#------------------------------------------------------------------------------
#$Date: 2020-03-20 07:55:08 +0200 (Fri, 20 Mar 2020) $
#$Revision: 249568 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/85/2108591.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_2108591
loop_
_publ_author_name
'Shin, Jong Won'
'Jeong, Ah Rim'
'Kim, Younghak'
'Kim, Dae-Woong'
'Lee, Sang-Geul'
'Lee, Hyosun'
'Moon, Dohyun'
_publ_section_title
;
 Solvent-triggered single-crystal-to-single-crystal transformation from a
 monomeric to polymeric copper(II) complex based on an aza macrocyclic
 ligand
;
_journal_coeditor_code           RM5028SUP1
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620002371
_journal_volume                  76
_journal_year                    2020
_chemical_formula_moiety         'C16 H42 Cu N6 O2, C12 H6 O4, H2 O'
_chemical_formula_sum            'C28 H50 Cu N6 O7'
_chemical_formula_weight         646.28
_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                70.34(3)
_cell_angle_beta                 79.99(3)
_cell_angle_gamma                73.06(3)
_cell_formula_units_Z            2
_cell_length_a                   10.946(2)
_cell_length_b                   12.502(3)
_cell_length_c                   13.029(3)
_cell_measurement_reflns_used    86556
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.350
_cell_volume                     1600.5(7)
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_collection
' PAL BL2D-SMDC Program(Shin et.al, 2016)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND 4(Putz & Brandenburg, 2014)'
_computing_publication_material  'publCIF(Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2018(Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018(Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17649
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.430
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
' HKL3000sm Scalepack(Otwinowski et al,2003)'
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       needle
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8899
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0526
_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/[σ²(Fo²)+(0.1181P)²+0.0613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7396
_reflns_number_total             8899
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            rm5028sup1.cif
_cod_data_source_block           CuNDC_mono
_cod_original_cell_volume        1600.4(7)
_cod_database_code               2108591
_shelx_shelxl_version_number     2018/3
_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   0.941
_shelx_estimated_absorpt_t_max   0.984
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.74253(2) 0.74501(2) -0.00637(2) 0.03540(10) Uani 1 1 d . . . . .
O1 O 0.94326(16) 0.61210(14) 0.05384(13) 0.0467(4) Uani 1 1 d D . . . .
H1O1 H 1.016(2) 0.620(2) 0.004(2) 0.070 Uiso 1 1 d D U . . .
H2O1 H 0.951(3) 0.5310(10) 0.080(2) 0.070 Uiso 1 1 d D U . . .
O2 O 0.5256(2) 0.89356(19) -0.07982(18) 0.0669(5) Uani 1 1 d D . . . .
H1O2 H 0.486(3) 0.912(3) -0.0138(18) 0.100 Uiso 1 1 d D U . . .
H2O2 H 0.456(2) 0.880(3) -0.106(3) 0.100 Uiso 1 1 d D U . . .
N1 N 0.66639(17) 0.61025(16) 0.01233(14) 0.0396(4) Uani 1 1 d . . . . .
H1 H 0.736112 0.538455 0.023860 0.048 Uiso 1 1 calc R U . . .
N2 N 0.66757(17) 0.73820(15) 0.14723(13) 0.0365(3) Uani 1 1 d . . . . .
H2 H 0.587434 0.799866 0.142621 0.044 Uiso 1 1 calc R U . . .
N3 N 0.76986(19) 0.87602(17) 0.16186(15) 0.0448(4) Uani 1 1 d . . . . .
N4 N 0.80889(18) 0.88598(15) -0.02700(14) 0.0394(4) Uani 1 1 d . . . . .
H4 H 0.736692 0.955532 -0.044052 0.047 Uiso 1 1 calc R U . . .
N5 N 0.81055(18) 0.75610(16) -0.16173(14) 0.0396(4) Uani 1 1 d . . . . .
H5 H 0.888265 0.692335 -0.160548 0.047 Uiso 1 1 calc R U . . .
N6 N 0.6805(2) 0.6363(2) -0.18439(16) 0.0536(5) Uani 1 1 d . . . . .
C1 C 0.5778(2) 0.5989(2) 0.11367(18) 0.0445(5) Uani 1 1 d . . . . .
H1A H 0.565089 0.520199 0.141581 0.053 Uiso 1 1 calc R U . . .
H1AB H 0.495164 0.653978 0.097674 0.053 Uiso 1 1 calc R U . . .
C2 C 0.6348(2) 0.62386(19) 0.19818(17) 0.0419(4) Uani 1 1 d . . . . .
H2A H 0.573523 0.626787 0.261262 0.050 Uiso 1 1 calc R U . . .
H2AB H 0.711078 0.562385 0.222212 0.050 Uiso 1 1 calc R U . . .
C3 C 0.7516(2) 0.7590(2) 0.21295(17) 0.0428(4) Uani 1 1 d . . . . .
H3A H 0.712195 0.751308 0.286911 0.051 Uiso 1 1 calc R U . . .
H3AB H 0.833621 0.701577 0.216469 0.051 Uiso 1 1 calc R U . . .
C4 C 0.8644(2) 0.8856(2) 0.06896(19) 0.0462(5) Uani 1 1 d . . . . .
H4A H 0.939193 0.819935 0.085845 0.055 Uiso 1 1 calc R U . . .
H4AB H 0.891150 0.957437 0.052645 0.055 Uiso 1 1 calc R U . . .
C5 C 0.9017(2) 0.8948(2) -0.12506(18) 0.0454(5) Uani 1 1 d . . . . .
H5A H 0.983284 0.839132 -0.106132 0.054 Uiso 1 1 calc R U . . .
H5AB H 0.915519 0.973123 -0.153178 0.054 Uiso 1 1 calc R U . . .
C6 C 0.8480(2) 0.8686(2) -0.21097(17) 0.0467(5) Uani 1 1 d . . . . .
H6A H 0.773890 0.931285 -0.238270 0.056 Uiso 1 1 calc R U . . .
H6AB H 0.912021 0.863297 -0.271896 0.056 Uiso 1 1 calc R U . . .
C7 C 0.7189(3) 0.7439(2) -0.22794(18) 0.0502(5) Uani 1 1 d . . . . .
H7A H 0.643141 0.808704 -0.232902 0.060 Uiso 1 1 calc R U . . .
H7AB H 0.758784 0.749714 -0.301525 0.060 Uiso 1 1 calc R U . . .
C8 C 0.6009(3) 0.6228(3) -0.0845(2) 0.0549(6) Uani 1 1 d . . . . .
H8A H 0.568776 0.554031 -0.069709 0.066 Uiso 1 1 calc R U . . .
H8AB H 0.527716 0.690396 -0.093446 0.066 Uiso 1 1 calc R U . . .
C9 C 0.7909(3) 0.9292(2) 0.2403(2) 0.0524(6) Uani 1 1 d . . . . .
H9A H 0.718567 0.929758 0.295172 0.063 Uiso 1 1 calc R U . . .
H9AB H 0.791985 1.010199 0.201751 0.063 Uiso 1 1 calc R U . . .
C10 C 0.9132(3) 0.8689(3) 0.2983(2) 0.0643(7) Uani 1 1 d . . . . .
H10A H 0.986240 0.866794 0.244290 0.077 Uiso 1 1 calc R U . . .
H10B H 0.911714 0.788535 0.339606 0.077 Uiso 1 1 calc R U . . .
C11 C 0.9290(4) 0.9323(3) 0.3766(3) 0.0755(8) Uani 1 1 d . . . . .
H11A H 1.019004 0.914282 0.387586 0.091 Uiso 1 1 calc R U . . .
H11B H 0.899598 1.016392 0.343575 0.091 Uiso 1 1 calc R U . . .
C12 C 0.8559(6) 0.8968(5) 0.4832(3) 0.1223(19) Uani 1 1 d . . . . .
H12A H 0.851984 0.949395 0.523670 0.183 Uiso 1 1 calc R U . . .
H12B H 0.897511 0.818332 0.523638 0.183 Uiso 1 1 calc R U . . .
H12C H 0.770588 0.899417 0.471846 0.183 Uiso 1 1 calc R U . . .
C13 C 0.7717(3) 0.5302(3) -0.1978(3) 0.0662(7) Uani 1 1 d . U . . .
H13A H 0.737565 0.463340 -0.155725 0.079 Uiso 1 1 calc R U . . .
H13B H 0.850560 0.521054 -0.167811 0.079 Uiso 1 1 calc R U . . .
C14 C 0.8019(6) 0.5286(4) -0.3127(4) 0.1160(15) Uani 1 1 d . U . . .
H14A H 0.866486 0.457053 -0.314662 0.139 Uiso 1 1 calc R U . . .
H14B H 0.838007 0.594270 -0.354620 0.139 Uiso 1 1 calc R U . . .
C15 C 0.6868(7) 0.5355(5) -0.3662(4) 0.1465(19) Uani 1 1 d . U . . .
H15A H 0.657100 0.464792 -0.330667 0.176 Uiso 1 1 calc R U . . .
H15B H 0.617999 0.601796 -0.356860 0.176 Uiso 1 1 calc R U . . .
C16 C 0.7189(10) 0.5489(7) -0.4861(5) 0.218(4) Uani 1 1 d . U . . .
H16A H 0.663796 0.516475 -0.510233 0.327 Uiso 1 1 calc R U . . .
H16B H 0.806561 0.508160 -0.498133 0.327 Uiso 1 1 calc R U . . .
H16C H 0.706815 0.630622 -0.526396 0.327 Uiso 1 1 calc R U . . .
O3 O 0.83009(17) 0.36242(15) 0.08615(12) 0.0506(4) Uani 1 1 d . . . . .
O4 O 0.93372(16) 0.39340(15) 0.20262(12) 0.0481(4) Uani 1 1 d . . . . .
O5 O 0.7453(2) 0.2086(2) 0.79533(14) 0.0697(6) Uani 1 1 d . . . . .
O6 O 0.59965(16) 0.10487(15) 0.86034(12) 0.0469(4) Uani 1 1 d . . . . .
C17 C 0.8509(2) 0.35402(18) 0.18148(16) 0.0391(4) Uani 1 1 d . . . . .
C18 C 0.76806(19) 0.29441(17) 0.27645(15) 0.0376(4) Uani 1 1 d . . . . .
C19 C 0.7812(2) 0.28976(18) 0.38141(16) 0.0384(4) Uani 1 1 d . . . . .
H19 H 0.841430 0.322966 0.392969 0.046 Uiso 1 1 calc R U . . .
C20 C 0.70458(19) 0.23525(17) 0.47177(15) 0.0365(4) Uani 1 1 d . . . . .
C21 C 0.7181(2) 0.22774(19) 0.58096(15) 0.0389(4) Uani 1 1 d . . . . .
H21 H 0.777109 0.261634 0.593351 0.047 Uiso 1 1 calc R U . . .
C22 C 0.64625(19) 0.17184(18) 0.66792(15) 0.0367(4) Uani 1 1 d . . . . .
C23 C 0.5557(2) 0.1210(2) 0.64888(17) 0.0437(4) Uani 1 1 d . . . . .
H23 H 0.506786 0.082624 0.707764 0.052 Uiso 1 1 calc R U . . .
C24 C 0.5392(2) 0.1278(2) 0.54513(18) 0.0480(5) Uani 1 1 d . . . . .
H24 H 0.478545 0.094639 0.534304 0.058 Uiso 1 1 calc R U . . .
C25 C 0.6133(2) 0.18446(19) 0.45376(16) 0.0408(4) Uani 1 1 d . . . . .
C26 C 0.6015(2) 0.1904(2) 0.34512(18) 0.0499(5) Uani 1 1 d . . . . .
H26 H 0.541975 0.157439 0.332145 0.060 Uiso 1 1 calc R U . . .
C27 C 0.6763(2) 0.2438(2) 0.25931(16) 0.0458(5) Uani 1 1 d . . . . .
H27 H 0.666807 0.247039 0.188704 0.055 Uiso 1 1 calc R U . . .
C28 C 0.6659(2) 0.1620(2) 0.78357(16) 0.0422(4) Uani 1 1 d . . . . .
O7 O 0.7517(4) 0.1956(3) 1.0086(2) 0.1104(11) Uani 1 1 d D U . . .
H1O7 H 0.787(5) 0.184(4) 0.940(2) 0.166 Uiso 1 1 d D U . . .
H2O7 H 0.764(6) 0.271(2) 1.002(4) 0.166 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0019 0.0011 '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 0.0040 0.0024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0074 0.0043 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3373 0.9674 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Cu1 N2 177.69(7) . . ?
N5 Cu1 N1 93.73(8) . . ?
N2 Cu1 N1 86.15(7) . . ?
N5 Cu1 N4 86.63(8) . . ?
N2 Cu1 N4 93.36(7) . . ?
N1 Cu1 N4 176.77(7) . . ?
N5 Cu1 O1 89.49(7) . . ?
N2 Cu1 O1 92.82(7) . . ?
N1 Cu1 O1 91.38(7) . . ?
N4 Cu1 O1 91.82(7) . . ?
Cu1 O1 H1O1 116.2(18) . . ?
Cu1 O1 H2O1 119.9(18) . . ?
H1O1 O1 H2O1 104.6(17) . . ?
H1O2 O2 H2O2 101.5(18) . . ?
C1 N1 C8 111.83(18) . . ?
C1 N1 Cu1 107.21(13) . . ?
C8 N1 Cu1 113.82(15) . . ?
C1 N1 H1 107.9 . . ?
C8 N1 H1 107.9 . . ?
Cu1 N1 H1 107.9 . . ?
C2 N2 C3 112.59(17) . . ?
C2 N2 Cu1 107.49(13) . . ?
C3 N2 Cu1 113.69(13) . . ?
C2 N2 H2 107.6 . . ?
C3 N2 H2 107.6 . . ?
Cu1 N2 H2 107.6 . . ?
C4 N3 C3 114.03(18) . . ?
C4 N3 C9 112.23(18) . . ?
C3 N3 C9 113.17(19) . . ?
C4 N4 C5 112.16(18) . . ?
C4 N4 Cu1 115.38(14) . . ?
C5 N4 Cu1 106.43(13) . . ?
C4 N4 H4 107.5 . . ?
C5 N4 H4 107.5 . . ?
Cu1 N4 H4 107.5 . . ?
C6 N5 C7 111.82(17) . . ?
C6 N5 Cu1 107.76(13) . . ?
C7 N5 Cu1 113.71(14) . . ?
C6 N5 H5 107.8 . . ?
C7 N5 H5 107.8 . . ?
Cu1 N5 H5 107.8 . . ?
C8 N6 C7 116.0(2) . . ?
C8 N6 C13 116.0(2) . . ?
C7 N6 C13 118.0(2) . . ?
N1 C1 C2 109.04(17) . . ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
N1 C1 H1AB 109.9 . . ?
C2 C1 H1AB 109.9 . . ?
H1A C1 H1AB 108.3 . . ?
N2 C2 C1 107.93(17) . . ?
N2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
N2 C2 H2AB 110.1 . . ?
C1 C2 H2AB 110.1 . . ?
H2A C2 H2AB 108.4 . . ?
N3 C3 N2 108.68(18) . . ?
N3 C3 H3A 110.0 . . ?
N2 C3 H3A 110.0 . . ?
N3 C3 H3AB 110.0 . . ?
N2 C3 H3AB 110.0 . . ?
H3A C3 H3AB 108.3 . . ?
N3 C4 N4 109.53(18) . . ?
N3 C4 H4A 109.8 . . ?
N4 C4 H4A 109.8 . . ?
N3 C4 H4AB 109.8 . . ?
N4 C4 H4AB 109.8 . . ?
H4A C4 H4AB 108.2 . . ?
N4 C5 C6 108.48(19) . . ?
N4 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
N4 C5 H5AB 110.0 . . ?
C6 C5 H5AB 110.0 . . ?
H5A C5 H5AB 108.4 . . ?
N5 C6 C5 109.19(17) . . ?
N5 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N5 C6 H6AB 109.8 . . ?
C5 C6 H6AB 109.8 . . ?
H6A C6 H6AB 108.3 . . ?
N6 C7 N5 114.10(18) . . ?
N6 C7 H7A 108.7 . . ?
N5 C7 H7A 108.7 . . ?
N6 C7 H7AB 108.7 . . ?
N5 C7 H7AB 108.7 . . ?
H7A C7 H7AB 107.6 . . ?
N6 C8 N1 114.3(2) . . ?
N6 C8 H8A 108.7 . . ?
N1 C8 H8A 108.7 . . ?
N6 C8 H8AB 108.7 . . ?
N1 C8 H8AB 108.7 . . ?
H8A C8 H8AB 107.6 . . ?
N3 C9 C10 115.6(2) . . ?
N3 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N3 C9 H9AB 108.4 . . ?
C10 C9 H9AB 108.4 . . ?
H9A C9 H9AB 107.5 . . ?
C9 C10 C11 112.0(3) . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C12 C11 C10 111.6(3) . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N6 C13 C14 114.3(3) . . ?
N6 C13 H13A 108.7 . . ?
C14 C13 H13A 108.7 . . ?
N6 C13 H13B 108.7 . . ?
C14 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C13 C14 C15 113.4(4) . . ?
C13 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C16 C15 C14 111.2(6) . . ?
C16 C15 H15A 109.4 . . ?
C14 C15 H15A 109.4 . . ?
C16 C15 H15B 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 O3 124.7(2) . . ?
O4 C17 C18 117.82(18) . . ?
O3 C17 C18 117.5(2) . . ?
C19 C18 C27 119.25(19) . . ?
C19 C18 C17 119.76(19) . . ?
C27 C18 C17 120.99(18) . . ?
C18 C19 C20 121.04(19) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C19 C20 C25 119.27(17) . . ?
C19 C20 C21 121.96(18) . . ?
C25 C20 C21 118.76(18) . . ?
C22 C21 C20 121.48(19) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 C23 119.21(18) . . ?
C21 C22 C28 120.20(19) . . ?
C23 C22 C28 120.57(18) . . ?
C24 C23 C22 120.84(19) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 121.0(2) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C20 118.72(18) . . ?
C24 C25 C26 122.6(2) . . ?
C20 C25 C26 118.62(19) . . ?
C27 C26 C25 121.0(2) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C18 120.85(19) . . ?
C26 C27 H27 119.6 . . ?
C18 C27 H27 119.6 . . ?
O5 C28 O6 125.5(2) . . ?
O5 C28 C22 117.83(19) . . ?
O6 C28 C22 116.7(2) . . ?
H1O7 O7 H2O7 104(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N5 2.0046(18) . ?
Cu1 N2 2.0102(17) . ?
Cu1 N1 2.0159(18) . ?
Cu1 N4 2.0164(18) . ?
Cu1 O1 2.4079(19) . ?
O1 H1O1 0.940(10) . ?
O1 H2O1 0.938(10) . ?
O2 H1O2 0.963(10) . ?
O2 H2O2 0.962(10) . ?
N1 C1 1.488(3) . ?
N1 C8 1.499(3) . ?
N1 H1 0.9800 . ?
N2 C2 1.480(3) . ?
N2 C3 1.486(3) . ?
N2 H2 0.9800 . ?
N3 C4 1.446(3) . ?
N3 C3 1.446(3) . ?
N3 C9 1.472(3) . ?
N4 C4 1.480(3) . ?
N4 C5 1.482(3) . ?
N4 H4 0.9800 . ?
N5 C6 1.481(3) . ?
N5 C7 1.501(3) . ?
N5 H5 0.9800 . ?
N6 C8 1.423(3) . ?
N6 C7 1.429(3) . ?
N6 C13 1.453(4) . ?
C1 C2 1.511(3) . ?
C1 H1A 0.9700 . ?
C1 H1AB 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2AB 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3AB 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4AB 0.9700 . ?
C5 C6 1.515(3) . ?
C5 H5A 0.9700 . ?
C5 H5AB 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6AB 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7AB 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8AB 0.9700 . ?
C9 C10 1.520(4) . ?
C9 H9A 0.9700 . ?
C9 H9AB 0.9700 . ?
C10 C11 1.543(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.474(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.481(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.511(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.503(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O3 C17 1.266(2) . ?
O4 C17 1.256(3) . ?
O5 C28 1.233(3) . ?
O6 C28 1.267(3) . ?
C17 C18 1.514(3) . ?
C18 C19 1.380(3) . ?
C18 C27 1.415(3) . ?
C19 C20 1.416(3) . ?
C19 H19 0.9300 . ?
C20 C25 1.417(3) . ?
C20 C21 1.425(3) . ?
C21 C22 1.367(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.416(3) . ?
C22 C28 1.518(3) . ?
C23 C24 1.366(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.417(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.419(3) . ?
C26 C27 1.366(3) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
O7 H1O7 0.956(10) . ?
O7 H2O7 0.957(10) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1O1 O3 0.940(10) 1.905(10) 2.843(2) 175(3) 2_765 yes
O1 H2O1 O4 0.938(10) 1.942(16) 2.788(3) 149(2) . yes
O2 H1O2 O6 0.963(10) 2.024(16) 2.953(3) 161(3) 2_666 yes
N1 H1 O3 0.98 2.08 3.015(3) 158.9 . yes
N2 H2 O6 0.98 2.05 3.007(3) 165.9 2_666 yes
N4 H4 O6 0.98 2.18 3.115(3) 159.7 1_564 yes
N5 H5 O4 0.98 2.01 2.952(3) 159.7 2_765 yes
O7 H1O7 O5 0.956(10) 1.92(4) 2.740(3) 143(5) . yes
O7 H2O7 O3 0.957(10) 2.16(3) 2.979(3) 143(4) 1_556 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 N1 C1 C2 -162.79(19) . . . . ?
Cu1 N1 C1 C2 -37.4(2) . . . . ?
C3 N2 C2 C1 -166.52(18) . . . . ?
Cu1 N2 C2 C1 -40.54(19) . . . . ?
N1 C1 C2 N2 52.5(2) . . . . ?
C4 N3 C3 N2 -79.6(2) . . . . ?
C9 N3 C3 N2 150.46(18) . . . . ?
C2 N2 C3 N3 -175.38(16) . . . . ?
Cu1 N2 C3 N3 62.1(2) . . . . ?
C3 N3 C4 N4 76.8(2) . . . . ?
C9 N3 C4 N4 -152.9(2) . . . . ?
C5 N4 C4 N3 -179.61(17) . . . . ?
Cu1 N4 C4 N3 -57.5(2) . . . . ?
C4 N4 C5 C6 168.01(18) . . . . ?
Cu1 N4 C5 C6 41.0(2) . . . . ?
C7 N5 C6 C5 161.1(2) . . . . ?
Cu1 N5 C6 C5 35.5(2) . . . . ?
N4 C5 C6 N5 -51.8(2) . . . . ?
C8 N6 C7 N5 68.9(3) . . . . ?
C13 N6 C7 N5 -75.3(3) . . . . ?
C6 N5 C7 N6 179.5(2) . . . . ?
Cu1 N5 C7 N6 -58.1(2) . . . . ?
C7 N6 C8 N1 -68.4(3) . . . . ?
C13 N6 C8 N1 76.5(3) . . . . ?
C1 N1 C8 N6 178.8(2) . . . . ?
Cu1 N1 C8 N6 57.2(3) . . . . ?
C4 N3 C9 C10 -65.9(3) . . . . ?
C3 N3 C9 C10 64.9(3) . . . . ?
N3 C9 C10 C11 178.5(2) . . . . ?
C9 C10 C11 C12 82.9(4) . . . . ?
C8 N6 C13 C14 149.4(3) . . . . ?
C7 N6 C13 C14 -66.4(4) . . . . ?
N6 C13 C14 C15 -61.6(5) . . . . ?
C13 C14 C15 C16 172.8(4) . . . . ?
O4 C17 C18 C19 3.0(3) . . . . ?
O3 C17 C18 C19 -175.81(19) . . . . ?
O4 C17 C18 C27 -177.5(2) . . . . ?
O3 C17 C18 C27 3.7(3) . . . . ?
C27 C18 C19 C20 0.0(3) . . . . ?
C17 C18 C19 C20 179.61(18) . . . . ?
C18 C19 C20 C25 0.2(3) . . . . ?
C18 C19 C20 C21 178.9(2) . . . . ?
C19 C20 C21 C22 -178.0(2) . . . . ?
C25 C20 C21 C22 0.7(3) . . . . ?
C20 C21 C22 C23 -0.5(3) . . . . ?
C20 C21 C22 C28 178.08(19) . . . . ?
C21 C22 C23 C24 -0.3(3) . . . . ?
C28 C22 C23 C24 -178.8(2) . . . . ?
C22 C23 C24 C25 0.8(4) . . . . ?
C23 C24 C25 C20 -0.5(4) . . . . ?
C23 C24 C25 C26 178.2(2) . . . . ?
C19 C20 C25 C24 178.5(2) . . . . ?
C21 C20 C25 C24 -0.2(3) . . . . ?
C19 C20 C25 C26 -0.2(3) . . . . ?
C21 C20 C25 C26 -179.0(2) . . . . ?
C24 C25 C26 C27 -178.7(2) . . . . ?
C20 C25 C26 C27 0.0(4) . . . . ?
C25 C26 C27 C18 0.3(4) . . . . ?
C19 C18 C27 C26 -0.3(3) . . . . ?
C17 C18 C27 C26 -179.8(2) . . . . ?
C21 C22 C28 O5 2.0(3) . . . . ?
C23 C22 C28 O5 -179.5(2) . . . . ?
C21 C22 C28 O6 -177.2(2) . . . . ?
C23 C22 C28 O6 1.4(3) . . . . ?

_cod_database_fobs_code 2108591
