#------------------------------------------------------------------------------
#$Date: 2024-08-24 05:20:25 +0300 (Sat, 24 Aug 2024) $
#$Revision: 294214 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312593.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_2312593
loop_
_publ_author_name
'Guimaraes, Samuel P.'
'Dos Santos, Leonardo H. R.'
'Rodrigues, Bernardo L.'
_publ_section_title
;
Coordination structure and intermolecular interactions in copper(II)
acetate complexes with 1,10-phenanthroline and 2,2'-bipyridine.
;
_journal_coeditor_code ZO3050
_journal_issue 9
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624007617
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac
'[Cu (C2 H3 O2) (C10 H8 N2)2] (C2 H3 O2), C2 H4 O2, 3H2 O1'
_chemical_formula_moiety
'C22 H19 Cu N4 O2 +, C2 H3 O2 -, C2 H4 O2, 3H2 O1'
_chemical_formula_sum 'C26 H32 Cu N4 O9'
_chemical_formula_weight 608.09
_chemical_name_systematic
;
(Acetato-\kO)bis(2,2'-bipyridine-\k^2^N,N')copper(II)
acetate--acetic acid--water (1/1/3)
;
_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 mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 86.5370(10)
_cell_angle_beta 69.8200(10)
_cell_angle_gamma 83.2610(10)
_cell_formula_units_Z 2
_cell_length_a 11.0826(18)
_cell_length_b 11.1840(19)
_cell_length_c 12.1880(18)
_cell_measurement_reflns_used 25526
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 30.9850
_cell_measurement_theta_min 2.5220
_cell_volume 1407.8(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR92 (Altomare et al., 1994)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0290
_diffrn_reflns_av_unetI/netI 0.0244
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 36611
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.688
_diffrn_reflns_theta_min 2.529
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.834
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.99486
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour Blue
_exptl_crystal_density_diffrn 1.435
_exptl_crystal_description Prism
_exptl_crystal_F_000 634
_exptl_crystal_size_max 0.128
_exptl_crystal_size_mid 0.074
_exptl_crystal_size_min 0.061
_refine_diff_density_max 0.419
_refine_diff_density_min -0.371
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 364
_refine_ls_number_reflns 7452
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0363
_refine_ls_R_factor_gt 0.0296
_refine_ls_shift/su_max 0.078
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.4639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0790
_refine_ls_wR_factor_ref 0.0815
_reflns_number_gt 6436
_reflns_number_total 7452
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zo3050sup1.cif
_cod_data_source_block III
_cod_database_code 2312593
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
-14 -4 -11 11.1676 2.30356 12
-14 -3 -7 6.59981 2.09958 7
-14 -3 -6-0.28848 1.72584 7
-14 -3 -5 1.74670 1.72477 7
-14 -2 -9 2.21824 1.75422 7
-14 -2 -8 44.8621 3.71440 7
-14 -2 -7 34.1721 3.15079 7
-14 -2 -6 5.04280 1.92356 7
-14 -2 -5-0.28378 1.68096 7
-14 -2 -4 0.57602 1.80554 7
-14 -2 0 23.5307 2.76702 3
-14 -1 -11 23.6435 2.82671 7
-14 -1 -10 23.1083 2.78927 7
-14 -1 -9 0.53216 1.72660 7
-14 -1 -8 22.1123 2.66668 7
-14 -1 -7 7.25293 2.11577 7
-14 -1 -6 97.0612 5.15233 7
-14 -1 -5 10.7658 2.22806 7
-14 -1 -4 8.99951 2.11459 7
-14 -1 -1 7.71242 1.99387 3
-14 -1 0 7.86126 2.10863 3
-14 -1 1 8.84411 2.14207 3
-14 0 -12 0.25130 1.83527 7
-14 0 -11 11.5753 2.20241 7
-14 0 -10 35.8968 3.14131 7
-14 0 -9 1.78038 1.66445 7
-14 0 -8 10.2374 2.20608 7
-14 0 -7 1.03578 1.68039 7
-14 0 -6 86.3547 4.72453 7
-14 0 -5 16.6352 2.56375 7
-14 0 -4 1.09857 1.81171 7
-14 0 -3 9.00140 2.14112 7
-14 0 -1 14.0648 2.29385 3
-14 0 0 3.76386 1.60266 3
-14 1 -11 12.3155 2.13205 7
-14 1 -10 26.0726 2.75114 7
-14 1 -9 7.50699 1.99307 7
-14 1 -8 18.5825 2.54316 7
-14 1 -7 11.4469 2.23703 7
-14 1 -6 26.7098 2.80312 7
-14 1 -5 23.4422 2.77235 7
-14 1 -4 28.3852 2.99416 7
-14 1 -3 17.3302 2.38562 7
-14 2 -9 36.3364 3.05613 7
-14 2 -8 23.2540 2.55831 7
-14 2 -7 9.76690 2.08268 7
-14 2 -6 33.0380 3.04062 7
-14 2 -5 6.30338 1.90496 7
-14 2 -4 5.72604 2.00148 7
-14 2 -3 44.5991 3.55922 7
-14 3 -7-0.68000 1.74035 7
-14 3 -6 12.2412 2.33048 5
-14 3 -6 11.4940 2.14715 7
-14 3 -5 7.78254 2.00201 7
-14 3 -4 39.8863 3.30109 7
-14 3 -3 12.3121 2.31419 7
-14 4 -5 30.5011 3.04738 5
-14 4 -5 25.9017 2.84557 7
-14 4 -4 10.7354 2.14426 7
-14 4 -3 10.9324 2.22372 7
-13 -6 -10 1.17412 1.72141 12
-13 -6 -7 89.8419 5.05793 7
-13 -6 -6 0.29477 1.69290 7
-13 -6 -5 3.23333 1.72482 7
-13 -6 -4 47.4116 3.71012 7
-13 -5 -12 1.37449 1.89917 12
-13 -5 -11-0.55129 1.80352 12
-13 -5 -9 18.7687 2.69388 7
-13 -5 -8 0.58033 1.75287 7
-13 -5 -7 31.9426 3.07535 7
-13 -5 -6 10.0203 2.11366 7
-13 -5 -5 26.6213 2.98287 7
-13 -5 -4 13.5247 2.35215 7
-13 -5 -3 0.57993 1.62951 7
-13 -5 -2 56.9762 4.03967 7
-13 -4 -13 0.25394 1.74129 12
-13 -4 -12 3.59435 1.91292 12
-13 -4 -11 1.55467 1.81632 12
-13 -4 -10 57.7134 3.97866 7
-13 -4 -9 68.9502 4.36872 7
-13 -4 -8-1.12251 1.57716 7
-13 -4 -7 14.4622 2.38146 7
-13 -4 -6 0.27779 1.50812 7
-13 -4 -5 6.68815 2.05269 7
-13 -4 -4 16.5552 2.43040 7
-13 -4 -3 24.1303 2.78309 7
-13 -4 -2 28.5399 2.99071 7
-13 -4 -1 6.15450 1.84118 7
-13 -4 1 0.29340 1.80616 3
-13 -3 -12 5.00220 1.85308 12
-13 -3 -11 1.11064 1.74070 7
-13 -3 -11 0.72675 1.53224 12
-13 -3 -10 15.6463 2.46356 7
-13 -3 -9 9.24386 2.10761 7
-13 -3 -8 8.64394 2.05610 7
-13 -3 -7 26.3291 2.83131 7
-13 -3 -6 0.26933 1.51351 7
-13 -3 -5 18.4335 2.55443 7
-13 -3 -4 40.5358 3.37200 7
-13 -3 -3 6.39548 1.98052 7
-13 -3 -2 40.4375 3.37674 7
-13 -3 -1-1.15528 1.99528 7
-13 -3 1 0.83650 1.66820 3
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-13 -2 -12 41.8846 3.47220 7
-13 -2 -11 9.01578 2.16093 7
-13 -2 -10 10.7696 2.15510 7
-13 -2 -9 4.95768 1.96966 7
-13 -2 -8 0.77898 1.50711 7
-13 -2 -7 15.5519 2.31806 7
-13 -2 -6 22.9529 2.63325 7
-13 -2 -5 51.6246 3.65917 7
-13 -2 -4 9.08554 2.10748 7
-13 -2 -3 1.90439 1.62799 7
-13 -2 -2 38.3236 3.30169 7
-13 -2 -1 0.85275 1.74990 7
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-13 -2 0 22.8358 2.63158 3
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-13 -2 2 16.6015 2.55954 3
-13 -1 -13 25.1949 2.86737 7
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-13 -1 -11-1.26074 1.66339 7
-13 -1 -10 1.00337 1.50079 7
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-13 -1 -8 21.1767 2.46020 7
-13 -1 -7 7.25049 1.79511 7
-13 -1 -6 34.5745 3.01419 7
-13 -1 -5 119.240 5.48952 7
-13 -1 -4 21.6221 2.56149 7
-13 -1 -3 0.53204 1.65273 7
-13 -1 -2 16.6146 2.33843 7
-13 -1 -1 1.39832 1.64018 7
-13 -1 0 17.8535 2.65759 7
-13 -1 0 19.9652 2.53611 3
-13 -1 1 0.24733 1.53660 3
-13 -1 2 10.2325 2.30682 3
-13 -1 3 22.9716 2.72830 3
-13 0 -13 3.85713 1.76217 7
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-13 0 -11-0.47647 1.58410 7
-13 0 -10 10.6973 2.12723 7
-13 0 -9 6.42530 1.97752 7
-13 0 -8 0.71507 1.57230 7
-13 0 -7 11.7801 2.11527 7
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-13 0 -4 7.87448 1.97938 7
-13 0 -3 1.30165 1.60277 7
-13 0 -2 6.95161 1.83840 7
-13 0 -1-0.27539 1.61487 7
-13 0 0 23.0600 2.73609 7
-13 0 0 23.2309 2.47456 3
-13 0 1 1.61273 1.63797 3
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-13 0 3 0.73823 1.56999 3
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-13 1 -11 1.11700 1.68445 7
-13 1 -10 24.4783 2.58976 7
-13 1 -9 13.3154 2.07017 7
-13 1 -9 13.2695 2.34373 5
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-13 1 -7 1.15282 1.48376 7
-13 1 -6-1.17541 1.42028 7
-13 1 -5 16.6045 2.23217 7
-13 1 -4 1.48360 1.49398 7
-13 1 -3 5.59941 1.77448 7
-13 1 -2 8.13166 1.97188 7
-13 1 -1 20.6325 2.63477 7
-13 1 -1 15.1919 2.09882 3
-13 1 0 21.1076 2.28913 3
-13 1 1 3.39207 1.54970 3
-13 2 -10 9.01809 1.83434 7
-13 2 -9-0.63743 1.43505 7
-13 2 -9 2.13654 1.78983 5
-13 2 -8 8.19895 1.78496 7
-13 2 -8 5.25648 1.73478 5
-13 2 -7 10.1298 1.90298 7
-13 2 -7 12.5430 2.16387 5
-13 2 -6 1.12996 1.41671 7
-13 2 -6-1.05885 1.59908 5
-13 2 -5 3.72411 1.71217 7
-13 2 -5 3.02117 1.25827 4
-13 2 -4 13.9266 2.21116 7
-13 2 -3-0.24844 1.57131 7
-13 2 -2 15.4339 2.32057 7
-13 2 -1 2.67480 1.77928 7
-13 3 -9 4.95333 1.56885 7
-13 3 -8 8.11438 1.77500 7
-13 3 -8 10.3925 2.05888 5
-13 3 -7 16.3069 2.15856 7
-13 3 -7 14.1541 2.18102 5
-13 3 -6 4.10715 1.64137 7
-13 3 -6 4.02028 1.48897 4
-13 3 -6 2.95370 1.51066 5
-13 3 -5 1.12067 1.57099 7
-13 3 -5-0.50704 1.54620 5
-13 3 -5 1.62852 1.22218 4
-13 3 -4 2.09667 1.58550 7
-13 3 -4-0.34250 1.22577 4
-13 3 -3 28.1011 2.77040 7
-13 3 -2 15.3751 2.37045 7
-13 4 -7 4.92135 1.58631 7
-13 4 -7 6.89213 1.69082 4
-13 4 -7 6.92124 1.87517 5
-13 4 -6-0.20561 1.46161 7
-13 4 -6-0.27369 1.45014 5
-13 4 -6-1.48296 1.60716 4
-13 4 -5 1.50513 1.41838 7
-13 4 -5 1.00916 1.33140 4
-13 4 -5-0.51633 1.57453 5
-13 4 -4 19.3601 2.44034 7
-13 4 -4 19.0856 2.35031 5
-13 4 -4 22.1998 2.24109 4
-13 4 -3 7.06443 1.87680 7
-13 4 -3 7.38768 1.72466 5
-13 4 -2 4.43555 1.78984 7
-13 5 -8 0.75685 1.58161 4
-13 5 -7-0.24188 1.48902 4
-13 5 -6 9.02744 1.90829 4
-13 5 -6 9.22700 2.11563 5
-13 5 -5 3.89266 1.57442 7
-13 5 -5 3.95524 1.90135 5
-13 5 -5 2.66745 1.47954 4
-13 5 -4 18.1809 2.24885 7
-13 5 -4 21.7141 2.60229 5
-13 5 -4 28.8615 2.65023 4
-13 5 -3 11.6333 2.04742 7
-13 5 -3 14.6184 2.08556 5
-13 5 -2 4.56314 1.75621 7
-13 6 -7 0.26050 1.57364 4
-13 6 -6-0.50171 1.55850 4
-13 6 -5 7.01583 2.12498 5
-13 6 -5 7.02187 1.90776 4
-13 6 -4 0.23405 1.48056 4
-13 6 -4 3.03408 1.73394 5
-13 6 -2 9.08553 2.09129 7
-12 -8 -6 16.9180 1.94905 8
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-12 -8 -4 7.80086 1.98701 7
-12 -8 -3 34.0121 3.29858 7
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-12 -7 -10 9.48059 2.21376 12
-12 -7 -9 54.3973 4.07009 12
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-12 -7 -8 46.4137 3.76166 7
-12 -7 -7 2.60334 1.67960 7
-12 -7 -6 90.2481 4.13243 8
-12 -7 -5 19.7101 2.01807 8
-12 -7 -4-0.63356 1.22335 8
-12 -7 -3 67.0747 4.32045 7
-12 -7 -3 78.4077 3.47758 8
-12 -7 -2 0.28311 1.62593 7
-12 -7 -1 19.4144 2.63665 7
-12 -7 0 9.80604 2.08725 7
-12 -6 -12 1.13091 1.69155 12
-12 -6 -11 24.4750 2.84897 12
-12 -6 -10 12.6003 2.32219 12
-12 -6 -10 11.4771 2.28505 7
-12 -6 -9 0.57666 1.65594 7
-12 -6 -8 23.8119 2.82841 7
-12 -6 -7 9.23642 2.03861 7
-12 -6 -6 34.8246 3.14653 7
-12 -6 -5 9.60648 2.01089 7
-12 -6 -5 7.30553 1.60181 8
-12 -6 -4 7.48495 1.48821 8
-12 -6 -3 34.5804 2.47371 8
-12 -6 -2 4.20571 1.33965 8
-12 -6 -1 28.0890 2.90124 7
-12 -6 -1 26.2359 2.20632 8
-12 -6 0 7.97486 2.05841 7
-12 -6 1-0.91213 1.65066 3
-12 -6 1 0.28961 1.66327 7
-12 -5 -14 0.79328 1.87967 12
-12 -5 -13-0.79187 1.69853 12
-12 -5 -12-0.79361 1.75901 12
-12 -5 -11 20.3139 2.55536 12
-12 -5 -11 16.7574 2.50646 7
-12 -5 -10 22.6822 2.71130 12
-12 -5 -10 20.0785 2.66050 7
-12 -5 -9 20.8245 2.69333 7
-12 -5 -8 87.2226 4.81933 7
-12 -5 -7 0.27012 1.41317 7
-12 -5 -6 65.0201 3.33939 2
-12 -5 -6 62.5670 3.99678 7
-12 -5 -5 34.6541 3.06179 7
-12 -5 -5 30.1933 2.54371 8
-12 -5 -5 38.0703 2.62675 2
-12 -5 -4 0.18082 1.28584 8
-12 -5 -4 3.25210 1.39585 2
-12 -5 -4 3.20593 1.59868 7
-12 -5 -3 56.4892 3.16256 8
-12 -5 -3 58.8661 3.88686 7
-12 -5 -2 0.17011 1.20078 8
-12 -5 -1 39.6636 2.72505 8
-12 -5 0 7.23708 1.57740 8
-12 -5 1 6.87230 1.90823 7
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-12 -5 2 16.1708 2.70879 3
-12 -4 -13 14.4099 2.34983 12
-12 -4 -12 2.54916 1.95683 7
-12 -4 -12 0.73808 1.64906 12
-12 -4 -11 6.36406 1.90314 7
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-12 -4 -9 22.6693 2.56642 7
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-12 -4 -6 27.9032 2.79250 7
-12 -4 -6 24.6788 2.10809 2
-12 -4 -5 0.15659 1.18071 2
-12 -4 -5 2.32617 1.66320 7
-12 -4 -4 20.2550 2.20479 8
-12 -4 -4 28.5925 2.86609 7
-12 -4 -4 29.4977 2.40013 2
-12 -4 -3 32.2531 2.46848 8
-12 -4 -3 31.7585 3.01457 7
-12 -4 -3 31.0495 2.53126 2
-12 -4 -2 3.84363 1.47221 8
-12 -4 -2 2.92951 1.68572 7
-12 -4 -1 39.9424 2.79973 8
-12 -4 -1 40.6339 3.37406 7
-12 -4 0 8.86503 1.74334 8
-12 -4 1 14.1219 2.26613 3
-12 -4 1 14.2709 1.98687 8
-12 -4 2 15.3956 2.43193 7
-12 -4 2 18.8771 2.60203 3
-12 -4 3 0.29629 1.85743 3
-12 -3 -13 17.6501 2.56995 7
-12 -3 -13 13.8946 2.30421 12
-12 -3 -12-1.35190 1.75456 7
-12 -3 -12-0.45411 1.47344 12
-12 -3 -11 8.72372 1.99053 7
-12 -3 -11 11.4267 2.01755 12
-12 -3 -10 80.1750 4.47704 7
-12 -3 -9 27.8719 2.79706 7
-12 -3 -8 35.9437 3.10223 7
-12 -3 -7 14.7532 2.19604 7
-12 -3 -6 21.2310 2.51604 7
-12 -3 -6 19.7744 1.73429 2
-12 -3 -5 25.8179 2.62451 7
-12 -3 -5 23.7572 1.95822 2
-12 -3 -4 16.9504 1.84614 2
-12 -3 -4 13.6446 2.07459 7
-12 -3 -3 96.1214 4.35325 8
-12 -3 -3 80.2351 4.56301 7
-12 -3 -3 90.4357 3.92309 2
-12 -3 -2 1.36759 1.41846 8
-12 -3 -2 3.61676 1.38496 2
-12 -3 -2 3.90911 1.74739 7
-12 -3 -1 74.0791 3.89732 8
-12 -3 -1 72.9184 4.32191 7
-12 -3 0 0.27262 1.54899 7
-12 -3 0-1.17736 1.58528 8
-12 -3 1 16.8115 2.44597 7
-12 -3 1 13.6629 2.26413 3
-12 -3 2 63.8376 4.09759 3
-12 -3 3 11.0070 2.26569 3
-12 -2 -13 26.9375 2.88002 7
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13 3 -2 7.48835 1.73522 6
13 3 -1 0.59525 1.39072 6
13 3 0 15.4859 2.54795 11
13 3 0 14.0487 1.93439 6
13 3 1 1.44756 1.76580 11
13 3 1 1.16160 1.32775 6
13 3 2 44.3606 2.98109 6
13 3 2 36.7852 3.28000 11
13 3 3 5.86130 1.60708 6
13 3 3 4.74883 1.80054 11
13 3 4 44.6133 3.49408 11
13 3 4 40.2487 2.88772 6
13 3 5 20.3801 2.48853 11
13 3 5 16.3816 2.08856 6
13 3 6 0.84759 1.37508 6
13 3 7 26.4066 2.52005 6
13 3 8 10.7910 1.66823 10
13 3 8 9.66984 1.85088 6
13 3 9 8.53845 1.60448 10
13 3 9 6.54031 1.82120 6
13 3 10 19.8431 2.22657 10
13 3 10 21.2187 2.54748 6
13 3 11 1.34326 1.51266 10
13 3 11 3.51040 1.85210 6
13 3 12 5.54902 1.85515 10
13 3 12 4.83221 1.89275 6
13 3 13 4.66005 1.80383 10
13 4 -3 2.07000 1.61254 6
13 4 -2 2.92718 1.54504 6
13 4 -1-0.66357 1.56137 6
13 4 0 27.8865 2.59370 6
13 4 1 6.88959 1.83542 6
13 4 2 32.2436 2.72092 6
13 4 3 25.0433 2.47556 6
13 4 4 12.6687 1.99472 6
13 4 5 5.58043 1.61228 6
13 4 6 0.68812 1.39892 6
13 4 7 10.4200 1.96451 6
13 4 8 0.24551 1.56634 6
13 4 9 62.5481 3.63159 10
13 4 9 73.9704 4.29748 6
13 4 10 63.2607 3.80942 10
13 4 10 58.1802 3.91051 6
13 4 11 0.23816 1.43872 10
13 4 11 0.56277 1.69982 6
13 4 12 3.82430 1.77569 10
13 4 13 0.27131 1.76054 10
13 5 -3 1.25788 1.67294 6
13 5 -2 15.2972 2.32102 6
13 5 -1 0.24259 1.62578 6
13 5 0 13.1530 2.16377 6
13 5 1 0.23636 1.50793 6
13 5 2 49.4080 3.44232 6
13 5 2 46.8873 3.77618 11
13 5 3 2.33409 1.69371 11
13 5 3 1.41500 1.47883 6
13 5 4 19.1161 2.66238 11
13 5 4 19.2577 2.46810 6
13 5 5 27.9594 2.70871 6
13 5 5 26.2197 3.05193 11
13 5 6 7.15112 1.88717 6
13 5 7 27.3717 2.85939 6
13 5 8 1.82691 1.65103 6
13 5 9 20.5509 2.67222 6
13 5 10 10.6825 2.19792 6
13 5 10 13.9114 1.76960 2
13 5 11 0.50810 1.59263 10
13 5 12 2.41912 1.77362 10
13 6 -2 18.7056 2.60754 6
13 6 -1-0.52621 1.69300 6
13 6 0 23.3558 2.66636 6
13 6 1 4.88439 1.82984 6
13 6 2 2.03862 1.72154 6
13 6 3 17.0841 2.42003 6
13 6 3 16.3469 2.51132 11
13 6 4 51.9713 3.96120 11
13 6 4 56.1192 3.73337 6
13 6 5 0.25896 1.62341 6
13 6 5 0.58757 1.85810 11
13 6 6-0.26352 1.56099 6
13 6 7 97.3267 5.05686 6
13 6 8 1.38381 1.73520 6
13 6 9 11.6190 1.87596 2
13 6 9 14.8065 2.45703 6
13 6 10 0.77532 1.30919 2
13 6 11 10.5606 1.83859 2
13 7 0 17.8661 2.68924 6
13 7 1 6.08066 1.98185 6
13 7 2 30.6890 3.07847 6
13 7 3 6.56922 2.05493 6
13 7 4 47.2294 3.64571 6
13 7 5 14.6601 2.36916 6
13 7 6 1.68187 1.78865 6
13 7 7 16.0057 2.49650 6
13 7 8 1.33692 1.50540 2
13 7 8 2.92239 1.78269 6
13 7 9 9.64550 1.90897 2
13 7 10-0.43368 1.40708 2
13 7 11 22.8416 2.44964 2
13 8 8-0.97612 1.58361 2
13 8 9 3.61269 1.76033 2
13 8 10 1.43267 1.64971 2
13 8 11 29.2079 2.87088 2
13 9 8 3.70332 1.97091 2
14 -4 1 6.14857 1.97984 11
14 -4 2 3.11488 1.69241 11
14 -4 3 10.9794 2.07296 11
14 -3 2-0.75680 1.69068 11
14 -3 3 10.8749 2.16222 11
14 -3 4 38.5323 3.21528 11
14 -2 2 2.36959 1.83269 11
14 -2 3 49.3766 3.59759 11
14 -2 4 6.35516 1.88486 11
14 -1 2-0.27292 1.66447 11
14 -1 3 12.3416 2.29381 11
14 -1 4 28.0869 2.85254 11
14 -1 5 15.4401 2.39054 11
14 -1 8 18.6889 1.94949 6
14 -1 9 8.93664 1.64065 6
14 -1 10 20.1370 2.28142 6
14 -1 11 10.6155 1.90614 6
14 -1 12 10.5311 2.14854 6
14 0 2 0.84509 1.76600 11
14 0 3 9.71295 2.16428 11
14 0 4-0.27396 1.74785 11
14 0 5 17.8893 1.78178 6
14 0 5 21.1468 2.69349 11
14 0 6 85.3683 3.77125 6
14 0 7 6.13829 1.64548 6
14 0 8 11.4607 1.81978 6
14 0 9 1.99872 1.37108 6
14 0 10 32.0628 2.81093 6
14 0 11 12.7329 2.19975 6
14 0 12 0.74234 1.73437 6
14 1 3 10.5643 2.28064 11
14 1 3 12.3181 1.72916 6
14 1 4 5.92637 1.89345 11
14 1 4 3.96151 1.36325 6
14 1 5 7.27281 2.14236 11
14 1 5 10.1909 1.59351 6
14 1 6 108.993 4.53085 6
14 1 7 4.54307 1.46470 6
14 1 8 22.2676 2.33518 6
14 1 9 0.64880 1.35582 6
14 1 10 19.5952 2.41171 6
14 1 11 22.5769 2.64573 6
14 1 12 1.30254 1.74604 6
14 2 1 18.8309 2.03631 6
14 2 2 0.69259 1.11422 6
14 2 3 13.0981 1.80384 6
14 2 4 2.03166 1.73635 11
14 2 4-0.36444 1.30426 6
14 2 5-0.28761 1.68656 11
14 2 5 0.37738 1.24465 6
14 2 6 7.68355 1.64075 6
14 2 7 36.0160 2.80437 6
14 2 8 43.1180 3.14514 6
14 2 9 3.23839 1.69048 6
14 2 10 18.1609 2.40774 6
14 2 10 18.9569 1.99406 10
14 2 11 16.8461 2.37151 6
14 3 0 4.13057 1.54783 6
14 3 1 36.1012 2.79186 6
14 3 2 4.13948 1.50658 6
14 3 3 0.79820 1.36840 6
14 3 4 7.74561 1.70574 6
14 3 5 2.09492 1.49999 6
14 3 6 0.43245 1.41473 6
14 3 7 8.54028 1.81288 6
14 3 7 7.88768 1.48376 10
14 3 8 30.2454 2.80968 6
14 3 8 28.9296 2.31058 10
14 3 9 23.1492 2.57674 6
14 3 9 19.5769 2.18680 10
14 3 10 23.3075 2.72601 6
14 3 10 25.3739 2.39123 10
14 3 11 8.72173 2.14801 6
14 3 11 7.96773 1.87310 10
14 3 12 3.02572 1.65549 10
14 3 13 18.2438 2.54623 10
14 4 -1 18.0267 2.53983 6
14 4 0 1.98234 1.74114 6
14 4 1 21.7206 2.41300 6
14 4 2 1.09739 1.41241 6
14 4 3 19.4495 2.43693 6
14 4 4 1.12128 1.60524 6
14 4 5 5.26792 1.70850 6
14 4 6 1.17566 1.51316 6
14 4 7 2.42124 1.54544 6
14 4 8 2.25734 1.58692 6
14 4 9 1.82688 1.77637 6
14 4 9 1.20497 1.31426 10
14 4 10 37.8989 3.42273 6
14 4 10 40.9914 3.06958 10
14 4 11 11.1182 2.05591 10
14 4 12 6.68676 1.93955 10
14 5 -1 10.0541 2.12414 6
14 5 0 1.94082 1.71288 6
14 5 1 13.9816 2.17348 6
14 5 2 2.64999 1.71322 6
14 5 3 20.0677 2.56013 6
14 5 4 8.77846 2.03976 6
14 5 5 5.70058 1.81351 6
14 5 6 2.78501 1.61618 6
14 5 7 1.55813 1.68536 6
14 5 8 2.13502 1.68841 6
14 5 9-1.10391 1.76083 6
14 5 10 22.4513 2.47848 10
14 5 11 0.99164 1.67446 10
14 6 1 13.8646 2.34531 6
14 6 2 0.52217 1.79030 6
14 6 3 24.3197 2.82018 6
14 6 4 2.36876 1.75064 6
14 6 5 7.98134 1.96191 6
14 6 6 2.70838 1.91250 6
14 6 7 8.57495 2.15545 6
15 1 9 21.6676 2.38137 6
15 1 10 1.14320 1.61406 6
15 1 11 6.06857 1.88953 6
15 2 6 7.90074 1.68640 6
15 2 7 28.6779 2.58460 6
15 2 8 15.8034 2.14300 6
15 2 9 40.8155 3.22720 6
15 2 10 1.95972 1.62926 6
15 3 4 3.28601 1.56873 6
15 3 5 17.3382 2.26612 6
15 3 6 0.43611 1.43836 6
15 3 7 5.66813 1.74429 6
15 3 8 0.23668 1.57371 6
15 3 9 29.7967 2.90381 6
15 4 3 0.89291 1.57580 6
15 4 4 19.5403 2.35474 6
15 4 5 24.8497 2.64808 6
15 4 6 5.24647 1.84470 6
15 4 7 31.8700 3.05475 6
15 4 8-1.26924 1.71463 6
15 5 2 2.43178 1.71718 6
15 5 3 10.2763 2.09993 6
15 5 4 44.8366 3.51510 6
15 5 5 38.0644 3.26792 6
15 5 6-0.25740 1.81692 6
0 0 0 0.00 0.00 0
TITL exp_209_auto in P1
REM P1 (#1 in standard setting)
CELL 0.71073 11.082665 11.184080 12.188051 86.5373 69.8205 83.2609
ZERR 2.00 0.000179 0.000191 0.000175 0.0013 0.0014 0.0014
LATT -1
SFAC C H N O Cu
UNIT 48.00 44.00 8.00 8.00 2.00
REM CrysAlisPro recorded range (K): Min=149.9; max=150.1; aver:150.0
TEMP -123
TREF
HKLF 4
END
;
_shelx_hkl_checksum 58195
_shelx_res_file
;
TITL SIR92 run in space group P -1
shelx.res
created by SHELXL-2018/3 at 13:32:10 on 17-Apr-2024
CELL 0.71073 11.0826 11.1840 12.1880 86.537 69.820 83.261
ZERR 2.00 0.0018 0.0019 0.0018 0.001 0.001 0.001
LATT 1
SFAC C H N O CU
UNIT 52 64 8 18 2
MERG 2
DFIX 0.850 0.020 H8A O8
DFIX 0.850 0.020 H8B O8
DFIX 0.850 0.020 H9A O9
DFIX 0.850 0.020 H9B O9
EQIV $1 x, y-1, z
HTAB C2 O6_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB C1 O9_$2
EQIV $3 -x, -y+1, -z+1
HTAB C14 O7_$2
HTAB O8 O9_$1
EQIV $4 x+1, y, z
HTAB O9 O3_$4
EQIV $5 -x+1, -y+1, -z+2
HTAB O9 O7_$5
HTAB O8 O6_$2
HTAB O7 O8
MPLA 12 C20 N3 C17 C19 N4 C15 C18 C13 C12 C11 C14 C16 CU01 O2
MPLA 4 O2 O1 C21 C22 CU01
MPLA 12 C2 C8 N1 N2 C1 C6 C4 C5 C7 C10 C9 C3 CU01 O2
MPLA N1 C1 C2 C3 C4 C5
MPLA N2 C6 C7 C8 C9 C10
MPLA N3 C11 C12 C13 C14 C15
MPLA N4 C16 C17 C18 C19 C20
RTAB Alfa Cu1 O1
RTAB Psi O1 O2
FMAP 2
PLAN 10
ACTA
BOND $H
CONF
L.S. 4
WGHT 0.043200 0.463900
FVAR 0.38990
CU01 5 0.272085 0.503900 0.209798 11.00000 0.01914 0.01857 =
0.01475 0.00140 -0.00622 -0.00464
C2 1 0.206860 0.192092 0.428570 11.00000 0.03037 0.02276 =
0.03901 0.00838 -0.00930 -0.00088
AFIX 43
H2 2 0.219242 0.109182 0.418838 11.00000 -1.20000
AFIX 0
C20 1 0.273797 0.677745 0.018455 11.00000 0.01917 0.02652 =
0.02131 0.00084 -0.00880 -0.00073
AFIX 43
H20 2 0.192645 0.654420 0.028961 11.00000 -1.20000
AFIX 0
O2 4 0.208648 0.407526 0.116142 11.00000 0.01982 0.02544 =
0.02053 -0.00468 -0.00721 -0.00334
O4 4 0.200813 0.993887 0.768591 11.00000 0.02839 0.04687 =
0.03342 -0.01733 -0.00976 0.00285
N3 3 0.467354 0.498743 0.208372 11.00000 0.01726 0.02194 =
0.01826 0.00107 -0.00659 -0.00142
O1 4 0.020702 0.519179 0.190818 11.00000 0.02192 0.03607 =
0.02592 -0.00716 -0.00710 0.00039
C17 1 0.513674 0.743964 -0.013680 11.00000 0.02058 0.02039 =
0.02256 -0.00017 -0.00373 -0.00309
AFIX 43
H17 2 0.595780 0.764818 -0.024124 11.00000 -1.20000
AFIX 0
C8 1 0.110456 0.760616 0.548408 11.00000 0.02513 0.04224 =
0.03517 -0.02197 -0.00567 -0.00376
AFIX 43
H8 2 0.081830 0.806154 0.615656 11.00000 -1.20000
AFIX 0
N1 3 0.218421 0.389843 0.344229 11.00000 0.01722 0.02027 =
0.01782 0.00072 -0.00473 -0.00276
N2 3 0.199276 0.625338 0.347389 11.00000 0.01741 0.02109 =
0.02090 -0.00318 -0.00475 -0.00415
C19 1 0.321373 0.765939 -0.064149 11.00000 0.02707 0.02518 =
0.02216 0.00361 -0.00956 0.00391
AFIX 43
H19 2 0.272712 0.802220 -0.108145 11.00000 -1.20000
AFIX 0
O3 4 0.017730 0.956568 0.748764 11.00000 0.03174 0.06400 =
0.05106 -0.03725 -0.00712 -0.00331
N4 3 0.341228 0.624361 0.084370 11.00000 0.01721 0.01970 =
0.01646 0.00023 -0.00572 -0.00162
C1 1 0.231915 0.269816 0.332762 11.00000 0.02210 0.02052 =
0.02738 0.00008 -0.00501 -0.00238
AFIX 43
H1 2 0.258859 0.238229 0.258286 11.00000 -1.20000
AFIX 0
C6 1 0.163986 0.570698 0.453673 11.00000 0.01435 0.02766 =
0.01956 -0.00373 -0.00620 -0.00322
C15 1 0.527389 0.590884 0.144514 11.00000 0.01599 0.01977 =
0.01473 -0.00346 -0.00356 0.00037
C18 1 0.442785 0.799615 -0.080534 11.00000 0.02806 0.02147 =
0.02228 0.00504 -0.00383 -0.00118
AFIX 43
H18 2 0.476656 0.858955 -0.135786 11.00000 -1.20000
AFIX 0
C13 1 0.702012 0.550111 0.218231 11.00000 0.01934 0.03606 =
0.02796 -0.00503 -0.01148 -0.00231
AFIX 43
H13 2 0.780400 0.567623 0.222134 11.00000 -1.20000
AFIX 0
C4 1 0.145237 0.363359 0.551933 11.00000 0.02711 0.04062 =
0.01864 0.00508 -0.00828 -0.00375
AFIX 43
H4 2 0.113584 0.396516 0.625898 11.00000 -1.20000
AFIX 0
C12 1 0.641921 0.454123 0.281888 11.00000 0.02509 0.03517 =
0.02984 0.00131 -0.01657 0.00148
AFIX 43
H12 2 0.679836 0.405328 0.328158 11.00000 -1.20000
AFIX 0
C5 1 0.175576 0.437064 0.452030 11.00000 0.01457 0.02761 =
0.01780 0.00117 -0.00626 -0.00277
C11 1 0.524178 0.431874 0.275553 11.00000 0.02281 0.02735 =
0.02521 0.00447 -0.01010 -0.00221
AFIX 43
H11 2 0.482997 0.368161 0.319549 11.00000 -1.20000
AFIX 0
C21 1 0.087276 0.431371 0.134940 11.00000 0.02150 0.02694 =
0.01579 0.00235 -0.00779 -0.00690
C14 1 0.644136 0.620223 0.148311 11.00000 0.02022 0.02541 =
0.02176 -0.00301 -0.00625 -0.00412
AFIX 43
H14 2 0.682800 0.685421 0.104979 11.00000 -1.20000
AFIX 0
C23 1 0.079638 1.012428 0.791199 11.00000 0.02969 0.02645 =
0.02013 -0.00413 -0.00684 0.00036
C7 1 0.119250 0.635756 0.556209 11.00000 0.02107 0.04149 =
0.02187 -0.00878 -0.00715 -0.00398
AFIX 43
H7 2 0.095642 0.596292 0.628728 11.00000 -1.20000
AFIX 0
C16 1 0.459669 0.656789 0.068856 11.00000 0.01673 0.01767 =
0.01564 -0.00285 -0.00437 -0.00068
C24 1 0.009193 1.112811 0.874465 11.00000 0.03919 0.03955 =
0.04612 -0.02309 -0.01251 0.00618
AFIX 137
H24A 2 0.019512 1.188813 0.833044 11.00000 -1.50000
H24B 2 0.044333 1.111701 0.936373 11.00000 -1.50000
H24C 2 -0.081002 1.101669 0.906858 11.00000 -1.50000
AFIX 0
C10 1 0.189655 0.746127 0.340646 11.00000 0.02465 0.02232 =
0.03186 -0.00353 -0.00372 -0.00619
AFIX 43
H10 2 0.213843 0.784045 0.267379 11.00000 -1.20000
AFIX 0
C9 1 0.144787 0.816035 0.439515 11.00000 0.03131 0.02589 =
0.04763 -0.01455 -0.00595 -0.00706
AFIX 43
H9 2 0.137909 0.899605 0.432432 11.00000 -1.20000
AFIX 0
C22 1 0.027867 0.344971 0.082796 11.00000 0.03099 0.04010 =
0.03721 -0.00647 -0.01692 -0.01118
AFIX 137
H22A 2 -0.063504 0.349434 0.124309 11.00000 -1.50000
H22B 2 0.066226 0.264444 0.088993 11.00000 -1.50000
H22C 2 0.043135 0.366143 0.001959 11.00000 -1.50000
AFIX 0
C3 1 0.163113 0.239574 0.539055 11.00000 0.03607 0.03850 =
0.03048 0.01697 -0.01167 -0.00522
AFIX 43
H3 2 0.145692 0.188654 0.604642 11.00000 -1.20000
AFIX 0
O5 4 0.359952 0.840961 0.631048 11.00000 0.04158 0.03364 =
0.02266 -0.00030 -0.00836 0.00946
O6 4 0.366371 0.959641 0.475890 11.00000 0.03504 0.03266 =
0.02899 0.00337 -0.01212 0.00426
O7 4 0.315736 0.091114 0.905559 11.00000 0.04008 0.03381 =
0.04476 -0.00531 -0.02285 -0.00209
O8 4 0.574124 0.064063 0.770425 11.00000 0.04338 0.06724 =
0.02897 0.00932 -0.01298 -0.00442
H8B 2 10.636127 10.034513 10.792909 11.00000 -1.50000
H8A 2 10.578784 10.040323 10.705070 11.00000 -1.50000
O9 4 0.755652 0.947670 0.854948 11.00000 0.03245 0.06702 =
0.04509 -0.01258 -0.01346 -0.00459
H9B 2 10.826163 10.978724 10.825294 11.00000 -1.50000
H9A 2 10.737103 10.958906 10.928370 11.00000 -1.50000
C25 1 0.403920 0.868794 0.519238 11.00000 0.02694 0.03215 =
0.02396 -0.00184 -0.01037 0.00374
C26 1 0.505143 0.776527 0.447467 11.00000 0.05397 0.05628 =
0.03020 -0.00505 -0.00988 0.02800
AFIX 137
H26A 2 0.467064 0.728772 0.407821 11.00000 -1.50000
H26B 2 0.540202 0.725416 0.497661 11.00000 -1.50000
H26C 2 0.572964 0.816326 0.390973 11.00000 -1.50000
AFIX 0
H7A 2 10.273421 10.103127 10.867949 11.00000 10.05000
H7B 2 10.393502 10.085423 10.858788 11.00000 10.05000
H5 2 10.302883 10.895436 10.668488 11.00000 10.07102
HKLF 4
REM SIR92 run in space group P -1
REM wR2 = 0.0815, GooF = S = 1.053, Restrained GooF = 1.053 for all data
REM R1 = 0.0296 for 6436 Fo > 4sig(Fo) and 0.0363 for all 7452 data
REM 364 parameters refined using 4 restraints
END
WGHT 0.0416 0.4558
REM Highest difference peak 0.419, deepest hole -0.371, 1-sigma level 0.054
Q1 1 0.4950 0.6279 0.1030 11.00000 0.05 0.42
Q2 1 0.2786 0.0421 0.8652 11.00000 0.05 0.39
Q3 1 0.7554 1.0157 0.8605 11.00000 0.05 0.38
Q4 1 0.4622 0.7736 -0.0319 11.00000 0.05 0.35
Q5 1 0.1727 0.4988 0.4564 11.00000 0.05 0.34
Q6 1 0.6666 0.5801 0.1872 11.00000 0.05 0.31
Q7 1 0.0368 0.9201 0.7944 11.00000 0.05 0.31
Q8 1 0.5792 0.4600 0.2768 11.00000 0.05 0.30
Q9 1 0.1661 0.3980 0.4971 11.00000 0.05 0.30
Q10 1 0.2126 0.4135 0.4028 11.00000 0.05 0.30
;
_shelx_res_checksum 83225
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
Cu Cu1 0.27208(2) 0.50390(2) 0.20980(2) 0.01722(6) Uani d 1 . .
C C2 0.20686(16) 0.19209(14) 0.42857(15) 0.0319(3) Uani d 1 . .
H H2 0.219242 0.109182 0.418838 0.038 Uiso calc 1 . .
C C20 0.27380(14) 0.67774(13) 0.01845(12) 0.0220(3) Uani d 1 . .
H H20 0.192645 0.654420 0.028961 0.026 Uiso calc 1 . .
O O2 0.20865(9) 0.40753(9) 0.11614(9) 0.0216(2) Uani d 1 . .
O O4 0.20081(11) 0.99389(11) 0.76859(11) 0.0363(3) Uani d 1 . .
N N3 0.46735(11) 0.49874(10) 0.20837(10) 0.0191(2) Uani d 1 . .
O O1 0.02070(10) 0.51918(10) 0.19082(9) 0.0282(2) Uani d 1 . .
C C17 0.51367(14) 0.74396(12) -0.01368(13) 0.0221(3) Uani d 1 . .
H H17 0.595780 0.764818 -0.024124 0.026 Uiso calc 1 . .
C C8 0.11046(16) 0.76062(16) 0.54841(16) 0.0344(4) Uani d 1 . .
H H8 0.081830 0.806154 0.615656 0.041 Uiso calc 1 . .
N N1 0.21842(11) 0.38984(10) 0.34423(10) 0.0187(2) Uani d 1 . .
N N2 0.19928(11) 0.62534(10) 0.34739(10) 0.0200(2) Uani d 1 . .
C C19 0.32137(15) 0.76594(13) -0.06415(13) 0.0252(3) Uani d 1 . .
H H19 0.272712 0.802220 -0.108145 0.030 Uiso calc 1 . .
O O3 0.01773(12) 0.95657(14) 0.74876(13) 0.0493(4) Uani d 1 . .
N N4 0.34123(11) 0.62436(10) 0.08437(10) 0.0178(2) Uani d 1 . .
C C1 0.23192(14) 0.26982(13) 0.33276(14) 0.0242(3) Uani d 1 . .
H H1 0.258859 0.238229 0.258286 0.029 Uiso calc 1 . .
C C6 0.16399(13) 0.57070(13) 0.45367(12) 0.0202(3) Uani d 1 . .
C C15 0.52739(12) 0.59088(12) 0.14451(11) 0.0173(2) Uani d 1 . .
C C18 0.44278(15) 0.79961(13) -0.08053(13) 0.0255(3) Uani d 1 . .
H H18 0.476656 0.858955 -0.135786 0.031 Uiso calc 1 . .
C C13 0.70201(14) 0.55011(14) 0.21823(14) 0.0267(3) Uani d 1 . .
H H13 0.780400 0.567623 0.222134 0.032 Uiso calc 1 . .
C C4 0.14524(15) 0.36336(15) 0.55193(13) 0.0289(3) Uani d 1 . .
H H4 0.113584 0.396516 0.625898 0.035 Uiso calc 1 . .
C C12 0.64192(15) 0.45412(15) 0.28189(14) 0.0286(3) Uani d 1 . .
H H12 0.679836 0.405328 0.328158 0.034 Uiso calc 1 . .
C C5 0.17558(13) 0.43706(13) 0.45203(12) 0.0198(3) Uani d 1 . .
C C11 0.52418(14) 0.43187(14) 0.27555(13) 0.0249(3) Uani d 1 . .
H H11 0.482997 0.368161 0.319549 0.030 Uiso calc 1 . .
C C21 0.08728(13) 0.43137(13) 0.13494(12) 0.0208(3) Uani d 1 . .
C C14 0.64414(14) 0.62022(13) 0.14831(13) 0.0224(3) Uani d 1 . .
H H14 0.682800 0.685421 0.104979 0.027 Uiso calc 1 . .
C C23 0.07964(15) 1.01243(14) 0.79120(13) 0.0260(3) Uani d 1 . .
C C7 0.11925(14) 0.63576(15) 0.55621(13) 0.0278(3) Uani d 1 . .
H H7 0.095642 0.596292 0.628728 0.033 Uiso calc 1 . .
C C16 0.45967(12) 0.65679(11) 0.06886(11) 0.0170(2) Uani d 1 . .
C C24 0.00919(19) 1.11281(17) 0.87447(18) 0.0421(4) Uani d 1 . .
H H24A 0.019512 1.188813 0.833044 0.063 Uiso calc 1 . .
H H24B 0.044333 1.111701 0.936373 0.063 Uiso calc 1 . .
H H24C -0.081002 1.101669 0.906858 0.063 Uiso calc 1 . .
C C10 0.18965(15) 0.74613(13) 0.34065(14) 0.0274(3) Uani d 1 . .
H H10 0.213843 0.784045 0.267379 0.033 Uiso calc 1 . .
C C9 0.14479(16) 0.81604(15) 0.43951(17) 0.0360(4) Uani d 1 . .
H H9 0.137909 0.899605 0.432432 0.043 Uiso calc 1 . .
C C22 0.02787(17) 0.34497(16) 0.08280(16) 0.0338(4) Uani d 1 . .
H H22A -0.063504 0.349434 0.124309 0.051 Uiso calc 1 . .
H H22B 0.066226 0.264444 0.088993 0.051 Uiso calc 1 . .
H H22C 0.043135 0.366143 0.001959 0.051 Uiso calc 1 . .
C C3 0.16311(17) 0.23957(16) 0.53906(15) 0.0356(4) Uani d 1 . .
H H3 0.145692 0.188654 0.604642 0.043 Uiso calc 1 . .
O O5 0.35995(12) 0.84096(11) 0.63105(10) 0.0344(3) Uani d 1 . .
O O6 0.36637(12) 0.95964(10) 0.47589(10) 0.0327(3) Uani d 1 . .
O O7 0.31574(12) 0.09111(11) 0.90556(12) 0.0373(3) Uani d 1 . .
O O8 0.57412(14) 0.06406(14) 0.77043(11) 0.0469(3) Uani d 1 . .
H H8B 0.636127 0.034513 0.792909 0.070 Uiso d 1 . .
H H8A 0.578784 0.040323 0.705070 0.070 Uiso d 1 . .
O O9 0.75565(13) 0.94767(14) 0.85495(13) 0.0477(3) Uani d 1 . .
H H9B 0.826163 0.978724 0.825294 0.072 Uiso d 1 . .
H H9A 0.737103 0.958906 0.928370 0.072 Uiso d 1 . .
C C25 0.40392(15) 0.86879(14) 0.51924(13) 0.0278(3) Uani d 1 . .
C C26 0.5051(2) 0.7765(2) 0.44747(17) 0.0507(5) Uani d 1 . .
H H26A 0.467064 0.728772 0.407821 0.076 Uiso calc 1 . .
H H26B 0.540202 0.725416 0.497661 0.076 Uiso calc 1 . .
H H26C 0.572964 0.816326 0.390973 0.076 Uiso calc 1 . .
H H7A 0.273421 0.103127 0.867949 0.050 Uiso d 1 . .
H H7B 0.393502 0.085423 0.858788 0.050 Uiso d 1 . .
H H5 0.302883 0.895436 0.668488 0.071 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 0.01914(9) 0.01857(9) 0.01475(9) -0.00464(6) -0.00622(6) 0.00140(6)
C2 0.0304(8) 0.0228(7) 0.0390(9) -0.0009(6) -0.0093(7) 0.0084(6)
C20 0.0192(6) 0.0265(7) 0.0213(7) -0.0007(5) -0.0088(5) 0.0008(5)
O2 0.0198(5) 0.0254(5) 0.0205(5) -0.0033(4) -0.0072(4) -0.0047(4)
O4 0.0284(6) 0.0469(7) 0.0334(6) 0.0029(5) -0.0098(5) -0.0173(5)
N3 0.0173(5) 0.0219(5) 0.0183(6) -0.0014(4) -0.0066(4) 0.0011(4)
O1 0.0219(5) 0.0361(6) 0.0259(5) 0.0004(4) -0.0071(4) -0.0072(4)
C17 0.0206(7) 0.0204(6) 0.0226(7) -0.0031(5) -0.0037(5) -0.0002(5)
C8 0.0251(8) 0.0422(9) 0.0352(9) -0.0038(7) -0.0057(7) -0.0220(7)
N1 0.0172(5) 0.0203(5) 0.0178(5) -0.0028(4) -0.0047(4) 0.0007(4)
N2 0.0174(5) 0.0211(5) 0.0209(6) -0.0041(4) -0.0048(4) -0.0032(4)
C19 0.0271(7) 0.0252(7) 0.0222(7) 0.0039(6) -0.0096(6) 0.0036(5)
O3 0.0317(7) 0.0640(9) 0.0511(8) -0.0033(6) -0.0071(6) -0.0373(7)
N4 0.0172(5) 0.0197(5) 0.0165(5) -0.0016(4) -0.0057(4) 0.0002(4)
C1 0.0221(7) 0.0205(6) 0.0274(7) -0.0024(5) -0.0050(6) 0.0001(5)
C6 0.0144(6) 0.0277(7) 0.0196(7) -0.0032(5) -0.0062(5) -0.0037(5)
C15 0.0160(6) 0.0198(6) 0.0147(6) 0.0004(5) -0.0036(5) -0.0035(5)
C18 0.0281(7) 0.0215(7) 0.0223(7) -0.0012(6) -0.0038(6) 0.0050(5)
C13 0.0193(7) 0.0361(8) 0.0280(8) -0.0023(6) -0.0115(6) -0.0050(6)
C4 0.0271(7) 0.0406(9) 0.0186(7) -0.0038(6) -0.0083(6) 0.0051(6)
C12 0.0251(7) 0.0352(8) 0.0298(8) 0.0015(6) -0.0166(6) 0.0013(6)
C5 0.0146(6) 0.0276(7) 0.0178(6) -0.0028(5) -0.0063(5) 0.0012(5)
C11 0.0228(7) 0.0274(7) 0.0252(7) -0.0022(6) -0.0101(6) 0.0045(6)
C21 0.0215(7) 0.0269(7) 0.0158(6) -0.0069(5) -0.0078(5) 0.0024(5)
C14 0.0202(7) 0.0254(7) 0.0218(7) -0.0041(5) -0.0062(5) -0.0030(5)
C23 0.0297(8) 0.0265(7) 0.0201(7) 0.0004(6) -0.0068(6) -0.0041(5)
C7 0.0211(7) 0.0415(9) 0.0219(7) -0.0040(6) -0.0071(6) -0.0088(6)
C16 0.0167(6) 0.0177(6) 0.0156(6) -0.0007(5) -0.0044(5) -0.0028(5)
C24 0.0392(10) 0.0395(9) 0.0461(11) 0.0062(8) -0.0125(8) -0.0231(8)
C10 0.0246(7) 0.0223(7) 0.0319(8) -0.0062(6) -0.0037(6) -0.0035(6)
C9 0.0313(8) 0.0259(7) 0.0476(10) -0.0071(6) -0.0059(7) -0.0146(7)
C22 0.0310(8) 0.0401(9) 0.0372(9) -0.0112(7) -0.0169(7) -0.0065(7)
C3 0.0361(9) 0.0385(9) 0.0305(9) -0.0052(7) -0.0117(7) 0.0170(7)
O5 0.0416(7) 0.0336(6) 0.0227(6) 0.0095(5) -0.0084(5) -0.0003(4)
O6 0.0350(6) 0.0327(6) 0.0290(6) 0.0043(5) -0.0121(5) 0.0034(5)
O7 0.0401(7) 0.0338(6) 0.0448(7) -0.0021(5) -0.0228(6) -0.0053(5)
O8 0.0434(7) 0.0672(9) 0.0290(7) -0.0044(7) -0.0130(6) 0.0093(6)
O9 0.0324(7) 0.0670(9) 0.0451(8) -0.0046(6) -0.0135(6) -0.0126(7)
C25 0.0269(7) 0.0322(8) 0.0240(7) 0.0037(6) -0.0104(6) -0.0018(6)
C26 0.0540(12) 0.0563(12) 0.0302(9) 0.0280(10) -0.0099(9) -0.0051(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O2 Cu1 N1 . . 91.16(5) y
O2 Cu1 N4 . . 95.59(5) y
N1 Cu1 N4 . . 172.71(5) y
O2 Cu1 N2 . . 139.29(4) y
N1 Cu1 N2 . . 79.92(5) y
N4 Cu1 N2 . . 96.61(5) y
O2 Cu1 N3 . . 127.23(4) y
N1 Cu1 N3 . . 94.57(5) y
N4 Cu1 N3 . . 79.16(4) y
N2 Cu1 N3 . . 93.23(4) y
C3 C2 C1 . . 118.86(15) ?
C3 C2 H2 . . 120.6 ?
C1 C2 H2 . . 120.6 ?
N4 C20 C19 . . 122.00(13) ?
N4 C20 H20 . . 119.0 ?
C19 C20 H20 . . 119.0 ?
C21 O2 Cu1 . . 113.10(9) ?
C11 N3 C15 . . 118.64(12) ?
C11 N3 Cu1 . . 128.67(10) ?
C15 N3 Cu1 . . 111.60(9) ?
C16 C17 C18 . . 118.78(13) ?
C16 C17 H17 . . 120.6 ?
C18 C17 H17 . . 120.6 ?
C9 C8 C7 . . 118.98(14) ?
C9 C8 H8 . . 120.5 ?
C7 C8 H8 . . 120.5 ?
C1 N1 C5 . . 119.72(12) ?
C1 N1 Cu1 . . 123.21(10) ?
C5 N1 Cu1 . . 116.87(9) ?
C10 N2 C6 . . 118.84(12) ?
C10 N2 Cu1 . . 127.93(10) ?
C6 N2 Cu1 . . 113.17(9) ?
C20 C19 C18 . . 118.91(13) ?
C20 C19 H19 . . 120.5 ?
C18 C19 H19 . . 120.5 ?
C20 N4 C16 . . 119.39(12) ?
C20 N4 Cu1 . . 123.11(10) ?
C16 N4 Cu1 . . 117.44(9) ?
N1 C1 C2 . . 121.78(14) ?
N1 C1 H1 . . 119.1 ?
C2 C1 H1 . . 119.1 ?
N2 C6 C7 . . 121.92(14) ?
N2 C6 C5 . . 114.82(12) ?
C7 C6 C5 . . 123.25(13) ?
N3 C15 C14 . . 122.15(12) ?
N3 C15 C16 . . 114.79(12) ?
C14 C15 C16 . . 123.05(12) ?
C19 C18 C17 . . 119.45(13) ?
C19 C18 H18 . . 120.3 ?
C17 C18 H18 . . 120.3 ?
C12 C13 C14 . . 119.32(13) ?
C12 C13 H13 . . 120.3 ?
C14 C13 H13 . . 120.3 ?
C3 C4 C5 . . 118.70(15) ?
C3 C4 H4 . . 120.6 ?
C5 C4 H4 . . 120.6 ?
C13 C12 C11 . . 118.80(14) ?
C13 C12 H12 . . 120.6 ?
C11 C12 H12 . . 120.6 ?
N1 C5 C4 . . 121.09(13) ?
N1 C5 C6 . . 114.84(12) ?
C4 C5 C6 . . 124.07(13) ?
N3 C11 C12 . . 122.47(14) ?
N3 C11 H11 . . 118.8 ?
C12 C11 H11 . . 118.8 ?
O1 C21 O2 . . 123.73(13) ?
O1 C21 C22 . . 120.78(13) ?
O2 C21 C22 . . 115.48(13) ?
C15 C14 C13 . . 118.59(13) ?
C15 C14 H14 . . 120.7 ?
C13 C14 H14 . . 120.7 ?
O3 C23 O4 . . 124.72(14) ?
O3 C23 C24 . . 118.88(15) ?
O4 C23 C24 . . 116.38(15) ?
C8 C7 C6 . . 118.84(15) ?
C8 C7 H7 . . 120.6 ?
C6 C7 H7 . . 120.6 ?
N4 C16 C17 . . 121.46(12) ?
N4 C16 C15 . . 115.27(11) ?
C17 C16 C15 . . 123.26(12) ?
C23 C24 H24A . . 109.5 ?
C23 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C23 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
N2 C10 C9 . . 122.01(15) ?
N2 C10 H10 . . 119.0 ?
C9 C10 H10 . . 119.0 ?
C8 C9 C10 . . 119.39(15) ?
C8 C9 H9 . . 120.3 ?
C10 C9 H9 . . 120.3 ?
C21 C22 H22A . . 109.5 ?
C21 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C21 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C2 C3 C4 . . 119.80(14) ?
C2 C3 H3 . . 120.1 ?
C4 C3 H3 . . 120.1 ?
C25 O5 H5 . . 110.82 ?
H7A O7 H7B . . 106.32 ?
H8B O8 H8A . . 114.12 ?
H9B O9 H9A . . 102.25 ?
O6 C25 O5 . . 124.02(14) ?
O6 C25 C26 . . 122.16(15) ?
O5 C25 C26 . . 113.81(14) ?
C25 C26 H26A . . 109.5 ?
C25 C26 H26B . . 109.5 ?
H26A C26 H26B . . 109.5 ?
C25 C26 H26C . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
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 O2 . 1.9594(10) y
Cu1 N1 . 1.9796(12) y
Cu1 N4 . 1.9810(12) y
Cu1 N2 . 2.0958(12) y
Cu1 N3 . 2.1522(12) y
C2 C3 . 1.381(3) ?
C2 C1 . 1.381(2) ?
C2 H2 . 0.9300 ?
C20 N4 . 1.3461(17) ?
C20 C19 . 1.379(2) ?
C20 H20 . 0.9300 ?
O2 C21 . 1.2820(17) ?
O4 C23 . 1.268(2) ?
N3 C11 . 1.3407(18) ?
N3 C15 . 1.3480(18) ?
O1 C21 . 1.2396(18) ?
C17 C16 . 1.3870(19) ?
C17 C18 . 1.391(2) ?
C17 H17 . 0.9300 ?
C8 C9 . 1.378(3) ?
C8 C7 . 1.388(2) ?
C8 H8 . 0.9300 ?
N1 C1 . 1.3435(18) ?
N1 C5 . 1.3510(18) ?
N2 C10 . 1.3424(19) ?
N2 C6 . 1.3473(18) ?
C19 C18 . 1.384(2) ?
C19 H19 . 0.9300 ?
O3 C23 . 1.230(2) ?
N4 C16 . 1.3500(17) ?
C1 H1 . 0.9300 ?
C6 C7 . 1.391(2) ?
C6 C5 . 1.486(2) ?
C15 C14 . 1.3880(19) ?
C15 C16 . 1.4908(18) ?
C18 H18 . 0.9300 ?
C13 C12 . 1.382(2) ?
C13 C14 . 1.390(2) ?
C13 H13 . 0.9300 ?
C4 C3 . 1.386(3) ?
C4 C5 . 1.392(2) ?
C4 H4 . 0.9300 ?
C12 C11 . 1.385(2) ?
C12 H12 . 0.9300 ?
C11 H11 . 0.9300 ?
C21 C22 . 1.511(2) ?
C14 H14 . 0.9300 ?
C23 C24 . 1.512(2) ?
C7 H7 . 0.9300 ?
C24 H24A . 0.9600 ?
C24 H24B . 0.9600 ?
C24 H24C . 0.9600 ?
C10 C9 . 1.386(2) ?
C10 H10 . 0.9300 ?
C9 H9 . 0.9300 ?
C22 H22A . 0.9600 ?
C22 H22B . 0.9600 ?
C22 H22C . 0.9600 ?
C3 H3 . 0.9300 ?
O5 C25 . 1.3106(19) ?
O5 H5 . 0.8506 ?
O6 C25 . 1.2133(19) ?
O7 H7A . 0.7577 ?
O7 H7B . 0.8511 ?
O8 H8B . 0.8498 ?
O8 H8A . 0.8376 ?
O9 H9B . 0.8459 ?
O9 H9A . 0.8599 ?
C25 C26 . 1.500(2) ?
C26 H26A . 0.9600 ?
C26 H26B . 0.9600 ?
C26 H26C . 0.9600 ?
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
C2 H2 O6 1_545 0.93 2.44 3.1081(19) 129.0 yes
C1 H1 O9 2_666 0.93 2.61 3.398(2) 142.4 yes
C14 H14 O7 2_666 0.93 2.50 3.306(2) 145.7 yes
O8 H8B O9 1_545 0.8498 1.8895 2.7306(19) 170.15 yes
O9 H9B O3 1_655 0.8459 1.9942 2.753(2) 148.84 yes
O9 H9A O7 2_667 0.8599 1.9685 2.769(2) 154.44 yes
O8 H8A O6 2_666 0.8376 2.0758 2.8648(18) 156.81 yes
O7 H7B O8 . 0.8511 1.9119 2.758(2) 172.63 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
N4 C20 C19 C18 . . . . 0.7(2) ?
C19 C20 N4 C16 . . . . -0.7(2) ?
C19 C20 N4 Cu1 . . . . 176.51(11) ?
C5 N1 C1 C2 . . . . -2.0(2) ?
Cu1 N1 C1 C2 . . . . 172.74(11) ?
C3 C2 C1 N1 . . . . 2.0(2) ?
C10 N2 C6 C7 . . . . -0.7(2) ?
Cu1 N2 C6 C7 . . . . 176.81(11) ?
C10 N2 C6 C5 . . . . 178.80(12) ?
Cu1 N2 C6 C5 . . . . -3.74(14) ?
C11 N3 C15 C14 . . . . -1.5(2) ?
Cu1 N3 C15 C14 . . . . 167.52(10) ?
C11 N3 C15 C16 . . . . 177.56(12) ?
Cu1 N3 C15 C16 . . . . -13.37(14) ?
C20 C19 C18 C17 . . . . 0.0(2) ?
C16 C17 C18 C19 . . . . -0.7(2) ?
C14 C13 C12 C11 . . . . -1.1(2) ?
C1 N1 C5 C4 . . . . 0.1(2) ?
Cu1 N1 C5 C4 . . . . -174.95(11) ?
C1 N1 C5 C6 . . . . -179.71(12) ?
Cu1 N1 C5 C6 . . . . 5.21(15) ?
C3 C4 C5 N1 . . . . 1.7(2) ?
C3 C4 C5 C6 . . . . -178.43(14) ?
N2 C6 C5 N1 . . . . -0.71(17) ?
C7 C6 C5 N1 . . . . 178.73(13) ?
N2 C6 C5 C4 . . . . 179.45(13) ?
C7 C6 C5 C4 . . . . -1.1(2) ?
C15 N3 C11 C12 . . . . 0.1(2) ?
Cu1 N3 C11 C12 . . . . -166.81(12) ?
C13 C12 C11 N3 . . . . 1.2(2) ?
Cu1 O2 C21 O1 . . . . 11.48(17) ?
Cu1 O2 C21 C22 . . . . -169.15(10) ?
N3 C15 C14 C13 . . . . 1.6(2) ?
C16 C15 C14 C13 . . . . -177.43(13) ?
C12 C13 C14 C15 . . . . -0.2(2) ?
C9 C8 C7 C6 . . . . 0.8(2) ?
N2 C6 C7 C8 . . . . 0.2(2) ?
C5 C6 C7 C8 . . . . -179.19(13) ?
C20 N4 C16 C17 . . . . -0.06(19) ?
Cu1 N4 C16 C17 . . . . -177.41(10) ?
C20 N4 C16 C15 . . . . -178.93(12) ?
Cu1 N4 C16 C15 . . . . 3.72(15) ?
C18 C17 C16 N4 . . . . 0.7(2) ?
C18 C17 C16 C15 . . . . 179.53(13) ?
N3 C15 C16 N4 . . . . 7.18(17) ?
C14 C15 C16 N4 . . . . -173.72(12) ?
N3 C15 C16 C17 . . . . -171.67(12) ?
C14 C15 C16 C17 . . . . 7.4(2) ?
C6 N2 C10 C9 . . . . 0.1(2) ?
Cu1 N2 C10 C9 . . . . -176.95(12) ?
C7 C8 C9 C10 . . . . -1.3(2) ?
N2 C10 C9 C8 . . . . 0.9(3) ?
C1 C2 C3 C4 . . . . 0.0(3) ?
C5 C4 C3 C2 . . . . -1.8(2) ?
_cod_database_fobs_code 2312593