# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_K16
_database_code_depnum_ccdc_archive 'CCDC 2365897'
loop_
_audit_author_name
_audit_author_address
'P. K. Sudhadevi Antharjanam'
;Sophisticated Analytical Instrument Facility, Indian Institute of Technology Madras, Chennai
India
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C27 H19 Cu2 N6 O3) + 2(N O3) + 5H2O'
_chemical_formula_sum            'C54 H48 Cu4 N14 O17'
_chemical_formula_weight         1419.22

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   19.498(4)
_cell_length_b                   17.355(3)
_cell_length_c                   33.032(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11178(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9811
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      16.72

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_F_000             5776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.589
_shelx_estimated_absorpt_T_min   0.797
_shelx_estimated_absorpt_T_max   0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed tube'
_diffrn_measurement_device_type  'Bruker axs kappa apex3 CMOS diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            127361
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_av_R_equivalents  0.2314
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.850
_diffrn_reflns_theta_max         20.857
_diffrn_reflns_theta_full        20.857
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5864
_reflns_number_gt                4227
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX3(Bruker, 2016)'
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+338.2379P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5864
_refine_ls_number_parameters     917
_refine_ls_number_restraints     1030
_refine_ls_R_factor_all          0.1696
_refine_ls_R_factor_gt           0.1230
_refine_ls_wR_factor_ref         0.2259
_refine_ls_wR_factor_gt          0.2043
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.42909(11) 0.52764(13) 0.18355(6) 0.0449(7) Uani 1 1 d . U . . .
Cu2 Cu 0.36051(12) 0.54548(13) 0.32194(7) 0.0491(7) Uani 1 1 d D U . . .
C1 C 0.4928(11) 0.5981(11) 0.1105(5) 0.055(6) Uani 1 1 d . U . . .
H1 H 0.534354 0.580833 0.120872 0.066 Uiso 1 1 calc R U . . .
C2 C 0.4933(11) 0.6413(12) 0.0748(6) 0.070(6) Uani 1 1 d . U . . .
H2 H 0.534794 0.652015 0.062182 0.084 Uiso 1 1 calc R U . . .
C3 C 0.4340(11) 0.6679(12) 0.0584(6) 0.063(6) Uani 1 1 d . U . . .
H3 H 0.434216 0.698858 0.035432 0.076 Uiso 1 1 calc R U . . .
C4 C 0.3717(10) 0.6467(11) 0.0775(5) 0.050(5) Uani 1 1 d . U . . .
C5 C 0.3743(10) 0.6055(10) 0.1131(5) 0.042(5) Uani 1 1 d . U . . .
C6 C 0.3128(9) 0.5815(10) 0.1331(5) 0.036(4) Uani 1 1 d . U . . .
C7 C 0.2489(10) 0.6023(11) 0.1160(5) 0.049(5) Uani 1 1 d . U . . .
C8 C 0.2479(12) 0.6487(12) 0.0801(6) 0.060(6) Uani 1 1 d . U . . .
H8 H 0.206016 0.665431 0.069852 0.072 Uiso 1 1 calc R U . . .
C9 C 0.3048(10) 0.6683(11) 0.0615(6) 0.052(5) Uani 1 1 d . U . . .
H9 H 0.302353 0.696497 0.037616 0.063 Uiso 1 1 calc R U . . .
C10 C 0.1924(11) 0.5754(12) 0.1362(6) 0.065(6) Uani 1 1 d . U . . .
H10 H 0.149289 0.588883 0.126505 0.078 Uiso 1 1 calc R U . . .
C11 C 0.1962(11) 0.5302(13) 0.1697(6) 0.071(6) Uani 1 1 d . U . . .
H11 H 0.156787 0.511813 0.182277 0.085 Uiso 1 1 calc R U . . .
C12 C 0.2628(10) 0.5119(12) 0.1850(6) 0.059(6) Uani 1 1 d . U . . .
H12 H 0.267142 0.481764 0.208118 0.071 Uiso 1 1 calc R U . . .
C13 C 0.4656(8) 0.3662(10) 0.1821(5) 0.038(4) Uani 1 1 d . U . . .
C14 C 0.4906(10) 0.3004(11) 0.1626(6) 0.051(5) Uani 1 1 d . U . . .
H14 H 0.514908 0.308008 0.138698 0.061 Uiso 1 1 calc R U . . .
C15 C 0.4829(10) 0.2276(12) 0.1750(6) 0.058(6) Uani 1 1 d . U . . .
H15 H 0.501929 0.187006 0.160457 0.070 Uiso 1 1 calc R U . . .
C16 C 0.4458(10) 0.2138(12) 0.2103(6) 0.061(6) Uani 1 1 d . U . . .
H16 H 0.437012 0.163697 0.218811 0.073 Uiso 1 1 calc R U . . .
C17 C 0.4221(10) 0.2763(11) 0.2326(6) 0.056(6) Uani 1 1 d . U . . .
H17 H 0.400186 0.267392 0.257213 0.067 Uiso 1 1 calc R U . . .
C18 C 0.4303(9) 0.3534(10) 0.2189(5) 0.038(4) Uani 1 1 d . U . . .
C19 C 0.4080(9) 0.4138(10) 0.2473(6) 0.042(5) Uani 1 1 d . U . . .
H19 H 0.391719 0.400579 0.272786 0.050 Uiso 1 1 calc R U . . .
C20 C 0.4091(9) 0.6129(10) 0.2494(6) 0.037(4) Uani 1 1 d . U . . .
C21 C 0.3587(9) 0.7107(11) 0.3377(6) 0.050(5) Uani 1 1 d . U . . .
H21 H 0.366458 0.760831 0.328825 0.060 Uiso 1 1 calc R U . . .
C22 C 0.3332(9) 0.6996(11) 0.3781(5) 0.045(5) Uani 1 1 d . U . . .
C23 C 0.3203(10) 0.7659(12) 0.4016(6) 0.058(6) Uani 1 1 d . U . . .
H23 H 0.327761 0.814266 0.390264 0.069 Uiso 1 1 calc R U . . .
C24 C 0.2968(11) 0.7607(13) 0.4409(7) 0.069(6) Uani 1 1 d . U . . .
H24 H 0.288164 0.804845 0.456024 0.083 Uiso 1 1 calc R U . . .
C25 C 0.2863(10) 0.6878(13) 0.4573(6) 0.060(6) Uani 1 1 d . U . . .
H25 H 0.272294 0.683725 0.484131 0.072 Uiso 1 1 calc R U . . .
C26 C 0.2959(9) 0.6208(11) 0.4349(6) 0.050(5) Uani 1 1 d . U . . .
H26 H 0.286662 0.572586 0.445917 0.060 Uiso 1 1 calc R U . . .
C27 C 0.3205(9) 0.6288(11) 0.3947(6) 0.045(5) Uani 1 1 d . U . . .
N1 N 0.4356(8) 0.5807(9) 0.1303(5) 0.055(4) Uani 1 1 d . U . . .
N2 N 0.3199(8) 0.5385(8) 0.1659(4) 0.044(4) Uani 1 1 d . U . . .
N3 N 0.3715(7) 0.6541(8) 0.3129(4) 0.045(4) Uani 1 1 d . U . . .
N4 N 0.3959(7) 0.6734(8) 0.2749(4) 0.048(3) Uani 1 1 d D U . . .
H4 H 0.402300 0.720510 0.267686 0.057 Uiso 1 1 calc DR U . . .
N5 N 0.3958(7) 0.5432(8) 0.2658(4) 0.041(4) Uani 1 1 d . U . . .
N6 N 0.4113(7) 0.4891(9) 0.2360(4) 0.040(4) Uani 1 1 d . U . . .
O1 O 0.4744(6) 0.4361(7) 0.1669(3) 0.043(3) Uani 1 1 d . U . . .
O2 O 0.4294(6) 0.6268(7) 0.2148(4) 0.050(3) Uani 1 1 d . U . . .
O3 O 0.3247(7) 0.5611(7) 0.3739(4) 0.064(4) Uani 1 1 d . U . . .
O4 O 0.3932(8) 0.4448(7) 0.3426(4) 0.061(4) Uani 1 1 d D U . . .
H4A H 0.423(5) 0.409(5) 0.341(4) 0.066(13) Uiso 1 1 d D U . . .
H4B H 0.354(2) 0.424(7) 0.344(10) 0.4(3) Uiso 1 1 d D . . . .
Cu3 Cu 0.12287(12) 0.57309(13) 0.39384(6) 0.0480(7) Uani 1 1 d D U . . .
Cu4 Cu 0.10088(11) 0.57369(14) 0.53765(6) 0.0448(7) Uani 1 1 d . U . . .
C28 C 0.2656(11) 0.5370(11) 0.5347(6) 0.056(5) Uani 1 1 d . U . . .
H28 H 0.257892 0.506412 0.512045 0.067 Uiso 1 1 calc R U . . .
C29 C 0.3335(11) 0.5481(12) 0.5478(7) 0.068(6) Uani 1 1 d . U . . .
H29 H 0.369860 0.525568 0.533955 0.082 Uiso 1 1 calc R U . . .
C30 C 0.3451(12) 0.5917(12) 0.5807(7) 0.067(6) Uani 1 1 d . U . . .
H30 H 0.389872 0.599957 0.589440 0.081 Uiso 1 1 calc R U . . .
C31 C 0.2928(12) 0.6233(12) 0.6010(6) 0.060(6) Uani 1 1 d . U . . .
C32 C 0.3000(13) 0.6709(13) 0.6364(7) 0.077(7) Uani 1 1 d . U . . .
H32 H 0.343629 0.682244 0.646036 0.093 Uiso 1 1 calc R U . . .
C33 C 0.2467(13) 0.6985(13) 0.6553(7) 0.073(7) Uani 1 1 d . U . . .
H33 H 0.253705 0.725940 0.679135 0.088 Uiso 1 1 calc R U . . .
C34 C 0.1792(12) 0.6889(12) 0.6415(7) 0.065(6) Uani 1 1 d . U . . .
C35 C 0.1678(11) 0.6431(11) 0.6065(6) 0.054(6) Uani 1 1 d . U . . .
C36 C 0.2259(9) 0.6123(10) 0.5860(5) 0.035(5) Uani 1 1 d . U . . .
C37 C 0.1185(15) 0.7146(14) 0.6597(7) 0.087(8) Uani 1 1 d . U . . .
H37 H 0.122899 0.742262 0.683710 0.104 Uiso 1 1 calc R U . . .
C38 C 0.0574(12) 0.7035(12) 0.6464(6) 0.067(6) Uani 1 1 d . U . . .
H38 H 0.019285 0.722282 0.660184 0.081 Uiso 1 1 calc R U . . .
C39 C 0.0504(12) 0.6616(13) 0.6099(6) 0.075(7) Uani 1 1 d . U . . .
H39 H 0.006718 0.654485 0.599176 0.090 Uiso 1 1 calc R U . . .
C40 C 0.1771(9) 0.7123(10) 0.3339(5) 0.040(5) Uani 1 1 d . U . . .
C41 C 0.2094(10) 0.7702(13) 0.3114(6) 0.066(6) Uani 1 1 d . U . . .
H41 H 0.213997 0.819355 0.322316 0.079 Uiso 1 1 calc R U . . .
C42 C 0.2344(10) 0.7551(12) 0.2734(6) 0.053(5) Uani 1 1 d . U . . .
H42 H 0.257998 0.792514 0.258830 0.063 Uiso 1 1 calc R U . . .
C43 C 0.2234(11) 0.6831(13) 0.2575(7) 0.073(7) Uani 1 1 d . U . . .
H43 H 0.238313 0.673071 0.231293 0.088 Uiso 1 1 calc R U . . .
C44 C 0.1914(11) 0.6253(13) 0.2786(6) 0.070(6) Uani 1 1 d . U . . .
H44 H 0.186844 0.576812 0.266906 0.084 Uiso 1 1 calc R U . . .
C45 C 0.1650(10) 0.6389(11) 0.3180(5) 0.049(5) Uani 1 1 d D U . . .
C46 C 0.1601(8) 0.7301(10) 0.3746(6) 0.040(5) Uani 1 1 d . U . . .
H46 H 0.166378 0.780810 0.382960 0.048 Uiso 1 1 calc R U . . .
C47 C 0.1152(9) 0.6521(11) 0.4675(6) 0.041(5) Uani 1 1 d . U . . .
C48 C 0.0888(8) 0.4546(10) 0.4755(5) 0.035(4) Uani 1 1 d . U . . .
H48 H 0.090575 0.439444 0.448490 0.042 Uiso 1 1 calc R U . . .
C49 C 0.0758(8) 0.3972(10) 0.5059(5) 0.038(4) Uani 1 1 d . U . . .
C50 C 0.0703(9) 0.3214(11) 0.4921(6) 0.049(5) Uani 1 1 d . U . . .
H50 H 0.075782 0.311463 0.464602 0.059 Uiso 1 1 calc R U . . .
C51 C 0.0570(9) 0.2610(12) 0.5178(6) 0.057(6) Uani 1 1 d . U . . .
H51 H 0.054613 0.210678 0.508248 0.068 Uiso 1 1 calc R U . . .
C52 C 0.0473(10) 0.2777(13) 0.5579(6) 0.059(6) Uani 1 1 d . U . . .
H52 H 0.039304 0.237808 0.576122 0.071 Uiso 1 1 calc R U . . .
C53 C 0.0493(10) 0.3514(12) 0.5715(6) 0.058(6) Uani 1 1 d . U . . .
H53 H 0.040954 0.359902 0.598900 0.070 Uiso 1 1 calc R U . . .
C54 C 0.0630(9) 0.4150(11) 0.5473(6) 0.045(5) Uani 1 1 d . U . . .
N7 N 0.1046(9) 0.6314(9) 0.5900(4) 0.050(4) Uani 1 1 d . U . . .
N8 N 0.2132(8) 0.5674(9) 0.5528(4) 0.054(4) Uani 1 1 d . U . . .
N9 N 0.0982(7) 0.5273(8) 0.4842(4) 0.035(3) Uani 1 1 d . U . . .
N10 N 0.1110(7) 0.5805(9) 0.4530(4) 0.038(4) Uani 1 1 d . U . . .
N11 N 0.1251(7) 0.7078(8) 0.4410(4) 0.038(4) Uani 1 1 d D U . . .
N12 N 0.1372(7) 0.6831(8) 0.4007(4) 0.039(4) Uani 1 1 d . U . . .
O5 O 0.0641(6) 0.4846(7) 0.5624(3) 0.043(3) Uani 1 1 d . U . . .
O6 O 0.1095(6) 0.6688(7) 0.5049(3) 0.044(3) Uani 1 1 d . U . . .
O7 O 0.1235(19) 0.5876(15) 0.3367(7) 0.033(4) Uani 0.55(5) 1 d D U P A 1
O7' O 0.153(3) 0.5756(13) 0.3403(8) 0.033(4) Uani 0.45(5) 1 d D U P A 2
O8 O 0.1938(8) 0.4764(9) 0.3931(5) 0.090(5) Uani 1 1 d D U . . .
O9 O 0.0401(7) 0.5013(9) 0.3845(4) 0.078(4) Uani 1 1 d D U . . .
H8A H 0.224(6) 0.471(7) 0.412(3) 0.092(11) Uiso 1 1 d D U . . .
H8B H 0.209(7) 0.448(7) 0.3734(16) 0.093(11) Uiso 1 1 d D U . . .
H9A H 0.030(4) 0.456(4) 0.394(4) 0.078(11) Uiso 1 1 d D U . . .
H9B H 0.002(3) 0.519(3) 0.374(5) 0.078(11) Uiso 1 1 d D U . . .
H11A H 0.147(6) 0.752(4) 0.446(4) 0.037(7) Uiso 1 1 d D U . . .
N14 N 0.1221(17) 0.8961(14) 0.4408(10) 0.18(2) Uani 0.53(4) 1 d D U P B 3
O13 O 0.1384(19) 0.863(2) 0.4742(9) 0.130(17) Uani 0.53(4) 1 d D U P B 3
O14 O 0.0609(19) 0.924(3) 0.4353(15) 0.21(2) Uani 0.53(4) 1 d D U P B 3
O15 O 0.168(2) 0.902(3) 0.4116(11) 0.189(19) Uani 0.53(4) 1 d D U P B 3
N14' N 0.133(3) 0.916(2) 0.4519(12) 0.26(3) Uani 0.47(4) 1 d D U P B 4
O13' O 0.107(3) 0.865(4) 0.427(2) 0.26(3) Uani 0.47(4) 1 d D U P B 4
O14' O 0.092(3) 0.966(3) 0.469(2) 0.26(3) Uani 0.47(4) 1 d D U P B 4
O15' O 0.199(3) 0.918(4) 0.459(2) 0.26(3) Uani 0.47(4) 1 d D U P B 4
O16 O 0.0088(12) 0.5123(15) 0.3035(7) 0.178(10) Uani 1 1 d . U . . .
O10 O 0.2532(14) 0.4605(15) 0.2973(7) 0.113(7) Uani 0.691(14) 1 d D U P C 5
O11 O 0.1581(12) 0.4025(13) 0.3191(7) 0.117(7) Uani 0.691(14) 1 d D U P C 5
O12 O 0.1679(13) 0.4321(15) 0.2542(8) 0.122(7) Uani 0.691(14) 1 d D U P C 5
N13 N 0.1940(10) 0.4322(8) 0.2902(6) 0.117(7) Uani 0.691(14) 1 d D U P C 5
O17 O 0.0683(19) 0.3307(17) 0.2656(10) 0.118(7) Uani 0.691(14) 1 d . U P C 5
O10' O 0.173(3) 0.384(3) 0.255(2) 0.123(8) Uani 0.309(14) 1 d D U P C 6
O11' O 0.077(3) 0.449(3) 0.2457(18) 0.122(8) Uani 0.309(14) 1 d D U P C 6
O12' O 0.073(4) 0.321(3) 0.253(2) 0.118(8) Uani 0.309(14) 1 d D U P C 6
N13' N 0.108(2) 0.384(2) 0.2514(10) 0.118(7) Uani 0.309(14) 1 d D U P C 6
O17' O 0.276(2) 0.480(3) 0.317(2) 0.117(18) Uani 0.309(14) 1 d D U P C 6


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N6 1.890(13) . ?
Cu1 O1 1.899(11) . ?
Cu1 N1 1.989(15) . ?
Cu1 O2 2.007(12) . ?
Cu1 N2 2.216(15) . ?
Cu2 O3 1.871(12) . ?
Cu2 N3 1.920(14) . ?
Cu2 N5 1.979(13) . ?
Cu2 O4 1.981(12) . ?
Cu2 O17' 2.02(2) . ?
C1 N1 1.33(2) . ?
C1 C2 1.40(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.36(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.42(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(2) . ?
C4 C9 1.46(2) . ?
C5 N1 1.39(2) . ?
C5 C6 1.43(2) . ?
C6 N2 1.32(2) . ?
C6 C7 1.41(2) . ?
C7 C10 1.37(3) . ?
C7 C8 1.43(3) . ?
C8 C9 1.31(2) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.36(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.43(3) . ?
C11 H11 0.9300 . ?
C12 N2 1.36(2) . ?
C12 H12 0.9300 . ?
C13 O1 1.323(19) . ?
C13 C14 1.40(2) . ?
C13 C18 1.42(2) . ?
C14 C15 1.34(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.39(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.39(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.42(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.47(2) . ?
C19 N6 1.36(2) . ?
C19 H19 0.9300 . ?
C20 O2 1.234(19) . ?
C20 N5 1.35(2) . ?
C20 N4 1.37(2) . ?
C21 N3 1.30(2) . ?
C21 C22 1.44(2) . ?
C21 H21 0.9300 . ?
C22 C27 1.37(2) . ?
C22 C23 1.41(2) . ?
C23 C24 1.38(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.39(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.39(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.42(2) . ?
C26 H26 0.9300 . ?
C27 O3 1.36(2) . ?
N3 N4 1.385(18) . ?
N4 H4 0.8600 . ?
N5 N6 1.391(17) . ?
O4 H4A 0.86(2) . ?
O4 H4B 0.85(2) . ?
Cu3 O7' 1.86(3) . ?
Cu3 O7 1.90(2) . ?
Cu3 N12 1.942(15) . ?
Cu3 N10 1.973(12) . ?
Cu3 O9 2.062(14) . ?
Cu3 O8 2.174(15) . ?
Cu4 O5 1.891(11) . ?
Cu4 N9 1.942(13) . ?
Cu4 O6 1.980(12) . ?
Cu4 N7 2.000(14) . ?
Cu4 N8 2.249(17) . ?
C28 N8 1.30(2) . ?
C28 C29 1.41(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.34(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.34(3) . ?
C30 H30 0.9300 . ?
C31 C36 1.41(2) . ?
C31 C32 1.44(3) . ?
C32 C33 1.30(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.40(3) . ?
C33 H33 0.9300 . ?
C34 C37 1.40(3) . ?
C34 C35 1.42(3) . ?
C35 N7 1.36(2) . ?
C35 C36 1.42(2) . ?
C36 N8 1.37(2) . ?
C37 C38 1.29(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.42(3) . ?
C38 H38 0.9300 . ?
C39 N7 1.35(2) . ?
C39 H39 0.9300 . ?
C40 C45 1.40(2) . ?
C40 C41 1.40(3) . ?
C40 C46 1.42(2) . ?
C41 C42 1.37(2) . ?
C41 H41 0.9300 . ?
C42 C43 1.37(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.37(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.42(3) . ?
C44 H44 0.9300 . ?
C45 O7' 1.34(2) . ?
C45 O7 1.35(2) . ?
C46 N12 1.27(2) . ?
C46 H46 0.9300 . ?
C47 O6 1.27(2) . ?
C47 N11 1.32(2) . ?
C47 N10 1.33(2) . ?
C48 N9 1.306(19) . ?
C48 C49 1.44(2) . ?
C48 H48 0.9300 . ?
C49 C50 1.40(2) . ?
C49 C54 1.42(2) . ?
C50 C51 1.37(2) . ?
C50 H50 0.9300 . ?
C51 C52 1.37(3) . ?
C51 H51 0.9300 . ?
C52 C53 1.36(3) . ?
C52 H52 0.9300 . ?
C53 C54 1.39(2) . ?
C53 H53 0.9300 . ?
C54 O5 1.31(2) . ?
N9 N10 1.405(17) . ?
N11 N12 1.417(18) . ?
N11 H11A 0.90(2) . ?
O8 H8A 0.87(2) . ?
O8 H8B 0.87(2) . ?
O9 H9A 0.864(19) . ?
O9 H9B 0.87(2) . ?
N14 O13 1.28(2) . ?
N14 O14 1.30(2) . ?
N14 O15 1.32(2) . ?
N14' O13' 1.30(2) . ?
N14' O14' 1.30(2) . ?
N14' O15' 1.31(2) . ?
O10 N13 1.28(2) . ?
O11 N13 1.29(2) . ?
O12 N13 1.29(2) . ?
O10' N13' 1.29(2) . ?
O11' N13' 1.29(2) . ?
O12' N13' 1.29(2) . ?

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
N6 Cu1 O1 93.2(5) . . ?
N6 Cu1 N1 170.5(6) . . ?
O1 Cu1 N1 95.8(6) . . ?
N6 Cu1 O2 80.3(6) . . ?
O1 Cu1 O2 149.9(5) . . ?
N1 Cu1 O2 93.3(6) . . ?
N6 Cu1 N2 95.5(5) . . ?
O1 Cu1 N2 116.2(5) . . ?
N1 Cu1 N2 77.8(6) . . ?
O2 Cu1 N2 93.7(5) . . ?
O3 Cu2 N3 92.4(6) . . ?
O3 Cu2 N5 172.6(6) . . ?
N3 Cu2 N5 80.6(6) . . ?
O3 Cu2 O4 86.1(5) . . ?
N3 Cu2 O4 152.0(6) . . ?
N5 Cu2 O4 101.1(5) . . ?
O3 Cu2 O17' 82(2) . . ?
N3 Cu2 O17' 129(2) . . ?
N5 Cu2 O17' 101(2) . . ?
O4 Cu2 O17' 78(2) . . ?
N1 C1 C2 123(2) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 121(2) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C2 C3 C4 117.6(18) . . ?
C2 C3 H3 121.2 . . ?
C4 C3 H3 121.2 . . ?
C5 C4 C3 118.9(18) . . ?
C5 C4 C9 118.4(18) . . ?
C3 C4 C9 122.7(17) . . ?
C4 C5 N1 122.8(18) . . ?
C4 C5 C6 120.9(18) . . ?
N1 C5 C6 116.2(15) . . ?
N2 C6 C7 124.3(17) . . ?
N2 C6 C5 116.9(15) . . ?
C7 C6 C5 118.7(16) . . ?
C10 C7 C6 115.2(18) . . ?
C10 C7 C8 126(2) . . ?
C6 C7 C8 119.1(19) . . ?
C9 C8 C7 121(2) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C4 121.4(18) . . ?
C8 C9 H9 119.3 . . ?
C4 C9 H9 119.3 . . ?
C11 C10 C7 123(2) . . ?
C11 C10 H10 118.3 . . ?
C7 C10 H10 118.3 . . ?
C10 C11 C12 118(2) . . ?
C10 C11 H11 121.1 . . ?
C12 C11 H11 121.1 . . ?
N2 C12 C11 120.3(18) . . ?
N2 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
O1 C13 C14 122.0(17) . . ?
O1 C13 C18 122.2(15) . . ?
C14 C13 C18 115.9(17) . . ?
C15 C14 C13 126.3(19) . . ?
C15 C14 H14 116.9 . . ?
C13 C14 H14 116.9 . . ?
C14 C15 C16 119(2) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
C17 C16 C15 119(2) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C16 C17 C18 121.8(19) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 H17 119.1 . . ?
C13 C18 C17 118.5(16) . . ?
C13 C18 C19 125.3(16) . . ?
C17 C18 C19 115.8(16) . . ?
N6 C19 C18 119.8(16) . . ?
N6 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
O2 C20 N5 127.5(16) . . ?
O2 C20 N4 118.6(16) . . ?
N5 C20 N4 113.9(16) . . ?
N3 C21 C22 123.2(18) . . ?
N3 C21 H21 118.4 . . ?
C22 C21 H21 118.4 . . ?
C27 C22 C23 118.8(17) . . ?
C27 C22 C21 123.7(17) . . ?
C23 C22 C21 117.5(18) . . ?
C24 C23 C22 122(2) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C25 118(2) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
C26 C25 C24 122(2) . . ?
C26 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C25 C26 C27 117.5(19) . . ?
C25 C26 H26 121.3 . . ?
C27 C26 H26 121.3 . . ?
O3 C27 C22 124.2(17) . . ?
O3 C27 C26 114.0(17) . . ?
C22 C27 C26 121.6(17) . . ?
C1 N1 C5 116.7(16) . . ?
C1 N1 Cu1 126.5(14) . . ?
C5 N1 Cu1 116.7(12) . . ?
C6 N2 C12 119.0(16) . . ?
C6 N2 Cu1 111.4(11) . . ?
C12 N2 Cu1 129.4(12) . . ?
C21 N3 N4 116.9(15) . . ?
C21 N3 Cu2 128.4(13) . . ?
N4 N3 Cu2 114.6(11) . . ?
C20 N4 N3 115.8(14) . . ?
C20 N4 H4 122.1 . . ?
N3 N4 H4 122.1 . . ?
C20 N5 N6 106.2(13) . . ?
C20 N5 Cu2 115.1(11) . . ?
N6 N5 Cu2 138.7(11) . . ?
C19 N6 N5 116.4(13) . . ?
C19 N6 Cu1 126.8(12) . . ?
N5 N6 Cu1 116.7(10) . . ?
C13 O1 Cu1 126.6(10) . . ?
C20 O2 Cu1 107.9(11) . . ?
C27 O3 Cu2 127.5(12) . . ?
Cu2 O4 H4A 147(5) . . ?
Cu2 O4 H4B 95(2) . . ?
H4A O4 H4B 108(4) . . ?
O7' Cu3 N12 92.4(8) . . ?
O7 Cu3 N12 89.1(8) . . ?
O7' Cu3 N10 167.5(14) . . ?
O7 Cu3 N10 167.0(12) . . ?
N12 Cu3 N10 80.6(6) . . ?
O7' Cu3 O9 96.6(12) . . ?
O7 Cu3 O9 86.4(8) . . ?
N12 Cu3 O9 136.4(6) . . ?
N10 Cu3 O9 95.5(6) . . ?
O7' Cu3 O8 79.0(13) . . ?
O7 Cu3 O8 95.0(12) . . ?
N12 Cu3 O8 131.9(6) . . ?
N10 Cu3 O8 97.8(6) . . ?
O9 Cu3 O8 91.7(6) . . ?
O5 Cu4 N9 92.5(5) . . ?
O5 Cu4 O6 161.8(5) . . ?
N9 Cu4 O6 81.5(5) . . ?
O5 Cu4 N7 92.8(5) . . ?
N9 Cu4 N7 174.4(6) . . ?
O6 Cu4 N7 93.0(5) . . ?
O5 Cu4 N8 103.5(5) . . ?
N9 Cu4 N8 102.0(6) . . ?
O6 Cu4 N8 94.6(5) . . ?
N7 Cu4 N8 78.2(6) . . ?
N8 C28 C29 123(2) . . ?
N8 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C30 C29 C28 119(2) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
C31 C30 C29 121(2) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C36 118(2) . . ?
C30 C31 C32 125(2) . . ?
C36 C31 C32 117(2) . . ?
C33 C32 C31 122(2) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C32 C33 C34 123(2) . . ?
C32 C33 H33 118.4 . . ?
C34 C33 H33 118.4 . . ?
C37 C34 C33 128(2) . . ?
C37 C34 C35 113(2) . . ?
C33 C34 C35 119(2) . . ?
N7 C35 C34 123(2) . . ?
N7 C35 C36 118.3(17) . . ?
C34 C35 C36 118.1(19) . . ?
N8 C36 C31 121.8(18) . . ?
N8 C36 C35 116.8(16) . . ?
C31 C36 C35 121.3(18) . . ?
C38 C37 C34 126(2) . . ?
C38 C37 H37 117.0 . . ?
C34 C37 H37 117.0 . . ?
C37 C38 C39 117(2) . . ?
C37 C38 H38 121.4 . . ?
C39 C38 H38 121.4 . . ?
N7 C39 C38 123(2) . . ?
N7 C39 H39 118.7 . . ?
C38 C39 H39 118.7 . . ?
C45 C40 C41 122.0(18) . . ?
C45 C40 C46 121.1(16) . . ?
C41 C40 C46 116.9(17) . . ?
C42 C41 C40 121(2) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C43 C42 C41 118(2) . . ?
C43 C42 H42 121.0 . . ?
C41 C42 H42 121.0 . . ?
C44 C43 C42 123(2) . . ?
C44 C43 H43 118.5 . . ?
C42 C43 H43 118.5 . . ?
C43 C44 C45 121(2) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
O7' C45 C40 124.6(19) . . ?
O7 C45 C40 121.9(18) . . ?
O7' C45 C44 116(2) . . ?
O7 C45 C44 122(2) . . ?
C40 C45 C44 115.8(18) . . ?
N12 C46 C40 125.8(17) . . ?
N12 C46 H46 117.1 . . ?
C40 C46 H46 117.1 . . ?
O6 C47 N11 119.4(17) . . ?
O6 C47 N10 123.6(16) . . ?
N11 C47 N10 117.0(17) . . ?
N9 C48 C49 122.7(15) . . ?
N9 C48 H48 118.6 . . ?
C49 C48 H48 118.6 . . ?
C50 C49 C54 120.3(17) . . ?
C50 C49 C48 116.0(16) . . ?
C54 C49 C48 123.4(16) . . ?
C51 C50 C49 122.1(18) . . ?
C51 C50 H50 118.9 . . ?
C49 C50 H50 118.9 . . ?
C52 C51 C50 118(2) . . ?
C52 C51 H51 121.2 . . ?
C50 C51 H51 121.2 . . ?
C53 C52 C51 121(2) . . ?
C53 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?
C52 C53 C54 124(2) . . ?
C52 C53 H53 117.9 . . ?
C54 C53 H53 117.9 . . ?
O5 C54 C53 121.1(17) . . ?
O5 C54 C49 124.4(17) . . ?
C53 C54 C49 114.5(17) . . ?
C39 N7 C35 117.2(17) . . ?
C39 N7 Cu4 125.9(15) . . ?
C35 N7 Cu4 116.9(13) . . ?
C28 N8 C36 117.4(17) . . ?
C28 N8 Cu4 133.1(13) . . ?
C36 N8 Cu4 109.1(12) . . ?
C48 N9 N10 119.9(13) . . ?
C48 N9 Cu4 127.2(11) . . ?
N10 N9 Cu4 112.8(10) . . ?
C47 N10 N9 111.2(13) . . ?
C47 N10 Cu3 114.1(12) . . ?
N9 N10 Cu3 134.7(11) . . ?
C47 N11 N12 115.3(14) . . ?
C47 N11 H11A 125(10) . . ?
N12 N11 H11A 111(10) . . ?
C46 N12 N11 120.1(15) . . ?
C46 N12 Cu3 127.2(12) . . ?
N11 N12 Cu3 112.5(10) . . ?
C54 O5 Cu4 126.6(11) . . ?
C47 O6 Cu4 110.4(11) . . ?
C45 O7 Cu3 123.0(19) . . ?
C45 O7' Cu3 127(2) . . ?
Cu3 O8 H8A 120(3) . . ?
Cu3 O8 H8B 132(3) . . ?
H8A O8 H8B 105(3) . . ?
Cu3 O9 H9A 132(3) . . ?
Cu3 O9 H9B 121(3) . . ?
H9A O9 H9B 106(3) . . ?
O13 N14 O14 120.8(17) . . ?
O13 N14 O15 119.5(17) . . ?
O14 N14 O15 119.7(17) . . ?
O13' N14' O14' 119.4(17) . . ?
O13' N14' O15' 120.2(17) . . ?
O14' N14' O15' 120.4(17) . . ?
O10 N13 O11 120.4(14) . . ?
O10 N13 O12 121.7(14) . . ?
O11 N13 O12 117.8(14) . . ?
O10' N13' O12' 120.6(17) . . ?
O10' N13' O11' 119.4(17) . . ?
O12' N13' O11' 120.0(17) . . ?

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
N1 C1 C2 C3 0(3) . . . . ?
C1 C2 C3 C4 -3(3) . . . . ?
C2 C3 C4 C5 5(3) . . . . ?
C2 C3 C4 C9 -177(2) . . . . ?
C3 C4 C5 N1 -3(3) . . . . ?
C9 C4 C5 N1 178.5(17) . . . . ?
C3 C4 C5 C6 -178.7(17) . . . . ?
C9 C4 C5 C6 3(3) . . . . ?
C4 C5 C6 N2 176.2(16) . . . . ?
N1 C5 C6 N2 0(2) . . . . ?
C4 C5 C6 C7 -1(3) . . . . ?
N1 C5 C6 C7 -177.4(16) . . . . ?
N2 C6 C7 C10 1(3) . . . . ?
C5 C6 C7 C10 178.4(17) . . . . ?
N2 C6 C7 C8 -179.6(17) . . . . ?
C5 C6 C7 C8 -2(3) . . . . ?
C10 C7 C8 C9 -176(2) . . . . ?
C6 C7 C8 C9 4(3) . . . . ?
C7 C8 C9 C4 -3(3) . . . . ?
C5 C4 C9 C8 -1(3) . . . . ?
C3 C4 C9 C8 -179(2) . . . . ?
C6 C7 C10 C11 -2(3) . . . . ?
C8 C7 C10 C11 178.7(19) . . . . ?
C7 C10 C11 C12 2(3) . . . . ?
C10 C11 C12 N2 -1(3) . . . . ?
O1 C13 C14 C15 -178.4(18) . . . . ?
C18 C13 C14 C15 2(3) . . . . ?
C13 C14 C15 C16 1(3) . . . . ?
C14 C15 C16 C17 -4(3) . . . . ?
C15 C16 C17 C18 5(3) . . . . ?
O1 C13 C18 C17 178.9(16) . . . . ?
C14 C13 C18 C17 -1(2) . . . . ?
O1 C13 C18 C19 -9(3) . . . . ?
C14 C13 C18 C19 171.2(16) . . . . ?
C16 C17 C18 C13 -2(3) . . . . ?
C16 C17 C18 C19 -175.0(17) . . . . ?
C13 C18 C19 N6 10(3) . . . . ?
C17 C18 C19 N6 -177.2(16) . . . . ?
N3 C21 C22 C27 1(3) . . . . ?
N3 C21 C22 C23 -178.8(17) . . . . ?
C27 C22 C23 C24 2(3) . . . . ?
C21 C22 C23 C24 -179.0(18) . . . . ?
C22 C23 C24 C25 0(3) . . . . ?
C23 C24 C25 C26 -3(3) . . . . ?
C24 C25 C26 C27 3(3) . . . . ?
C23 C22 C27 O3 173.5(17) . . . . ?
C21 C22 C27 O3 -6(3) . . . . ?
C23 C22 C27 C26 -1(3) . . . . ?
C21 C22 C27 C26 179.4(17) . . . . ?
C25 C26 C27 O3 -176.2(16) . . . . ?
C25 C26 C27 C22 -1(3) . . . . ?
C2 C1 N1 C5 2(3) . . . . ?
C2 C1 N1 Cu1 -174.4(15) . . . . ?
C4 C5 N1 C1 0(3) . . . . ?
C6 C5 N1 C1 175.5(17) . . . . ?
C4 C5 N1 Cu1 176.4(14) . . . . ?
C6 C5 N1 Cu1 -8(2) . . . . ?
C7 C6 N2 C12 0(3) . . . . ?
C5 C6 N2 C12 -177.6(16) . . . . ?
C7 C6 N2 Cu1 -176.3(14) . . . . ?
C5 C6 N2 Cu1 6.3(19) . . . . ?
C11 C12 N2 C6 0(3) . . . . ?
C11 C12 N2 Cu1 175.5(14) . . . . ?
C22 C21 N3 N4 179.9(16) . . . . ?
C22 C21 N3 Cu2 0(3) . . . . ?
O2 C20 N4 N3 178.3(15) . . . . ?
N5 C20 N4 N3 0(2) . . . . ?
C21 N3 N4 C20 179.9(15) . . . . ?
Cu2 N3 N4 C20 -0.6(18) . . . . ?
O2 C20 N5 N6 2(2) . . . . ?
N4 C20 N5 N6 179.4(14) . . . . ?
O2 C20 N5 Cu2 -177.7(14) . . . . ?
N4 C20 N5 Cu2 0.2(19) . . . . ?
C18 C19 N6 N5 -173.8(14) . . . . ?
C18 C19 N6 Cu1 10(2) . . . . ?
C20 N5 N6 C19 173.8(14) . . . . ?
Cu2 N5 N6 C19 -7(2) . . . . ?
C20 N5 N6 Cu1 -9.9(16) . . . . ?
Cu2 N5 N6 Cu1 169.0(10) . . . . ?
O1 Cu1 N6 C19 -23.0(14) . . . . ?
O2 Cu1 N6 C19 -173.4(15) . . . . ?
N2 Cu1 N6 C19 93.7(14) . . . . ?
O1 Cu1 N6 N5 161.1(11) . . . . ?
O2 Cu1 N6 N5 10.8(11) . . . . ?
N2 Cu1 N6 N5 -82.1(11) . . . . ?
C14 C13 O1 Cu1 166.7(13) . . . . ?
C18 C13 O1 Cu1 -13(2) . . . . ?
N6 Cu1 O1 C13 24.7(14) . . . . ?
N1 Cu1 O1 C13 -152.2(13) . . . . ?
O2 Cu1 O1 C13 100.9(15) . . . . ?
N2 Cu1 O1 C13 -72.9(14) . . . . ?
N5 C20 O2 Cu1 7(2) . . . . ?
N4 C20 O2 Cu1 -171.2(12) . . . . ?
C22 C27 O3 Cu2 10(3) . . . . ?
C26 C27 O3 Cu2 -175.0(12) . . . . ?
N3 Cu2 O3 C27 -7.1(15) . . . . ?
O4 Cu2 O3 C27 144.9(15) . . . . ?
O17' Cu2 O3 C27 -137(2) . . . . ?
N8 C28 C29 C30 0(3) . . . . ?
C28 C29 C30 C31 1(3) . . . . ?
C29 C30 C31 C36 -3(3) . . . . ?
C29 C30 C31 C32 -180(2) . . . . ?
C30 C31 C32 C33 -178(2) . . . . ?
C36 C31 C32 C33 4(3) . . . . ?
C31 C32 C33 C34 -5(4) . . . . ?
C32 C33 C34 C37 179(2) . . . . ?
C32 C33 C34 C35 4(3) . . . . ?
C37 C34 C35 N7 6(3) . . . . ?
C33 C34 C35 N7 -178.5(19) . . . . ?
C37 C34 C35 C36 -178.5(19) . . . . ?
C33 C34 C35 C36 -3(3) . . . . ?
C30 C31 C36 N8 3(3) . . . . ?
C32 C31 C36 N8 -179.2(17) . . . . ?
C30 C31 C36 C35 178.8(18) . . . . ?
C32 C31 C36 C35 -4(3) . . . . ?
N7 C35 C36 N8 -5(3) . . . . ?
C34 C35 C36 N8 178.9(17) . . . . ?
N7 C35 C36 C31 179.0(17) . . . . ?
C34 C35 C36 C31 3(3) . . . . ?
C33 C34 C37 C38 -179(2) . . . . ?
C35 C34 C37 C38 -4(4) . . . . ?
C34 C37 C38 C39 0(4) . . . . ?
C37 C38 C39 N7 2(3) . . . . ?
C45 C40 C41 C42 -4(3) . . . . ?
C46 C40 C41 C42 172.7(17) . . . . ?
C40 C41 C42 C43 3(3) . . . . ?
C41 C42 C43 C44 -3(3) . . . . ?
C42 C43 C44 C45 3(3) . . . . ?
C41 C40 C45 O7' 161(3) . . . . ?
C46 C40 C45 O7' -16(4) . . . . ?
C41 C40 C45 O7 -168(3) . . . . ?
C46 C40 C45 O7 15(3) . . . . ?
C41 C40 C45 C44 4(3) . . . . ?
C46 C40 C45 C44 -172.9(17) . . . . ?
C43 C44 C45 O7' -162(3) . . . . ?
C43 C44 C45 O7 169(3) . . . . ?
C43 C44 C45 C40 -3(3) . . . . ?
C45 C40 C46 N12 4(3) . . . . ?
C41 C40 C46 N12 -172.5(17) . . . . ?
N9 C48 C49 C50 -176.8(16) . . . . ?
N9 C48 C49 C54 9(3) . . . . ?
C54 C49 C50 C51 -4(3) . . . . ?
C48 C49 C50 C51 -179.1(17) . . . . ?
C49 C50 C51 C52 2(3) . . . . ?
C50 C51 C52 C53 1(3) . . . . ?
C51 C52 C53 C54 -2(3) . . . . ?
C52 C53 C54 O5 180.0(18) . . . . ?
C52 C53 C54 C49 -1(3) . . . . ?
C50 C49 C54 O5 -176.9(16) . . . . ?
C48 C49 C54 O5 -3(3) . . . . ?
C50 C49 C54 C53 4(3) . . . . ?
C48 C49 C54 C53 177.9(16) . . . . ?
C38 C39 N7 C35 0(3) . . . . ?
C38 C39 N7 Cu4 -178.3(15) . . . . ?
C34 C35 N7 C39 -4(3) . . . . ?
C36 C35 N7 C39 -179.7(18) . . . . ?
C34 C35 N7 Cu4 174.1(15) . . . . ?
C36 C35 N7 Cu4 -1(2) . . . . ?
C29 C28 N8 C36 0(3) . . . . ?
C29 C28 N8 Cu4 172.3(14) . . . . ?
C31 C36 N8 C28 -2(3) . . . . ?
C35 C36 N8 C28 -177.8(17) . . . . ?
C31 C36 N8 Cu4 -176.1(14) . . . . ?
C35 C36 N8 Cu4 8.3(19) . . . . ?
C49 C48 N9 N10 179.7(14) . . . . ?
C49 C48 N9 Cu4 3(2) . . . . ?
O6 C47 N10 N9 1(2) . . . . ?
N11 C47 N10 N9 -178.1(14) . . . . ?
O6 C47 N10 Cu3 -179.4(13) . . . . ?
N11 C47 N10 Cu3 1(2) . . . . ?
C48 N9 N10 C47 176.2(15) . . . . ?
Cu4 N9 N10 C47 -6.3(16) . . . . ?
C48 N9 N10 Cu3 -3(2) . . . . ?
Cu4 N9 N10 Cu3 174.6(9) . . . . ?
O6 C47 N11 N12 174.2(14) . . . . ?
N10 C47 N11 N12 -6(2) . . . . ?
C40 C46 N12 N11 177.3(15) . . . . ?
C40 C46 N12 Cu3 3(3) . . . . ?
C47 N11 N12 C46 -166.5(16) . . . . ?
C47 N11 N12 Cu3 8.4(17) . . . . ?
C53 C54 O5 Cu4 164.9(13) . . . . ?
C49 C54 O5 Cu4 -14(2) . . . . ?
N9 Cu4 O5 C54 19.1(14) . . . . ?
O6 Cu4 O5 C54 89(2) . . . . ?
N7 Cu4 O5 C54 -162.5(14) . . . . ?
N8 Cu4 O5 C54 -83.9(14) . . . . ?
N11 C47 O6 Cu4 -176.5(13) . . . . ?
N10 C47 O6 Cu4 4(2) . . . . ?
C40 C45 O7 Cu3 -41(4) . . . . ?
C44 C45 O7 Cu3 148(2) . . . . ?
C40 C45 O7' Cu3 19(5) . . . . ?
C44 C45 O7' Cu3 176(3) . . . . ?
N12 Cu3 O7' C45 -10(4) . . . . ?
N10 Cu3 O7' C45 -66(8) . . . . ?
O9 Cu3 O7' C45 127(4) . . . . ?
O8 Cu3 O7' C45 -142(4) . . . . ?

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
C12 H12 O12^e 0.93 2.61 3.25(3) 126.7 . yes
C19 H19 O4 0.93 2.43 3.21(2) 141.1 . yes
C21 H21 O11^e 0.93 2.52 3.40(3) 156.9 8_665 yes
N4 H4 O17^e 0.86 2.00 2.83(4) 163.9 8_665 yes
N4 H4 O12'^f 0.86 1.88 2.73(6) 173.5 8_665 yes
O4 H4A O1 0.86(2) 2.07(10) 2.604(18) 120(9) 3_655 yes
O4 H4B O10^e 0.85(2) 2.56(15) 3.13(3) 124(14) . yes
O4 H4B O17'^f 0.85(2) 2.01(10) 2.52(6) 118(7) . yes
C28 H28 O15'^d 0.93 2.47 3.31(7) 150.0 8_655 yes
C29 H29 O14'^d 0.93 2.50 3.31(7) 145.7 8_655 yes
C44 H44 O10^e 0.93 2.60 3.17(3) 119.8 . yes
C44 H44 O12^e 0.93 2.57 3.48(4) 164.8 . yes
C44 H44 N13^e 0.93 2.63 3.37(3) 137.6 . yes
C46 H46 O15^c 0.93 2.30 3.22(5) 170.3 . yes
C46 H46 O13'^d 0.93 2.37 3.09(6) 134.5 . yes
C48 H48 O9 0.93 2.57 3.25(2) 131.0 . yes
O8 H8A O15^c 0.87(2) 2.43(7) 3.05(4) 129(6) 8_655 yes
O8 H8A O15'^d 0.87(2) 2.36(8) 3.20(7) 162(10) 8_655 yes
O8 H8B O11^e 0.87(2) 2.20(8) 2.85(3) 131(9) . yes
O8 H8B O17'^f 0.87(2) 2.35(14) 2.99(6) 131(14) . yes
N11 H11A N14^c 0.90(2) 2.55(10) 3.27(3) 138(12) . yes
N11 H11A O13^c 0.90(2) 2.15(9) 2.93(4) 145(12) . yes
N11 H11A O13'^d 0.90(2) 2.19(13) 2.78(7) 123(11) . yes
C12 H12 O12^e 0.93 2.61 3.25(3) 126.7 . yes
C19 H19 O4 0.93 2.43 3.21(2) 141.1 . yes
C21 H21 O11^e 0.93 2.52 3.40(3) 156.9 8_665 yes
N4 H4 O17^e 0.86 2.00 2.83(4) 163.9 8_665 yes
N4 H4 O12'^f 0.86 1.88 2.73(6) 173.5 8_665 yes
O4 H4A O1 0.86(2) 2.07(10) 2.604(18) 120(9) 3_655 yes
O4 H4B O10^e 0.85(2) 2.56(15) 3.13(3) 124(14) . yes
O4 H4B O17'^f 0.85(2) 2.01(10) 2.52(6) 118(7) . yes
C28 H28 O15'^d 0.93 2.47 3.31(7) 150.0 8_655 yes
C29 H29 O14'^d 0.93 2.50 3.31(7) 145.7 8_655 yes
C44 H44 O10^e 0.93 2.60 3.17(3) 119.8 . yes
C44 H44 O12^e 0.93 2.57 3.48(4) 164.8 . yes
C44 H44 N13^e 0.93 2.63 3.37(3) 137.6 . yes
C46 H46 O15^c 0.93 2.30 3.22(5) 170.3 . yes
C46 H46 O13'^d 0.93 2.37 3.09(6) 134.5 . yes
C48 H48 O9 0.93 2.57 3.25(2) 131.0 . yes
O8 H8A O15^c 0.87(2) 2.43(7) 3.05(4) 129(6) 8_655 yes
O8 H8A O15'^d 0.87(2) 2.36(8) 3.20(7) 162(10) 8_655 yes
O8 H8B O11^e 0.87(2) 2.20(8) 2.85(3) 131(9) . yes
O8 H8B O17'^f 0.87(2) 2.35(14) 2.99(6) 131(14) . yes
N11 H11A N14^c 0.90(2) 2.55(10) 3.27(3) 138(12) . yes
N11 H11A O13^c 0.90(2) 2.15(9) 2.93(4) 145(12) . yes
N11 H11A O13'^d 0.90(2) 2.19(13) 2.78(7) 123(11) . yes

_refine_diff_density_max         0.715
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.129



# start Validation Reply Form
_vrf_THETM01_K16                 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal was very poorly diffracting. Crystallisation
of the compound was very difficult. After several attempts of 
crystallisation only the presnt sample could be obtained. 
;
_vrf_RINTA01_K16                 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: This is due to weak diffraction of the crystal.
;
_vrf_PLAT020_K16                 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.231 Report
RESPONSE: This is due to weak diffraction of the crystal.
;
_vrf_PLAT088_K16                 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.39 Note  
RESPONSE: Resolution of the diffraction data is poor. Also the 
disorder of the counter anions and solvent water molecules have
increased the number of refinement parameters.
;
_vrf_PLAT306_K16                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O16 Check 
RESPONSE: The hydrogen atoms could not be located in the 
difference Fourier map.
;
_vrf_PLAT341_K16                 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02981 Ang.  
RESPONSE: This could be due to poor resolution data.
;
_vrf_PLAT420_K16                 
;
PROBLEM: D-H Bond Without Acceptor  O9       --H9A      .     Please Check 
RESPONSE: There are no acceptor atoms in the vicinity.
;
_vrf_PLAT430_K16                 
;
PROBLEM: Short Inter D...A Contact  O7       ..O16      .       2.81 Ang.  
RESPONSE: It must be a hydrogen bonded interaction between
water molecules. The hydrogen atoms could not be located.
;
_vrf_PLAT910_K16                 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: These reflections might have been occluded by
x-ray beam stop.
;
# end Validation Reply Form

