 16.00 4.00
REM CrysAlisPro recorded range (K): Min=89.5; max=219.4; aver:154.4
TEMP -119
SIZE 0.12 0.22 0.45
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 20653
_shelx_res_file
;
TITL exp_1764_ob-2-46b_a.res in P2(1)/n
exp_1764_ob-2-46b.res
created by SHELXL-2018/3 at 14:48:59 on 22-Feb-2024
REM Old TITL exp_1764_OB-2-46b in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.306, Rweak 0.011, Alpha 0.027
REM 0.493 for 183 systematic absences, Orientation as input
REM Formula found by SHELXT: N8 O3 Cu
CELL 1.54184 12.2214 7.023 13.0537 90 94.511 90
ZERR 4 0.0002 0.0001 0.0003 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cl Cu N O
UNIT 4 76 8 4 28 4
L.S. 5
PLAN 10
SIZE 0.118 0.217 0.453
TEMP -119
CONF
RTAB dis Cu1 N11
RTAB dis Cu1 N12
RTAB dis Cu1 N13
RTAB dis Cu1 N14
RTAB dis Cu1 N15
RTAB ang N15 Cu1 N11
RTAB ang N15 Cu1 N12
RTAB ang N15 Cu1 N13
RTAB ang N15 Cu1 N14
HTAB
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM
REM
REM
WGHT 0.051500 1.097700
FVAR 0.37912
CU1 4 0.586038 0.733733 0.215775 11.00000 0.00948 0.00316 =
0.00894 0.00008 0.00069 0.00087
N12 5 0.486867 0.964317 0.192438 11.00000 0.01483 0.00803 =
0.01377 0.00034 0.00235 0.00088
AFIX 137
H12A 2 0.517997 1.048085 0.150183 11.00000 -1.20000
H12B 2 0.477733 1.021555 0.253724 11.00000 -1.20000
H12C 2 0.420444 0.926610 0.162954 11.00000 -1.20000
AFIX 0
N15 5 0.464063 0.504542 0.184109 11.00000 0.01497 0.00662 =
0.01672 -0.00113 0.00289 -0.00039
AFIX 137
H15A 2 0.492053 0.415157 0.142989 11.00000 -1.20000
H15B 2 0.401766 0.554421 0.151974 11.00000 -1.20000
H15C 2 0.448160 0.449703 0.244330 11.00000 -1.20000
AFIX 0
N11 5 0.580817 0.748724 0.371295 11.00000 0.01517 0.01223 =
0.01272 0.00091 0.00199 0.00284
AFIX 137
H11A 2 0.543429 0.855049 0.387772 11.00000 -1.20000
H11B 2 0.650406 0.754010 0.401582 11.00000 -1.20000
H11C 2 0.546287 0.643803 0.393945 11.00000 -1.20000
AFIX 0
N13 5 0.615746 0.750149 0.063660 11.00000 0.01544 0.01228 =
0.01383 -0.00023 0.00361 0.00164
AFIX 137
H13A 2 0.550830 0.753527 0.024449 11.00000 -1.20000
H13B 2 0.654939 0.646477 0.046280 11.00000 -1.20000
H13C 2 0.654659 0.857730 0.052718 11.00000 -1.20000
AFIX 0
N14 5 0.715785 0.553072 0.238151 11.00000 0.01886 0.01142 =
0.02005 -0.00084 -0.00091 0.00499
AFIX 137
H14A 2 0.703349 0.447470 0.198543 11.00000 -1.20000
H14B 2 0.724294 0.518588 0.305504 11.00000 -1.20000
H14C 2 0.777763 0.612328 0.220417 11.00000 -1.20000
AFIX 0
CL31 3 0.854232 0.740195 0.457887 11.00000 0.01258 0.00754 =
0.01258 0.00015 -0.00004 -0.00014
CL41 3 0.918792 0.746441 0.105316 11.00000 0.02181 0.00751 =
0.01103 0.00017 -0.00104 0.00044
O23 6 0.250995 0.756272 0.237699 11.00000 0.02309 0.00781 =
0.01024 -0.00055 -0.00260 0.00211
N24 5 0.317707 0.918979 0.379165 11.00000 0.02349 0.00311 =
0.01218 0.00023 -0.00248 0.00204
N21 5 0.306058 0.593040 0.382610 11.00000 0.02685 0.00361 =
0.01107 -0.00096 -0.00195 -0.00213
C22 1 0.289470 0.755962 0.329625 11.00000 0.00860 0.00565 =
0.01299 -0.00081 0.00356 0.00169
H21A 2 0.290271 0.494579 0.354580 11.00000 0.01077
H24A 2 0.301802 1.018097 0.350457 11.00000 0.01562
H21B 2 0.333126 0.601189 0.446125 11.00000 0.02020
H24B 2 0.345569 0.911700 0.442521 11.00000 0.02572
HKLF 4
REM exp_1764_ob-2-46b_a.res in P2(1)/n
REM wR2 = 0.0920, GooF = S = 1.078, Restrained GooF = 1.078 for all data
REM R1 = 0.0332 for 1835 Fo > 4sig(Fo) and 0.0350 for all 1977 data
REM 130 parameters refined using 0 restraints
END
WGHT 0.0515 1.0977
REM Instructions for potential hydrogen bonds
EQIV $1 -x+3/2, y+1/2, -z+1/2
HTAB N12 Cl31_$1
HTAB N12 Cl41_$1
EQIV $2 x-1/2, -y+3/2, z-1/2
HTAB N12 Cl31_$2
HTAB N12 O23
EQIV $3 -x+3/2, y-1/2, -z+1/2
HTAB N15 Cl31_$3
HTAB N15 Cl31_$2
HTAB N15 O23
HTAB N15 Cl41_$3
HTAB N11 Cl41_$1
HTAB N11 Cl31
HTAB N11 Cl41_$3
HTAB N13 Cl31_$2
HTAB N13 Cl31_$3
HTAB N13 Cl31_$1
HTAB N14 Cl31_$3
HTAB N14 Cl31
HTAB N14 Cl41_$3
HTAB N14 Cl41
EQIV $4 -x+1/2, y-1/2, -z+1/2
HTAB N21 O23_$4
EQIV $5 -x+1/2, y+1/2, -z+1/2
HTAB N24 O23_$5
EQIV $6 x-1/2, -y+3/2, z+1/2
HTAB N21 Cl41_$6
HTAB N24 Cl41_$6
REM Highest difference peak 0.674, deepest hole -0.799, 1-sigma level 0.104
Q1 1 0.5893 0.8564 0.2151 11.00000 0.05 0.67
Q2 1 0.5301 0.7402 0.1370 11.00000 0.05 0.60
Q3 1 0.6615 0.7421 0.1448 11.00000 0.05 0.57
Q4 1 0.6401 0.7205 0.2889 11.00000 0.05 0.50
Q5 1 0.5801 0.5999 0.2129 11.00000 0.05 0.48
Q6 1 0.5156 0.7353 0.2693 11.00000 0.05 0.43
Q7 1 0.7972 0.7366 0.3833 11.00000 0.05 0.39
Q8 1 0.7488 0.6010 0.2813 11.00000 0.05 0.39
Q9 1 0.8437 0.7410 0.1552 11.00000 0.05 0.38
Q10 1 0.8559 0.8609 0.4575 11.00000 0.05 0.36
;
_shelx_res_checksum 46771
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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
Cu Cu1 0.58604(3) 0.73373(4) 0.21577(2) 0.00720(15) Uani d 1 . .
N N12 0.48687(15) 0.9643(3) 0.19244(13) 0.0121(4) Uani d 1 . .
H H12A 0.517997 1.048085 0.150183 0.015 Uiso calc 1 . .
H H12B 0.477733 1.021555 0.253724 0.015 Uiso calc 1 . .
H H12C 0.420444 0.926610 0.162954 0.015 Uiso calc 1 . .
N N15 0.46406(15) 0.5045(3) 0.18411(14) 0.0127(4) Uani d 1 . .
H H15A 0.492053 0.415157 0.142989 0.015 Uiso calc 1 . .
H H15B 0.401766 0.554421 0.151974 0.015 Uiso calc 1 . .
H H15C 0.448160 0.449703 0.244330 0.015 Uiso calc 1 . .
N N11 0.58082(18) 0.7487(3) 0.37130(16) 0.0133(5) Uani d 1 . .
H H11A 0.543429 0.855049 0.387772 0.016 Uiso calc 1 . .
H H11B 0.650406 0.754010 0.401582 0.016 Uiso calc 1 . .
H H11C 0.546287 0.643803 0.393945 0.016 Uiso calc 1 . .
N N13 0.61575(18) 0.7501(2) 0.06366(15) 0.0137(5) Uani d 1 . .
H H13A 0.550830 0.753527 0.024449 0.016 Uiso calc 1 . .
H H13B 0.654939 0.646477 0.046280 0.016 Uiso calc 1 . .
H H13C 0.654659 0.857730 0.052718 0.016 Uiso calc 1 . .
N N14 0.71579(15) 0.5531(3) 0.23815(14) 0.0169(4) Uani d 1 . .
H H14A 0.703349 0.447470 0.198543 0.020 Uiso calc 1 . .
H H14B 0.724294 0.518588 0.305504 0.020 Uiso calc 1 . .
H H14C 0.777763 0.612328 0.220417 0.020 Uiso calc 1 . .
Cl Cl31 0.85423(5) 0.74020(7) 0.45789(4) 0.01096(18) Uani d 1 . .
Cl Cl41 0.91879(5) 0.74644(7) 0.10532(4) 0.01357(18) Uani d 1 . .
O O23 0.25100(15) 0.7563(2) 0.23770(13) 0.0139(4) Uani d 1 . .
N N24 0.31771(16) 0.9190(3) 0.37916(15) 0.0131(4) Uani d 1 . .
N N21 0.30606(17) 0.5930(3) 0.38261(15) 0.0140(4) Uani d 1 . .
C C22 0.2895(2) 0.7560(3) 0.32963(19) 0.0089(5) Uani d 1 . .
H H21A 0.290(2) 0.495(4) 0.355(2) 0.011(7) Uiso d 1 . .
H H24A 0.302(2) 1.018(5) 0.350(2) 0.016(7) Uiso d 1 . .
H H21B 0.333(2) 0.601(4) 0.446(2) 0.020(7) Uiso d 1 . .
H H24B 0.346(2) 0.912(5) 0.443(2) 0.026(8) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cu1 0.0095(2) 0.0032(2) 0.0089(2) 0.00087(11) 0.00069(14) 0.00008(10)
N12 0.0148(9) 0.0080(10) 0.0138(8) 0.0009(8) 0.0024(7) 0.0003(7)
N15 0.0150(9) 0.0066(10) 0.0167(9) -0.0004(7) 0.0029(7) -0.0011(7)
N11 0.0152(11) 0.0122(12) 0.0127(10) 0.0028(7) 0.0020(8) 0.0009(6)
N13 0.0154(11) 0.0123(12) 0.0138(10) 0.0016(7) 0.0036(8) -0.0002(7)
N14 0.0189(9) 0.0114(11) 0.0201(9) 0.0050(8) -0.0009(7) -0.0008(8)
Cl31 0.0126(3) 0.0075(3) 0.0126(3) -0.00014(17) 0.0000(2) 0.00015(17)
Cl41 0.0218(3) 0.0075(3) 0.0110(3) 0.00044(18) -0.0010(2) 0.00017(17)
O23 0.0231(10) 0.0078(10) 0.0102(8) 0.0021(6) -0.0026(7) -0.0006(5)
N24 0.0235(10) 0.0031(10) 0.0122(9) 0.0020(8) -0.0025(7) 0.0002(8)
N21 0.0269(11) 0.0036(10) 0.0111(9) -0.0021(8) -0.0020(7) -0.0010(8)
C22 0.0086(11) 0.0057(13) 0.0130(11) 0.0017(7) 0.0036(9) -0.0008(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 4 1 0.2285
0 -4 -2 0.1954
-5 0 -6 0.1032
5 0 6 0.1169
-1 4 -1 0.2376
1 -4 1 0.2227
6 0 -6 0.0507
5 0 6 0.1091
-6 0 6 0.0590
-6 3 3 0.1420
-5 -2 6 0.0889
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
N11 Cu1 N15 . . 98.65(7) yes
N12 Cu1 N15 . . 99.60(8) yes
N13 Cu1 N15 . . 91.61(7) yes
N14 Cu1 N15 . . 94.55(8) yes
N12 Cu1 N11 . . 92.47(7) ?
N12 Cu1 N13 . . 87.65(7) ?
N12 Cu1 N14 . . 165.49(8) ?
N11 Cu1 N13 . . 169.57(8) ?
N14 Cu1 N11 . . 88.53(8) ?
N14 Cu1 N13 . . 88.78(8) ?
Cu1 N12 H12A . . 109.5 ?
Cu1 N12 H12B . . 109.5 ?
Cu1 N12 H12C . . 109.5 ?
H12A N12 H12B . . 109.5 ?
H12A N12 H12C . . 109.5 ?
H12B N12 H12C . . 109.5 ?
Cu1 N15 H15A . . 109.5 ?
Cu1 N15 H15B . . 109.5 ?
Cu1 N15 H15C . . 109.5 ?
H15A N15 H15B . . 109.5 ?
H15A N15 H15C . . 109.5 ?
H15B N15 H15C . . 109.5 ?
Cu1 N11 H11A . . 109.5 ?
Cu1 N11 H11B . . 109.5 ?
Cu1 N11 H11C . . 109.5 ?
H11A N11 H11B . . 109.5 ?
H11A N11 H11C . . 109.5 ?
H11B N11 H11C . . 109.5 ?
Cu1 N13 H13A . . 109.5 ?
Cu1 N13 H13B . . 109.5 ?
Cu1 N13 H13C . . 109.5 ?
H13A N13 H13B . . 109.5 ?
H13A N13 H13C . . 109.5 ?
H13B N13 H13C . . 109.5 ?
Cu1 N14 H14A . . 109.5 ?
Cu1 N14 H14B . . 109.5 ?
Cu1 N14 H14C . . 109.5 ?
H14A N14 H14B . . 109.5 ?
H14A N14 H14C . . 109.5 ?
H14B N14 H14C . . 109.5 ?
C22 N24 H24A . . 118(2) ?
C22 N24 H24B . . 118(2) ?
H24A N24 H24B . . 124(3) ?
C22 N21 H21A . . 118.7(19) ?
C22 N21 H21B . . 118(2) ?
H21A N21 H21B . . 124(3) ?
O23 C22 N24 . . 121.39(19) ?
O23 C22 N21 . . 121.60(19) ?
N21 C22 N24 . . 117.0(2) ?
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 N11 . 2.039(2) yes
Cu1 N12 . 2.0313(19) yes
Cu1 N13 . 2.050(2) yes
Cu1 N14 . 2.0339(19) yes
Cu1 N15 . 2.2107(19) yes
N12 H12A . 0.9100 ?
N12 H12B . 0.9100 ?
N12 H12C . 0.9100 ?
N15 H15A . 0.9100 ?
N15 H15B . 0.9100 ?
N15 H15C . 0.9100 ?
N11 H11A . 0.9100 ?
N11 H11B . 0.9100 ?
N11 H11C . 0.9100 ?
N13 H13A . 0.9100 ?
N13 H13B . 0.9100 ?
N13 H13C . 0.9100 ?
N14 H14A . 0.9100 ?
N14 H14B . 0.9100 ?
N14 H14C . 0.9100 ?
O23 C22 . 1.254(3) ?
N24 C22 . 1.346(3) ?
N24 H24A . 0.81(3) ?
N24 H24B . 0.87(3) ?
N21 C22 . 1.344(3) ?
N21 H21A . 0.80(3) ?
N21 H21B . 0.87(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
N11 H11A Cl41 2_655 0.91 2.79 3.509(2) 137 yes
N11 H11B Cl31 1_555 0.91 2.54 3.443(2) 170 yes
N11 H11C Cl41 2_645 0.91 2.82 3.541(2) 137 yes
N12 H12A Cl31 2_655 0.91 2.57 3.461(2) 167 yes
N12 H12B Cl41 2_655 0.91 2.67 3.4273(19) 142 yes
N13 H13A Cl31 4_575 0.91 2.49 3.381(2) 166 yes
N13 H13C Cl31 2_655 0.91 2.69 3.4752(15) 145 yes
N14 H14A Cl31 2_645 0.91 2.56 3.430(2) 160 yes
N14 H14C Cl41 1_555 0.91 2.55 3.418(2) 159 yes
N15 H15A Cl31 2_645 0.91 2.68 3.530(2) 157 yes
N21 H21A O23 2_545 0.79(3) 2.11(3) 2.893(3) 172(3) yes
N21 H21B Cl41 4_576 0.87(3) 2.50(3) 3.315(2) 158(2) yes
N24 H24A O23 2_555 0.81(3) 2.10(3) 2.906(3) 173(3) yes
N24 H24B Cl41 4_576 0.88(3) 2.50(3) 3.319(2) 157(3) yes