# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_compound-Cu6Zn
_database_code_depnum_ccdc_archive 'CCDC 2153696'
loop_
_audit_author_name
_audit_author_address
'Oscar Castillo'
;University of the Basque Country
Spain
;
_audit_update_record             
;
2022-09-13 deposited with the CCDC.	2023-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL

_chemical_name_systematic        
hexakis(mu-adeninato)hexa(mu3-hidroxido)hexa(mu-aqua)hexacopper(II)zincsulfate-water(1/16)
_chemical_formula_moiety         
;
(C30 H42 Cu6 Zn N30 O12), (O4 S), 32(H2O)
;
_chemical_formula_sum            'C30 H106 Cu6 N30 O48 S Zn'
_chemical_formula_weight         2134.11

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   19.1078(10)
_cell_length_b                   19.1078(10)
_cell_length_c                   43.046(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13610.9(17)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5438
_cell_measurement_theta_min      3.106
_cell_measurement_theta_max      27.438
_cell_measurement_wavelength     0.71073

_exptl_crystal_description       prism
_exptl_crystal_colour            'light blue'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_F_000             6600
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun  6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.847

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            29410
_diffrn_reflns_av_unetI/netI     0.1348
_diffrn_reflns_av_R_equivalents  0.1878
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_theta_min         3.106
_diffrn_reflns_theta_max         27.438
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3284
_reflns_number_gt                1552
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'


_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 One of the adeninato ligands is dissordered over two coplanar positions 
 which has imply to refine several atoms with partial occupation factors.,SQUEEZE
;

# SQUEEZE RESULTS (Version = 120716)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.008 0.486 0.003 5703 1734 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_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)+(0.1629P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3284
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1643
_refine_ls_R_factor_gt           0.0876
_refine_ls_wR_factor_ref         0.3055
_refine_ls_wR_factor_gt          0.2612
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_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
Zn Zn 1.000000 1.000000 0.500000 0.0436(7) Uani 1 6 d S T P . .
Cu2 Cu 0.81914(5) 0.95462(6) 0.50064(3) 0.0503(5) Uani 1 1 d . . . . .
N1 N 0.6560(5) 0.6373(4) 0.54466(19) 0.066(2) Uani 1 1 d . . . . .
C2 C 0.7254(6) 0.6803(5) 0.5301(2) 0.067(3) Uani 1 1 d . . . . .
H2 H 0.755357 0.655209 0.525862 0.080 Uiso 1 1 calc R U . . .
N3 N 0.7569(4) 0.7585(4) 0.52073(17) 0.0557(18) Uani 1 1 d . . . . .
C4 C 0.7117(4) 0.7952(5) 0.5286(2) 0.053(2) Uani 1 1 d . . . . .
C5A C 0.6371(5) 0.7517(5) 0.5449(2) 0.064(3) Uani 1 1 d . . . A 1
C6A C 0.6070(6) 0.6694(6) 0.5527(2) 0.068(3) Uani 1 1 d . . . A 1
N6 N 0.5370(4) 0.6227(4) 0.5672(2) 0.080(3) Uani 1 1 d . . . A 1
H6A1 H 0.522548 0.573315 0.571457 0.096 Uiso 1 1 calc R U . A 1
H6A2 H 0.506417 0.641925 0.572198 0.096 Uiso 1 1 calc R U . A 1
N7 N 0.6071(4) 0.8042(4) 0.55018(16) 0.0575(19) Uani 1 1 d . . . . .
C8 C 0.6626(5) 0.8716(5) 0.5363(2) 0.063(3) Uani 1 1 d . . . . .
H8 H 0.658052 0.917816 0.535600 0.075 Uiso 1 1 calc R U . . .
N9 N 0.7265(4) 0.8693(4) 0.52326(18) 0.0559(18) Uani 1 1 d . . . . .
O1 O 0.9208(3) 1.0304(3) 0.47930(13) 0.0446(14) Uani 1 1 d . . . . .
H1 H 0.919325 1.029685 0.456544 0.054 Uiso 1 1 calc R U . . .
O1W O 0.7953(3) 0.8536(3) 0.45982(16) 0.0593(16) Uani 1 1 d . . . . .
S1 S 0.4046(5) 0.7345(5) 0.5636(2) 0.024(2) Uani 0.1667 1 d . . P B -1
O1S O 0.4504(19) 0.709(2) 0.5812(8) 0.036(9) Uiso 0.1667 1 d . . P B -1
O2S O 0.453(2) 0.7981(18) 0.5373(8) 0.052(8) Uiso 0.1667 1 d . . P B -1
O3S O 0.341(9) 0.666(13) 0.5475(4) 0.031(9) Uiso 0.1667 1 d . . P B -1
O4S O 0.3670(12) 0.7638(12) 0.5837(5) 0.017(5) Uiso 0.1667 1 d . . P B -1
O2W O 0.2743(14) 0.5294(13) 0.5830(5) 0.067(8) Uiso 0.33(2) 1 d . . . C -1
O4W O 0.1916(12) 0.6683(12) 0.5671(5) 0.043(9) Uiso 0.240(17) 1 d . . . D -1


_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
Zn O1 2.075(5) . ?
Zn O1 2.075(5) 20_566 ?
Zn O1 2.075(5) 2_765 ?
Zn O1 2.075(5) 21_656 ?
Zn O1 2.075(5) 19_776 ?
Zn O1 2.075(5) 3_675 ?
Zn Cu2 3.1143(9) . ?
Cu2 N9 1.963(7) . ?
Cu2 O1 1.974(4) 21_656 ?
Cu2 O1 1.974(5) . ?
Cu2 N3 2.009(7) 20_566 ?
Cu2 O1W 2.440(6) 20_566 ?
Cu2 Cu2 3.1147(9) 20_566 ?
N1 C2 1.318(11) . ?
N1 C6A 1.395(12) . ?
C2 N3 1.363(10) . ?
N3 C4 1.400(10) . ?
C4 N9 1.319(10) . ?
C4 C5A 1.424(12) . ?
C5A N7 1.402(11) . ?
C5A C6A 1.418(12) . ?
C6A N6 1.335(11) . ?
N7 C8 1.332(11) . ?
C8 N9 1.364(10) . ?
S1 O4S 1.41(2) . ?
S1 O1S 1.41(3) . ?
S1 O3S 1.45(18) . ?
S1 O2S 1.58(3) . ?

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
O1 Zn O1 77.09(18) . 20_566 ?
O1 Zn O1 102.91(18) . 2_765 ?
O1 Zn O1 180.0 20_566 2_765 ?
O1 Zn O1 77.09(18) . 21_656 ?
O1 Zn O1 102.91(18) 20_566 21_656 ?
O1 Zn O1 77.09(18) 2_765 21_656 ?
O1 Zn O1 180.00(14) . 19_776 ?
O1 Zn O1 102.91(18) 20_566 19_776 ?
O1 Zn O1 77.09(18) 2_765 19_776 ?
O1 Zn O1 102.91(18) 21_656 19_776 ?
O1 Zn O1 102.91(18) . 3_675 ?
O1 Zn O1 77.09(18) 20_566 3_675 ?
O1 Zn O1 102.91(18) 2_765 3_675 ?
O1 Zn O1 180.0 21_656 3_675 ?
O1 Zn O1 77.09(18) 19_776 3_675 ?
O1 Zn Cu2 38.56(13) . . ?
O1 Zn Cu2 89.36(12) 20_566 . ?
O1 Zn Cu2 90.64(12) 2_765 . ?
O1 Zn Cu2 38.54(13) 21_656 . ?
O1 Zn Cu2 141.44(13) 19_776 . ?
O1 Zn Cu2 141.46(13) 3_675 . ?
N9 Cu2 O1 89.7(2) . 21_656 ?
N9 Cu2 O1 171.0(2) . . ?
O1 Cu2 O1 81.8(3) 21_656 . ?
N9 Cu2 N3 96.6(3) . 20_566 ?
O1 Cu2 N3 173.3(3) 21_656 20_566 ?
O1 Cu2 N3 92.0(2) . 20_566 ?
N9 Cu2 O1W 95.3(2) . 20_566 ?
O1 Cu2 O1W 90.6(2) 21_656 20_566 ?
O1 Cu2 O1W 87.8(2) . 20_566 ?
N3 Cu2 O1W 86.5(2) 20_566 20_566 ?
N9 Cu2 Zn 130.6(2) . . ?
O1 Cu2 Zn 40.91(15) 21_656 . ?
O1 Cu2 Zn 40.92(14) . . ?
N3 Cu2 Zn 132.8(2) 20_566 . ?
O1W Cu2 Zn 88.22(12) 20_566 . ?
N9 Cu2 Cu2 146.5(2) . 20_566 ?
O1 Cu2 Cu2 92.56(13) 21_656 20_566 ?
O1 Cu2 Cu2 37.91(13) . 20_566 ?
N3 Cu2 Cu2 80.9(2) 20_566 20_566 ?
O1W Cu2 Cu2 51.26(14) 20_566 20_566 ?
Zn Cu2 Cu2 60.0 . 20_566 ?
C2 N1 C6A 122.0(8) . . ?
N1 C2 N3 125.4(9) . . ?
C2 N3 C4 115.7(8) . . ?
C2 N3 Cu2 122.1(6) . 21_656 ?
C4 N3 Cu2 122.1(5) . 21_656 ?
N9 C4 N3 129.9(7) . . ?
N9 C4 C5A 109.1(8) . . ?
N3 C4 C5A 121.0(8) . . ?
N7 C5A C6A 132.2(9) . . ?
N7 C5A C4 108.1(8) . . ?
C6A C5A C4 119.7(9) . . ?
N6 C6A N1 119.3(9) . . ?
N6 C6A C5A 124.6(10) . . ?
N1 C6A C5A 116.1(9) . . ?
C8 N7 C5A 101.9(7) . . ?
N7 C8 N9 116.6(8) . . ?
C4 N9 C8 104.3(7) . . ?
C4 N9 Cu2 126.7(6) . . ?
C8 N9 Cu2 128.9(6) . . ?
Cu2 O1 Cu2 104.2(2) 20_566 . ?
Cu2 O1 Zn 100.5(2) 20_566 . ?
Cu2 O1 Zn 100.5(2) . . ?
O4S S1 O1S 109.4(17) . . ?
O4S S1 O3S 107(3) . . ?
O1S S1 O3S 109(5) . . ?
O4S S1 O2S 110.9(15) . . ?
O1S S1 O2S 114.8(19) . . ?
O3S S1 O2S 105(5) . . ?

_refine_diff_density_max         1.591
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.150

# start Validation Reply Form
_vrf_RINTA01_compound-Cu6Zn      
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Although we performed many synthesis of this compound only small
sized specimens were obtained and containing always minor twin components 
that were very difficult to deal with. It means that the intensity of 
the reflection peaks is greatly dismished and affected by the overlapping 
of these minor twin components.
;
_vrf_PLAT020_compound-Cu6Zn      
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.188 Report
RESPONSE: Although we performed many synthesis of this compound only small
sized specimens were obtained and containing always minor twin components 
that were very difficult to deal with. It means that the intensity of 
the reflection peaks is greatly dismished and affected by the overlapping 
of these minor twin components.
;
_vrf_PLAT430_compound-Cu6Zn      
;
PROBLEM: Short Inter D...A Contact  O1W      ..O4S      .       2.80 Ang.  
RESPONSE: It corresponds to a hydrogen bond interaction but the hydrogen 
atoms of the water molecules were not placed due to the dissorder of the 
solvent molecules located in the pores.
;
_vrf_PLAT934_compound-Cu6Zn      
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          2 Check 
RESPONSE: The presence of minor twin components that have been impossible 
to deal with provides some intensity to these reflections because of the 
overlapping with reflections that should have zero intensity (extinctions).
;
_vrf_PLAT973_compound-Cu6Zn      
;
PROBLEM: Check Calcd Positive Resid. Density on        Zn       1.89 eA-3  
RESPONSE: It probably arises from the previously explained unaccounted 
presence of minor twin components that alter the intensity of some 
reflections and can generate this kind of effect.
;
# end Validation Reply Form


_exptl_crystal_preparation       'Magnetic properties,Porosity'
####################################################################### 
# 
# 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_compound-Cu6Cu
_database_code_depnum_ccdc_archive 'CCDC 2153697'
loop_
_audit_author_name
_audit_author_address
'Oscar Castillo'
;University of the Basque Country
Spain
;
_audit_update_record             
;
2022-09-13 deposited with the CCDC.	2023-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL

_chemical_name_systematic        
hexakis(mu-adeninato)hexa(mu3-hidroxido)tetra(mu-aqua)heptacopper(II)sulfate-water(1/20)
_chemical_formula_moiety         
;
(C30 H38 Cu7 N30 O10), O4 S, 20(H2O)
;
_chemical_formula_sum            'C30 H78 Cu7 N30 O34 S'
_chemical_formula_weight         1880.06

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'
Cu Cu 0.3201 1.2651 '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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_H-M_alt        'C c c m'
_space_group_name_Hall           '-C 2 2c'

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

_cell_length_a                   10.5080(3)
_cell_length_b                   24.8920(8)
_cell_length_c                   27.0312(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7070.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    27320
_cell_measurement_theta_min      3.014
_cell_measurement_theta_max      27.378
_cell_measurement_wavelength     0.71073

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7450 4774 24475 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.2550 4951 24475 nmt 0.9948 -0.0145 -0.0017 -0.0891 -1.0013 -0.0083 -0.0199
0.0109 -1.0002
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by 179.4346° 
 around [1.00 -0.04 -0.01] (reciprocal) or [1.00 -0.01 -0.00] (direct)
;

_cell_special_details            
;

;

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.34
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_F_000             3836
_exptl_absorpt_coefficient_mu    2.200
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun  6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_absorpt_correction_T_min  0.285
_exptl_absorpt_correction_T_max  0.473

# SQUEEZE RESULTS (Version = 120716)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.279 0.218 -0.014 1974 839 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            27320
_diffrn_reflns_av_unetI/netI     0.1263
_diffrn_reflns_av_R_equivalents  0.2493
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.014
_diffrn_reflns_theta_max         27.378
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3846
_reflns_number_gt                2252
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'


_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 One of the adeninato ligands is dissordered over two coplanar positions 
 which has imply to refine several atoms with partial occupation factors.,Twin,SQUEEZE
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1854P)²+99.9101P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3846
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1550
_refine_ls_R_factor_gt           0.1134
_refine_ls_wR_factor_ref         0.3398
_refine_ls_wR_factor_gt          0.3207
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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 0.000000 0.000000 0.11119(6) 0.0324(5) Uani 1 2 d S T P . .
Cu2 Cu 0.000000 0.000000 0.000000 0.0240(6) Uani 1 4 d S T P . .
Cu3 Cu -0.13331(12) 0.09497(5) 0.05811(5) 0.0301(4) Uani 1 1 d . . . . .
O1 O 0.0254(6) 0.0506(3) 0.0554(2) 0.0275(15) Uani 1 1 d . . . . .
H1 H 0.104779 0.069944 0.055620 0.041 Uiso 1 1 d . U . . .
O2 O -0.1802(8) 0.0532(3) 0.000000 0.024(2) Uani 1 2 d S T P D .
H2 H -0.260615 0.047460 0.000000 0.036 Uiso 1 2 d S U P . .
N11 N 0.1604(10) 0.0945(5) 0.2237(4) 0.053(3) Uani 1 1 d . . . . .
C12 C 0.1189(12) 0.0534(7) 0.1979(4) 0.054(4) Uani 1 1 d . . . . .
H12 H 0.146051 0.019287 0.207024 0.065 Uiso 1 1 calc R U . A 2
N13 N 0.0390(9) 0.0576(4) 0.1588(3) 0.041(2) Uani 1 1 d . . . . .
C14 C 0.0128(12) 0.1102(5) 0.1521(4) 0.046(3) Uani 1 1 d . . . . .
C15A C 0.048(2) 0.1568(10) 0.1793(8) 0.033(5) Uiso 0.5 1 d . . P B 1
C16A C 0.137(2) 0.1451(9) 0.2188(8) 0.033(5) Uiso 0.5 1 d . . P B 1
N16A N 0.182(2) 0.1851(9) 0.2485(8) 0.051(5) Uiso 0.5 1 d . . P B 1
H16A H 0.229694 0.177411 0.273249 0.061 Uiso 0.5 1 calc R U P B 1
H16B H 0.161383 0.217913 0.242584 0.061 Uiso 0.5 1 calc R U P B 1
C15B C 0.091(2) 0.1305(11) 0.1911(9) 0.044(6) Uiso 0.5 1 d . . P B 2
C16B C 0.082(3) 0.1860(13) 0.1939(11) 0.060(7) Uiso 0.5 1 d . . P B 2
N16B N 0.159(3) 0.2132(12) 0.2249(10) 0.082(8) Uiso 0.5 1 d . . P B 2
H16C H 0.160303 0.247779 0.224108 0.099 Uiso 0.5 1 calc R U P B 2
H16D H 0.205854 0.196143 0.245603 0.099 Uiso 0.5 1 calc R U P B 2
N17 N 0.0048(11) 0.2096(5) 0.1601(4) 0.057(3) Uani 1 1 d . . . . .
C18 C -0.0582(11) 0.1861(5) 0.1235(4) 0.045(3) Uani 1 1 d . . . . .
H18 H -0.102782 0.208096 0.101700 0.054 Uiso 1 1 calc R U . B 1
N19 N -0.0621(9) 0.1341(4) 0.1158(4) 0.039(2) Uani 1 1 d . . . . .
N21 N -0.4545(11) 0.1957(4) 0.0682(4) 0.053(3) Uani 1 1 d . . . . .
C22 C -0.3517(12) 0.1667(5) 0.0804(5) 0.048(3) Uani 1 1 d . . . . .
H22 H -0.333869 0.160427 0.113645 0.058 Uiso 1 1 calc R U . . .
N23 N -0.2731(9) 0.1461(4) 0.0452(4) 0.041(2) Uani 1 1 d . . . . .
C24 C -0.3202(15) 0.1577(7) 0.000000 0.049(5) Uani 1 2 d S T P . .
C25 C -0.426(2) 0.1904(9) -0.0146(7) 0.040(6) Uiso 0.5 1 d . . P C -1
C26 C -0.498(2) 0.2107(9) 0.0259(8) 0.041(5) Uiso 0.5 1 d . . P C -1
N26 N -0.6019(18) 0.2410(7) 0.0186(7) 0.044(5) Uiso 0.5 1 d . . P C -1
H26A H -0.645422 0.252261 0.043484 0.053 Uiso 0.5 1 calc R U P C -1
H26B H -0.624956 0.249234 -0.010973 0.053 Uiso 0.5 1 calc R U P C -1
O1W O -0.2242(7) 0.0332(3) 0.1097(3) 0.0384(18) Uani 1 1 d . . . D -1
S1 S 0.500000 0.000000 0.0347(3) 0.0294(15) Uani 0.5 2 d S T P E 2
O11 O 0.4036(16) 0.0258(7) 0.0686(6) 0.040(4) Uiso 0.5 1 d . . P E 2
O2W O 0.5971(16) -0.0529(7) -0.0812(6) 0.041(4) Uiso 0.5 1 d . . P E 2
O12 O 0.5579(9) 0.0417(4) 0.0065(6) 0.021(3) Uiso 0.5 1 d . . P E 2
H11W H -0.281050 0.008870 0.104230 0.031 Uiso 1 1 d . U . . .
H12W H -0.233050 0.041970 0.140310 0.031 Uiso 1 1 d . U . . .


_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 N13 1.969(10) . ?
Cu1 N13 1.969(10) 2 ?
Cu1 O1 1.983(7) . ?
Cu1 O1 1.983(7) 2 ?
Cu1 Cu2 3.0056(17) . ?
Cu2 O1 1.975(7) 9 ?
Cu2 O1 1.975(7) 10 ?
Cu2 O1 1.975(7) 2 ?
Cu2 O1 1.975(7) . ?
Cu2 O2 2.310(9) . ?
Cu2 O2 2.310(9) 9 ?
Cu3 O2 1.947(5) . ?
Cu3 N23 1.975(10) . ?
Cu3 N19 1.984(9) . ?
Cu3 O1 2.001(7) . ?
Cu3 O1W 2.286(8) . ?
O1 H1 0.9633 . ?
O2 H2 0.8569 . ?
N11 C16A 1.29(2) . ?
N11 C12 1.313(17) . ?
N11 C15B 1.45(3) . ?
C12 N13 1.354(15) . ?
C12 C15B 1.95(3) . ?
C12 H12 0.9300 . ?
N13 C14 1.351(16) . ?
C14 N19 1.391(16) . ?
C14 C15A 1.42(3) . ?
C14 C15B 1.43(3) . ?
C15A C16A 1.45(3) . ?
C15A N17 1.48(3) . ?
C15A C18 2.01(3) . ?
C16A N16A 1.36(3) . ?
N16A H16A 0.8600 . ?
N16A H16B 0.8600 . ?
C15B C16B 1.39(4) . ?
C16B N16B 1.34(4) . ?
C16B N17 1.36(3) . ?
N16B H16C 0.8600 . ?
N16B H16D 0.8600 . ?
N17 C18 1.328(15) . ?
C18 N19 1.313(15) . ?
C18 H18 0.9300 . ?
N21 C26 1.29(3) . ?
N21 C22 1.341(17) . ?
C22 N23 1.360(15) . ?
C22 H22 0.9300 . ?
N23 C24 1.349(12) . ?
C24 C25 1.44(3) . ?
C25 C26 1.42(3) . ?
C26 N26 1.34(3) . ?
N26 H26A 0.8600 . ?
N26 H26B 0.8600 . ?
O1W H11W 0.8632 . ?
O1W H12W 0.8598 . ?
S1 O12 1.423(13) . ?
S1 O12 1.423(12) 2_655 ?
S1 O11 1.510(18) . ?
S1 O11 1.510(18) 2_655 ?
S1 O12 1.639(14) 9_655 ?
S1 O12 1.639(14) 10 ?
S1 S1 1.876(15) 9_655 ?
S1 O2W 2.087(18) 9_655 ?
S1 O2W 2.087(18) 10 ?
S1 O2W 3.548(18) . ?
O11 O2W 0.755(19) 9_655 ?
O12 O12 0.35(3) 10 ?

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
N13 Cu1 N13 98.4(6) . 2 ?
N13 Cu1 O1 90.4(4) . . ?
N13 Cu1 O1 170.9(3) 2 . ?
N13 Cu1 O1 170.9(3) . 2 ?
N13 Cu1 O1 90.4(4) 2 2 ?
O1 Cu1 O1 81.0(4) . 2 ?
N13 Cu1 Cu2 130.8(3) . . ?
N13 Cu1 Cu2 130.8(3) 2 . ?
O1 Cu1 Cu2 40.5(2) . . ?
O1 Cu1 Cu2 40.5(2) 2 . ?
O1 Cu2 O1 81.4(4) 9 10 ?
O1 Cu2 O1 98.6(4) 9 2 ?
O1 Cu2 O1 180.0(4) 10 2 ?
O1 Cu2 O1 180.0 9 . ?
O1 Cu2 O1 98.6(4) 10 . ?
O1 Cu2 O1 81.4(4) 2 . ?
O1 Cu2 O2 104.8(2) 9 . ?
O1 Cu2 O2 75.2(2) 10 . ?
O1 Cu2 O2 104.8(2) 2 . ?
O1 Cu2 O2 75.2(2) . . ?
O1 Cu2 O2 75.2(2) 9 9 ?
O1 Cu2 O2 104.8(2) 10 9 ?
O1 Cu2 O2 75.2(2) 2 9 ?
O1 Cu2 O2 104.8(2) . 9 ?
O2 Cu2 O2 180.0 . 9 ?
O1 Cu2 Cu1 139.3(2) 9 . ?
O1 Cu2 Cu1 139.3(2) 10 . ?
O1 Cu2 Cu1 40.7(2) 2 . ?
O1 Cu2 Cu1 40.7(2) . . ?
O2 Cu2 Cu1 90.0 . . ?
O2 Cu2 Cu1 90.0 9 . ?
O1 Cu2 Cu1 40.7(2) 9 9 ?
O1 Cu2 Cu1 40.7(2) 10 9 ?
O1 Cu2 Cu1 139.3(2) 2 9 ?
O1 Cu2 Cu1 139.3(2) . 9 ?
O2 Cu2 Cu1 90.0 . 9 ?
O2 Cu2 Cu1 90.0 9 9 ?
Cu1 Cu2 Cu1 180.0 . 9 ?
O2 Cu3 N23 90.8(4) . . ?
O2 Cu3 N19 172.4(4) . . ?
N23 Cu3 N19 95.9(4) . . ?
O2 Cu3 O1 83.5(3) . . ?
N23 Cu3 O1 165.7(4) . . ?
N19 Cu3 O1 89.1(3) . . ?
O2 Cu3 O1W 91.6(3) . . ?
N23 Cu3 O1W 103.3(3) . . ?
N19 Cu3 O1W 90.5(3) . . ?
O1 Cu3 O1W 90.0(3) . . ?
Cu2 O1 Cu1 98.8(3) . . ?
Cu2 O1 Cu3 105.5(3) . . ?
Cu1 O1 Cu3 102.2(3) . . ?
Cu2 O1 H1 116.1 . . ?
Cu1 O1 H1 115.4 . . ?
Cu3 O1 H1 116.5 . . ?
Cu3 O2 Cu3 107.5(4) 10 . ?
Cu3 O2 Cu2 95.7(3) 10 . ?
Cu3 O2 Cu2 95.7(3) . . ?
Cu3 O2 H2 109.8 10 . ?
Cu3 O2 H2 109.8 . . ?
Cu2 O2 H2 135.5 . . ?
C16A N11 C12 129.9(15) . . ?
C12 N11 C15B 89.5(13) . . ?
N11 C12 N13 124.2(14) . . ?
N11 C12 C15B 48.1(10) . . ?
N13 C12 C15B 76.1(11) . . ?
N11 C12 H12 117.9 . . ?
N13 C12 H12 117.9 . . ?
C15B C12 H12 165.9 . . ?
C14 N13 C12 107.7(11) . . ?
C14 N13 Cu1 125.2(8) . . ?
C12 N13 Cu1 125.7(10) . . ?
N13 C14 N19 128.6(10) . . ?
N13 C14 C15A 132.1(15) . . ?
N19 C14 C15A 99.3(13) . . ?
N13 C14 C15B 97.2(15) . . ?
N19 C14 C15B 134.1(15) . . ?
C14 C15A C16A 113(2) . . ?
C14 C15A N17 117.7(17) . . ?
C16A C15A N17 129(2) . . ?
C14 C15A C18 76.4(12) . . ?
C16A C15A C18 169.2(19) . . ?
N17 C15A C18 41.3(8) . . ?
N11 C16A N16A 126(2) . . ?
N11 C16A C15A 113(2) . . ?
N16A C16A C15A 121(2) . . ?
C16A N16A H16A 120.0 . . ?
C16A N16A H16B 120.0 . . ?
H16A N16A H16B 120.0 . . ?
C16B C15B C14 111(2) . . ?
C16B C15B N11 128(2) . . ?
C14 C15B N11 121(2) . . ?
C16B C15B C12 170(2) . . ?
C14 C15B C12 78.9(13) . . ?
N11 C15B C12 42.3(9) . . ?
N16B C16B N17 124(3) . . ?
N16B C16B C15B 120(3) . . ?
N17 C16B C15B 116(3) . . ?
C16B N16B H16C 120.0 . . ?
C16B N16B H16D 120.0 . . ?
H16C N16B H16D 120.0 . . ?
C18 N17 C16B 127.6(17) . . ?
C18 N17 C15A 91.2(13) . . ?
N19 C18 N17 124.7(12) . . ?
N19 C18 C15A 77.2(10) . . ?
N17 C18 C15A 47.5(9) . . ?
N19 C18 H18 117.7 . . ?
N17 C18 H18 117.7 . . ?
C15A C18 H18 165.1 . . ?
C18 N19 C14 107.0(10) . . ?
C18 N19 Cu3 128.3(9) . . ?
C14 N19 Cu3 123.9(7) . . ?
C26 N21 C22 131.6(16) . . ?
N21 C22 N23 121.2(12) . . ?
N21 C22 H22 119.4 . . ?
N23 C22 H22 119.4 . . ?
C24 N23 C22 109.4(11) . . ?
C24 N23 Cu3 124.7(9) . . ?
C22 N23 Cu3 124.8(9) . . ?
N23 C24 N23 129.8(15) 10 . ?
N23 C24 C25 99.0(10) 10 . ?
N23 C24 C25 130.9(12) . . ?
C26 C25 C24 113.8(15) . . ?
N21 C26 N26 126(2) . . ?
N21 C26 C25 112.8(19) . . ?
N26 C26 C25 121(2) . . ?
C26 N26 H26A 120.0 . . ?
C26 N26 H26B 120.0 . . ?
H26A N26 H26B 120.0 . . ?
Cu3 O1W H11W 131.0 . . ?
Cu3 O1W H12W 117.4 . . ?
H11W O1W H12W 105.6 . . ?
O12 S1 O11 107.5(8) . . ?
O12 S1 O11 110.4(8) 2_655 . ?
O12 S1 O12 10.5(10) . 10 ?
O12 S1 O12 104.8(6) 2_655 10 ?
O11 S1 O12 113.1(7) . 10 ?
O11 S1 O12 115.7(8) 2_655 10 ?
O12 S1 O12 94.3(10) 9_655 10 ?
O12 S1 O2W 71.1(7) . . ?
O12 S1 O2W 51.7(6) 2_655 . ?
O11 S1 O2W 152.5(8) . . ?
O11 S1 O2W 100.6(6) 2_655 . ?
O12 S1 O2W 43.2(5) 9_655 . ?
O12 S1 O2W 61.8(5) 10 . ?
S1 S1 O2W 28.0(3) 9_655 . ?
O2W S1 O2W 155.0(3) 9_655 . ?
O2W S1 O2W 99.0(7) 10 . ?
O2W O11 S1 131(2) 9_655 . ?
O11 O2W S1 43.0(18) 9_655 . ?
S1 O2W S1 25.0(3) 9_655 . ?
O12 O12 S1 122.4(7) 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
O2 H2 O12 0.86 1.92 2.773(13) 172.6 1_455

_refine_diff_density_max         2.355
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.214

# start Validation Reply Form
_vrf_RINTA01_compound-Cu6Cu      
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Although we performed many synthesis of this compound only small
sized specimens were obtained and containing always minor twin components 
that were very difficult to deal with. It means that the intensity of 
the reflection peaks is greatly dismished and affected by the overlapping 
of these minor twin components.
;
_vrf_PLAT020_compound-Cu6Cu      
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.249 Report
RESPONSE: Although we performed many synthesis of this compound only small
sized specimens were obtained and containing always minor twin components 
that were very difficult to deal with. It means that the intensity of 
the reflection peaks is greatly dismished and affected by the overlapping 
of these minor twin components.
;
_vrf_PLAT420_compound-Cu6Cu      
;
PROBLEM: D-H Bond Without Acceptor  O1       --H1       .     Please Check 
RESPONSE: The solvent molecules occupying the pores of the compound are so
disordered that they were not located, instead the electron density located
inside the pore was removed using the SQUEEZE procedure. Therefore, the 
hydrogen bonding acceptor of this molecule is not located although for sure 
there should be.
;
# end Validation Reply Form


_exptl_crystal_preparation       'Magnetic properties,Porous'
####################################################################### 
# 
# 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_compound-Cu6Co
_database_code_depnum_ccdc_archive 'CCDC 2153698'
loop_
_audit_author_name
_audit_author_address
'Oscar Castillo'
;University of the Basque Country
Spain
;
_audit_update_record             
;
2022-09-13 deposited with the CCDC.	2023-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL

_chemical_name_systematic        
hexakis(mu-adeninato)hexa(mu3-hidroxido)hexa(mu-aqua)cobalt(II)hexacopper(II)sulfate-water(1/35)
_chemical_formula_moiety         
;
(C30 H42 Co Cu6 N30 O12), (O4 S), 35(H2O)
;
_chemical_formula_sum            'C30 H112 Co Cu6 N30 O51 S'
_chemical_formula_weight         2181.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   19.058(3)
_cell_length_b                   19.058(3)
_cell_length_c                   43.157(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13575(5)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    27448
_cell_measurement_theta_min      3.371
_cell_measurement_theta_max      64.999

_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5854 28191 5671 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.4146 27316 5671 nmt 1.0246 0.0504 0.0048 -0.9760 -1.0216 0.0195 -0.0465
-0.1592 -0.9991
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -176.4808° 
 around [0.90 -0.43 0.01] (reciprocal) or [1.00 0.02 0.00] (direct)
;
_cell_special_details            
;

;

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_F_000             6762
_exptl_absorpt_coefficient_mu    4.095
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun  6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.847

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            27448
_diffrn_reflns_av_unetI/netI     0.2541
_diffrn_reflns_av_R_equivalents  0.4476
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_theta_min         3.371
_diffrn_reflns_theta_max         64.999
_diffrn_reflns_theta_full        64.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2581
_reflns_number_gt                571
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'


_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 One of the adeninato ligands is dissordered over two coplanar positions 
 which has imply to refine several atoms with partial occupation factors.,Twin,SQUEEZE
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1345P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2581
_refine_ls_number_parameters     118
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.2402
_refine_ls_R_factor_gt           0.1058
_refine_ls_wR_factor_ref         0.3189
_refine_ls_wR_factor_gt          0.2648
_refine_ls_goodness_of_fit_ref   0.789
_refine_ls_restrained_S_all      0.785
_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
Co1 Co 0.000000 0.000000 0.500000 0.0771(18) Uani 1 6 d S T P . .
Cu1 Cu -0.12378(15) -0.18442(14) 0.49921(6) 0.1026(10) Uani 1 1 d D . . . .
O1 O -0.0199(6) -0.1076(6) 0.4792(2) 0.098(3) Uani 1 1 d . . . . .
H1 H -0.018558 -0.108373 0.456529 0.118 Uiso 1 1 calc R U . . .
N11A N -0.1736(15) -0.4073(13) 0.4533(3) 0.089(9) Uiso 0.5 1 d D . P A 1
C12A C -0.1716(16) -0.3380(12) 0.4686(3) 0.082(9) Uiso 0.5 1 d D . P A 1
H12A H -0.223652 -0.346201 0.471115 0.099 Uiso 0.5 1 calc R U P A 1
N13A N -0.1202(12) -0.2711(8) 0.4792(3) 0.058(6) Uiso 0.5 1 d D . P A 1
C14A C -0.0229(11) -0.2619(13) 0.4732(4) 0.060(7) Uiso 0.5 1 d D . P A 1
C15A C -0.0213(16) -0.3324(15) 0.4573(4) 0.085(9) Uiso 0.5 1 d D . P A 1
C16A C -0.1019(13) -0.4019(13) 0.4485(4) 0.079(8) Uiso 0.5 1 d D . P A 1
N16A N -0.1139(15) -0.4764(11) 0.4329(4) 0.091(8) Uiso 0.5 1 d D . P A 1
H16A H -0.161962 -0.514620 0.428453 0.109 Uiso 0.5 1 calc R U P A 1
H16B H -0.072700 -0.481525 0.428310 0.109 Uiso 0.5 1 calc R U P A 1
N17A N 0.0571(18) -0.3078(17) 0.4561(5) 0.159(17) Uiso 0.5 1 d D . P A 1
C18A C 0.0963(17) -0.2396(17) 0.4679(5) 0.097(11) Uiso 0.5 1 d D . P A 1
H18A H 0.152577 -0.213400 0.468756 0.116 Uiso 0.5 1 calc R U P A 1
N19A N 0.061(2) -0.2086(14) 0.4779(4) 0.23(3) Uiso 0.5 1 d D . P A 1
N11B N 0.0295(13) -0.3393(12) 0.4556(3) 0.075(7) Uiso 0.5 1 d D . P A 2
C12B C 0.0562(15) -0.2643(12) 0.4726(3) 0.074(8) Uiso 0.5 1 d D . P A 2
H12B H 0.111136 -0.238240 0.477234 0.089 Uiso 0.5 1 calc R U P A 2
N13B N 0.0232(12) -0.2268(8) 0.4823(3) 0.059(6) Uiso 0.5 1 d D . P A 2
C14B C -0.0817(11) -0.2836(11) 0.4718(4) 0.060(7) Uiso 0.5 1 d D . P A 2
C15B C -0.1130(16) -0.3630(16) 0.4539(4) 0.114(12) Uiso 0.5 1 d D . P A 2
C16B C -0.0483(15) -0.3832(14) 0.4474(4) 0.122(14) Uiso 0.5 1 d D . P A 2
N16B N -0.0613(17) -0.4566(13) 0.4305(5) 0.174(17) Uiso 0.5 1 d D . P A 2
H16C H -0.021361 -0.464838 0.427434 0.208 Uiso 0.5 1 calc R U P A 2
H16D H -0.108741 -0.490902 0.423691 0.208 Uiso 0.5 1 calc R U P A 2
N17B N -0.1913(14) -0.3875(14) 0.4502(4) 0.081(8) Uiso 0.5 1 d D . P A 2
C18B C -0.2060(17) -0.3370(16) 0.4623(5) 0.092(10) Uiso 0.5 1 d D . P A 2
H18B H -0.258312 -0.345022 0.461709 0.111 Uiso 0.5 1 calc R U P A 2
N19B N -0.153(2) -0.2781(10) 0.4748(4) 0.20(2) Uiso 0.5 1 d D . P A 2
O1W O -0.2005(8) -0.1617(7) 0.4595(3) 0.125(4) Uani 1 1 d . . . . .
S1 S 0.000000 0.000000 0.4094(5) 0.138(7) Uiso 0.5 3 d S . P B 1
O1S O 0.000000 0.000000 0.3762(7) 0.067(8) Uiso 0.5 3 d S . P B 1
O2S O 0.105(3) 0.062(4) 0.4105(13) 0.27(2) Uiso 0.5 1 d . . P B 1
O2W O -0.0716(18) -0.011(2) 0.6063(8) 0.068(15) Uiso 0.28(3) 1 d . . . C 2
O3W O 0.0896(15) 0.0312(18) 0.5824(6) 0.128(14) Uiso 0.52(4) 1 d . . . D 2


_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
Co1 O1 2.093(10) 21_556 ?
Co1 O1 2.093(10) 3 ?
Co1 O1 2.093(10) 20_556 ?
Co1 O1 2.093(10) 2 ?
Co1 O1 2.093(10) . ?
Co1 O1 2.093(10) 19_556 ?
Cu1 N19A 1.896(13) 20_556 ?
Cu1 N13A 1.896(12) . ?
Cu1 N13B 1.897(12) 20_556 ?
Cu1 N19B 1.900(13) . ?
Cu1 O1 1.946(11) 20_556 ?
Cu1 O1 1.977(11) . ?
Cu1 O1W 2.426(13) . ?
O1 H1 0.9800 . ?
N11A C16A 1.34(3) . ?
N11A C12A 1.46(3) . ?
C12A N13A 1.24(2) . ?
C12A H12A 0.9300 . ?
N13A C14A 1.79(2) . ?
C14A N19A 1.41(4) . ?
C14A C15A 1.52(3) . ?
C15A N17A 1.32(3) . ?
C15A C16A 1.49(3) . ?
C16A N16A 1.48(2) . ?
N16A H16A 0.8600 . ?
N16A H16B 0.8600 . ?
N17A C18A 1.24(3) . ?
C18A N19A 1.18(3) . ?
C18A H18A 0.9300 . ?
N11B C16B 1.34(3) . ?
N11B C12B 1.45(3) . ?
C12B N13B 1.24(2) . ?
C12B H12B 0.9300 . ?
N13B C14B 1.79(2) . ?
C14B N19B 1.42(4) . ?
C14B C15B 1.53(3) . ?
C15B N17B 1.33(3) . ?
C15B C16B 1.49(3) . ?
C16B N16B 1.49(2) . ?
N16B H16C 0.8600 . ?
N16B H16D 0.8600 . ?
N17B C18B 1.24(3) . ?
C18B N19B 1.20(3) . ?
C18B H18B 0.9300 . ?
S1 O1S 1.43(3) . ?
S1 O2S 1.74(6) . ?
S1 O2S 1.74(6) 3 ?
S1 O2S 1.74(6) 2 ?
O2W O3W 1.54(4) 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
O1 Co1 O1 180.0(5) 21_556 3 ?
O1 Co1 O1 103.0(3) 21_556 20_556 ?
O1 Co1 O1 77.0(3) 3 20_556 ?
O1 Co1 O1 77.0(3) 21_556 2 ?
O1 Co1 O1 103.0(3) 3 2 ?
O1 Co1 O1 180.0(7) 20_556 2 ?
O1 Co1 O1 77.0(3) 21_556 . ?
O1 Co1 O1 103.0(3) 3 . ?
O1 Co1 O1 77.0(3) 20_556 . ?
O1 Co1 O1 103.0(3) 2 . ?
O1 Co1 O1 103.0(3) 21_556 19_556 ?
O1 Co1 O1 77.0(3) 3 19_556 ?
O1 Co1 O1 103.0(3) 20_556 19_556 ?
O1 Co1 O1 77.0(3) 2 19_556 ?
O1 Co1 O1 180.0 . 19_556 ?
N19A Cu1 N13A 83.1(11) 20_556 . ?
N19A Cu1 N13B 19.7(13) 20_556 20_556 ?
N13A Cu1 N13B 95.4(9) . 20_556 ?
N13B Cu1 N19B 83.9(11) 20_556 . ?
N19A Cu1 O1 102.9(11) 20_556 20_556 ?
N13A Cu1 O1 170.2(7) . 20_556 ?
N13B Cu1 O1 92.5(6) 20_556 20_556 ?
N19B Cu1 O1 170.9(12) . 20_556 ?
N19A Cu1 O1 166.0(12) 20_556 . ?
N13A Cu1 O1 89.2(6) . . ?
N13B Cu1 O1 174.1(7) 20_556 . ?
N19B Cu1 O1 99.7(10) . . ?
O1 Cu1 O1 83.3(6) 20_556 . ?
N19A Cu1 O1W 100.8(10) 20_556 . ?
N13A Cu1 O1W 97.0(6) . . ?
N13B Cu1 O1W 84.1(6) 20_556 . ?
N19B Cu1 O1W 81.7(10) . . ?
O1 Cu1 O1W 89.6(4) 20_556 . ?
O1 Cu1 O1W 91.7(4) . . ?
Cu1 O1 Cu1 104.6(5) 21_556 . ?
Cu1 O1 Co1 100.3(4) 21_556 . ?
Cu1 O1 Co1 99.3(4) . . ?
Cu1 O1 H1 116.6 21_556 . ?
Cu1 O1 H1 116.6 . . ?
Co1 O1 H1 116.6 . . ?
C16A N11A C12A 116(2) . . ?
N13A C12A N11A 138(2) . . ?
N13A C12A H12A 110.9 . . ?
N11A C12A H12A 110.9 . . ?
C12A N13A C14A 107.2(14) . . ?
C12A N13A Cu1 135.1(16) . . ?
C14A N13A Cu1 117.8(12) . . ?
N19A C14A C15A 100.6(15) . . ?
N19A C14A N13A 142.3(18) . . ?
C15A C14A N13A 117.0(17) . . ?
N17A C15A C16A 142(3) . . ?
N17A C15A C14A 103(2) . . ?
C16A C15A C14A 116(2) . . ?
N11A C16A N16A 110(2) . . ?
N11A C16A C15A 126(2) . . ?
N16A C16A C15A 124.3(19) . . ?
C16A N16A H16A 120.0 . . ?
C16A N16A H16B 120.0 . . ?
H16A N16A H16B 120.0 . . ?
C18A N17A C15A 110(3) . . ?
N19A C18A N17A 119(3) . . ?
N19A C18A H18A 120.7 . . ?
N17A C18A H18A 120.7 . . ?
C18A N19A C14A 108(2) . . ?
C18A N19A Cu1 150(4) . 21_556 ?
C14A N19A Cu1 102(2) . 21_556 ?
C16B N11B C12B 119(2) . . ?
N13B C12B N11B 135(2) . . ?
N13B C12B H12B 112.3 . . ?
N11B C12B H12B 112.3 . . ?
C12B N13B C14B 107.5(14) . . ?
C12B N13B Cu1 134.7(16) . 21_556 ?
C14B N13B Cu1 117.5(12) . 21_556 ?
N19B C14B C15B 101.8(15) . . ?
N19B C14B N13B 138.8(18) . . ?
C15B C14B N13B 119.5(17) . . ?
N17B C15B C16B 145(3) . . ?
N17B C15B C14B 103(2) . . ?
C16B C15B C14B 113(2) . . ?
N11B C16B N16B 109(2) . . ?
N11B C16B C15B 126(2) . . ?
N16B C16B C15B 124.4(19) . . ?
C16B N16B H16C 120.0 . . ?
C16B N16B H16D 120.0 . . ?
H16C N16B H16D 120.0 . . ?
C18B N17B C15B 109(3) . . ?
N19B C18B N17B 120(3) . . ?
N19B C18B H18B 119.8 . . ?
N17B C18B H18B 119.8 . . ?
C18B N19B C14B 106(2) . . ?
C18B N19B Cu1 148(4) . . ?
C14B N19B Cu1 106(2) . . ?
O1S S1 O2S 92(2) . . ?
O1S S1 O2S 92(2) . 3 ?
O2S S1 O2S 119.93(19) . 3 ?
O1S S1 O2S 92(2) . 2 ?
O2S S1 O2S 119.9(2) . 2 ?
O2S S1 O2S 119.9(2) 3 2 ?

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
C16A N11A C12A N13A 0.0(4) . . . . ?
N11A C12A N13A C14A -0.2(3) . . . . ?
N11A C12A N13A Cu1 -179.4(11) . . . . ?
N19A Cu1 N13A C12A 44.8(9) 20_556 . . . ?
O1 Cu1 N13A C12A -147.0(9) . . . . ?
O1W Cu1 N13A C12A -55.3(9) . . . . ?
N19A Cu1 N13A C14A -134.3(11) 20_556 . . . ?
O1 Cu1 N13A C14A 33.9(7) . . . . ?
O1W Cu1 N13A C14A 125.6(7) . . . . ?
C12A N13A C14A N19A 179.4(10) . . . . ?
Cu1 N13A C14A N19A -1.3(15) . . . . ?
C12A N13A C14A C15A 0.2(7) . . . . ?
Cu1 N13A C14A C15A 179.5(10) . . . . ?
N19A C14A C15A N17A 0.0(9) . . . . ?
N13A C14A C15A N17A 179.5(6) . . . . ?
N19A C14A C15A C16A -179.5(7) . . . . ?
N13A C14A C15A C16A 0.0(10) . . . . ?
C12A N11A C16A N16A 179.9(4) . . . . ?
C12A N11A C16A C15A 0.3(9) . . . . ?
N17A C15A C16A N11A -179.4(10) . . . . ?
C14A C15A C16A N11A -0.2(12) . . . . ?
N17A C15A C16A N16A 1.0(17) . . . . ?
C14A C15A C16A N16A -179.8(7) . . . . ?
C16A C15A N17A C18A 179.1(11) . . . . ?
C14A C15A N17A C18A -0.1(10) . . . . ?
C15A N17A C18A N19A 0.2(13) . . . . ?
N17A C18A N19A C14A -0.3(12) . . . . ?
N17A C18A N19A Cu1 171(2) . . . 21_556 ?
C15A C14A N19A C18A 0.2(9) . . . . ?
N13A C14A N19A C18A -179.1(9) . . . . ?
C15A C14A N19A Cu1 -175.3(9) . . . 21_556 ?
N13A C14A N19A Cu1 5.4(15) . . . 21_556 ?
C16B N11B C12B N13B -0.1(4) . . . . ?
N11B C12B N13B C14B 0.2(3) . . . . ?
N11B C12B N13B Cu1 -172.6(11) . . . 21_556 ?
C12B N13B C14B N19B -179.4(9) . . . . ?
Cu1 N13B C14B N19B -5.2(14) 21_556 . . . ?
C12B N13B C14B C15B -0.4(7) . . . . ?
Cu1 N13B C14B C15B 173.8(10) 21_556 . . . ?
N19B C14B C15B N17B -0.4(8) . . . . ?
N13B C14B C15B N17B -179.8(6) . . . . ?
N19B C14B C15B C16B 179.8(7) . . . . ?
N13B C14B C15B C16B 0.5(9) . . . . ?
C12B N11B C16B N16B 179.9(4) . . . . ?
C12B N11B C16B C15B 0.2(9) . . . . ?
N17B C15B C16B N11B -180.0(10) . . . . ?
C14B C15B C16B N11B -0.4(11) . . . . ?
N17B C15B C16B N16B 0.3(18) . . . . ?
C14B C15B C16B N16B 179.9(7) . . . . ?
C16B C15B N17B C18B -180(100) . . . . ?
C14B C15B N17B C18B 0.5(9) . . . . ?
C15B N17B C18B N19B -0.3(12) . . . . ?
N17B C18B N19B C14B 0.0(12) . . . . ?
N17B C18B N19B Cu1 -173.3(19) . . . . ?
C15B C14B N19B C18B 0.3(9) . . . . ?
N13B C14B N19B C18B 179.4(8) . . . . ?
C15B C14B N19B Cu1 176.5(9) . . . . ?
N13B C14B N19B Cu1 -4.4(14) . . . . ?
N13B Cu1 N19B C18B 33.2(18) 20_556 . . . ?
O1 Cu1 N19B C18B -142.0(18) . . . . ?
O1W Cu1 N19B C18B -51.7(19) . . . . ?
N13B Cu1 N19B C14B -140.0(10) 20_556 . . . ?
O1 Cu1 N19B C14B 44.7(8) . . . . ?
O1W Cu1 N19B C14B 135.0(8) . . . . ?

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
O1 H1 S1 0.98 2.79 3.56(2) 135.4 .
O1 H1 O2S 0.98 2.05 3.00(6) 164.1 3
O1 H1 O3W 0.98 1.93 2.82(3) 150.7 20_556
N16B H16D O3W 0.86 2.45 3.29(4) 165.5 29_445
O1 H1 S1 0.98 2.79 3.56(2) 135.4 .
O1 H1 O2S 0.98 2.05 3.00(6) 164.1 3
O1 H1 O3W 0.98 1.93 2.82(3) 150.7 20_556
N16A H16A O2S 0.86 1.82 2.64(6) 156.7 12_445
N16B H16D O3W 0.86 2.45 3.29(4) 165.5 29_445

_refine_diff_density_max         0.813
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.100

# start Validation Reply Form
_vrf_RINTA01_compound-Cu6Co      
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The crystal is very weakly diffracting (small sized, twinned 
and highly porous) so that a large proportion of essentially "unobserved" 
reflections are being used in the refinement.
;
_vrf_PLAT020_compound-Cu6Co      
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.448 Report
RESPONSE: The crystal is very weakly diffracting (small sized, twinned 
and highly porous) so that a large proportion of essentially "unobserved" 
reflections are being used in the refinement.
;
_vrf_PLAT026_compound-Cu6Co      
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        22% Check 
RESPONSE: The crystal is very weakly diffracting (small sized, twinned 
and highly porous) so that a large proportion of essentially "unobserved" 
reflections are being used in the refinement.
;
# end Validation Reply Form





_exptl_crystal_preparation       'Magnetic properties,Porosity'
