# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_DUT63
_database_code_depnum_ccdc_archive 'CCDC 1480874'
_audit_update_record             
;
2016-05-19 deposited with the CCDC.
2016-08-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_DUT63               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Because of the weak diffraction of the highly porous crystals
at the higher 2Thetha angles, the dataset was integrated to 2Thetha (max)
25 deg.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        DUT-63
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H48 Cu3 N2 O15'
_chemical_formula_weight         1443.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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'
Cu Cu 0.1640 1.8640 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   F432

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

_cell_length_a                   60.910(7)
_cell_length_b                   60.910(7)
_cell_length_c                   60.910(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     225978(45)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    452
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      21.54

_exptl_crystal_description       cubic
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             11792
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_type   .
_exptl_absorpt_correction_T_min  .
_exptl_absorpt_correction_T_max  .
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            8853
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.1282
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       2
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         24.94
_reflns_number_total             8549
_reflns_number_gt                2605
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0321P)²+0.0000P] 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_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.278(13)
_refine_ls_number_reflns         8549
_refine_ls_number_parameters     125
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   0.650
_refine_ls_restrained_S_all      0.658
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.765238(9) 0.234762(9) 0.2339(4) Uani 1 2 d S . .
O1 O 0.01716(6) 0.74529(7) 0.22161(5) 0.2339(17) Uani 1 1 d D . .
O2 O 0.02485(5) 0.71933(6) 0.25032(5) 0.2113(14) Uani 1 1 d D . .
O3 O 0.0000 0.79241(3) 0.20759(3) 0.2742(15) Uani 1 2 d S . .
N1 N 0.15502(7) 0.65502(7) 0.15502(7) 0.325(3) Uani 1 3 d SD . .
C1 C 0.02813(9) 0.73010(14) 0.23223(10) 0.263(4) Uani 1 1 d DU . .
C2 C 0.04703(5) 0.71661(8) 0.21935(7) 0.252(2) Uani 1 1 d GDU . .
C3 C 0.05543(7) 0.72485(6) 0.19980(7) 0.317(3) Uani 1 1 d GDU . .
H3A H 0.0493 0.7374 0.1935 0.380 Uiso 1 1 calc R . .
C4 C 0.07294(7) 0.71437(8) 0.18958(5) 0.302(3) Uani 1 1 d GU . .
H4A H 0.0786 0.7199 0.1765 0.362 Uiso 1 1 calc R . .
C5 C 0.08205(6) 0.69564(8) 0.19892(8) 0.276(2) Uani 1 1 d GDU . .
C6 C 0.07365(8) 0.68740(5) 0.21847(8) 0.306(3) Uani 1 1 d GU . .
H6A H 0.0797 0.6749 0.2247 0.368 Uiso 1 1 calc R . .
C7 C 0.05614(7) 0.69788(8) 0.22869(6) 0.288(3) Uani 1 1 d GDU . .
H7A H 0.0505 0.6924 0.2418 0.345 Uiso 1 1 calc R . .
C8 C 0.10055(6) 0.68335(11) 0.18791(7) 0.355(4) Uani 1 1 d GDU . .
C9 C 0.11512(10) 0.69676(7) 0.17656(8) 0.393(4) Uani 1 1 d GU . .
H9A H 0.1132 0.7119 0.1766 0.472 Uiso 1 1 calc R . .
C10 C 0.13254(8) 0.68752(9) 0.16507(7) 0.428(5) Uani 1 1 d GDU . .
H10A H 0.1423 0.6965 0.1575 0.514 Uiso 1 1 calc R . .
C11 C 0.13540(6) 0.66488(10) 0.16495(8) 0.394(4) Uani 1 1 d GDU . .
C12 C 0.12083(9) 0.65148(6) 0.17630(9) 0.477(5) Uani 1 1 d GDU . .
H12A H 0.1227 0.6363 0.1762 0.572 Uiso 1 1 calc R . .
C13 C 0.10341(7) 0.66071(10) 0.18779(8) 0.432(5) Uani 1 1 d GU . .
H13A H 0.0937 0.6517 0.1954 0.519 Uiso 1 1 calc R . .


_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 O1 1.792(5) 19_566 ?
Cu1 O1 1.792(5) . ?
Cu1 O2 2.000(3) 42_554 ?
Cu1 O2 2.000(3) 28_565 ?
Cu1 O3 2.341(3) . ?
Cu1 Cu1 2.6255(15) 28_565 ?
O1 C1 1.312(7) . ?
O2 C1 1.298(7) . ?
O2 Cu1 2.000(3) 28_565 ?
N1 C11 1.468(3) . ?
N1 C11 1.468(5) 81_455 ?
N1 C11 1.468(5) 29_554 ?
C1 C2 1.617(6) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3A 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4A 0.9300 . ?
C5 C6 1.3900 . ?
C5 C8 1.510(3) . ?
C6 C7 1.3900 . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.3900 . ?
C8 C13 1.3900 . ?
C9 C10 1.3900 . ?
C9 H9A 0.9300 . ?
C10 C11 1.3900 . ?
C10 H10A 0.9300 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?

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 Cu1 O1 161.17(18) 19_566 . ?
O1 Cu1 O2 94.61(12) 19_566 42_554 ?
O1 Cu1 O2 85.59(12) . 42_554 ?
O1 Cu1 O2 85.60(12) 19_566 28_565 ?
O1 Cu1 O2 94.62(12) . 28_565 ?
O2 Cu1 O2 178.7(2) 42_554 28_565 ?
O1 Cu1 O3 99.41(9) 19_566 . ?
O1 Cu1 O3 99.41(9) . . ?
O2 Cu1 O3 89.36(10) 42_554 . ?
O2 Cu1 O3 89.36(10) 28_565 . ?
O1 Cu1 Cu1 80.59(9) 19_566 28_565 ?
O1 Cu1 Cu1 80.59(9) . 28_565 ?
O2 Cu1 Cu1 90.64(10) 42_554 28_565 ?
O2 Cu1 Cu1 90.64(10) 28_565 28_565 ?
O3 Cu1 Cu1 180.00(7) . 28_565 ?
C1 O1 Cu1 123.7(4) . . ?
C1 O2 Cu1 105.4(4) . 28_565 ?
C11 N1 C11 120.0(3) . 81_455 ?
C11 N1 C11 120.0(3) . 29_554 ?
C11 N1 C11 120.0 81_455 29_554 ?
O2 C1 O1 134.1(6) . . ?
O2 C1 C2 105.3(6) . . ?
O1 C1 C2 118.8(6) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 119.6(4) . . ?
C7 C2 C1 120.2(4) . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 C8 118.4(5) . . ?
C4 C5 C8 121.5(5) . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6A 120.0 . . ?
C7 C6 H6A 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C2 C7 H7A 120.0 . . ?
C9 C8 C13 120.0 . . ?
C9 C8 C5 114.0(5) . . ?
C13 C8 C5 126.0(5) . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9A 120.0 . . ?
C10 C9 H9A 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 N1 119.0(4) . . ?
C10 C11 N1 120.7(5) . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C12 C13 C8 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C8 C13 H13A 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.94
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.011

# SQUEEZE RESULTS (APPEND TO CIF)
# 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 -0.002 -0.002 -0.004 206888 29745 ' '
_platon_squeeze_details          
;
;
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_pm3n_sqd
_database_code_depnum_ccdc_archive 'CCDC 1480875'
_audit_update_record             
;
2016-05-19 deposited with the CCDC.
2016-08-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_pm3n_sqd            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Because of the weak diffraction of the highly porous crystals
at the higher 2Thetha angles, the dataset was integrated to 2Thetha (max)
25 deg.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        DUT-64
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H32 Cu2 N1.33 O10'
_chemical_formula_weight         962.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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'
Cu Cu 0.1640 1.8640 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_H-M_alt        'P m -3 n'
_space_group_name_Hall           '-P 4n 2 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   35.490(4)
_cell_length_b                   35.490(4)
_cell_length_c                   35.490(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     44701(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    472
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      18.23

_exptl_crystal_description       cuboctahedral
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.215
_exptl_crystal_F_000             2948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.275
_shelx_estimated_absorpt_T_min   0.978
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            5818
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       1
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.430
_diffrn_reflns_theta_max         23.532
_diffrn_reflns_theta_full        23.532
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3055
_reflns_number_gt                1091
_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       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1879P)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         3055
_refine_ls_number_parameters     83
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.2861
_refine_ls_wR_factor_gt          0.2502
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_restrained_S_all      0.843
_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 0.5000 0.0000 0.21279(4) 0.283(2) Uani 1 4 d S T P . .
N1 N 0.2500 0.2500 0.2500 0.408(8) Uani 1 6 d DS T P . .
O2 O 0.5000 0.0000 0.14745(18) 0.364(4) Uani 1 4 d S T P . .
O1 O 0.46254(17) 0.03746(18) 0.21922(16) 0.317(3) Uani 1 1 d D . . . .
C1 C 0.4492(2) 0.0508(2) 0.2500 0.319(10) Uani 1 2 d DS T P . .
C2 C 0.4210(3) 0.0790(3) 0.2500 0.288(5) Uani 1 2 d DS T P . .
C3 C 0.4067(3) 0.0951(3) 0.2181(2) 0.351(4) Uani 1 1 d D . . . .
H3A H 0.4157 0.0872 0.1948 0.421 Uiso 1 1 calc R U . . .
C4 C 0.3770(3) 0.1251(3) 0.2191(3) 0.364(4) Uani 1 1 d D . . . .
H4A H 0.3694 0.1345 0.1959 0.437 Uiso 1 1 calc R U . . .
C5 C 0.3596(4) 0.1404(4) 0.2500 0.350(8) Uani 1 2 d DS T P . .
C6 C 0.3313(3) 0.1687(3) 0.2500 0.341(8) Uani 1 2 d DS T P . .
C7 C 0.3198(3) 0.1785(3) 0.2141(3) 0.424(6) Uani 1 1 d D . . . .
H7A H 0.3293 0.1685 0.1919 0.508 Uiso 1 1 calc R U . . .
C8 C 0.2932(3) 0.2044(3) 0.2164(2) 0.424(6) Uani 1 1 d D . . . .
H8A H 0.2826 0.2128 0.1940 0.509 Uiso 1 1 calc R U . . .
C9 C 0.27945(17) 0.22055(17) 0.2500 0.420(9) Uani 1 2 d DS T P . .


_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 O1 1.894(6) 28_655 ?
Cu1 O1 1.894(6) 27 ?
Cu1 O1 1.894(6) 2_655 ?
Cu1 O1 1.894(6) . ?
Cu1 O2 2.319(6) . ?
Cu1 Cu1 2.642(3) 13_545 ?
N1 C9 1.478(8) 9 ?
N1 C9 1.478(8) 5 ?
N1 C9 1.478(8) . ?
O1 C1 1.282(5) . ?
C1 O1 1.282(5) 14 ?
C1 C2 1.415(12) . ?
C2 C3 1.366(6) 14 ?
C2 C3 1.366(6) . ?
C3 C4 1.496(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.370(8) . ?
C4 H4A 0.9300 . ?
C5 C4 1.370(8) 14 ?
C5 C6 1.421(14) . ?
C6 C7 1.382(7) 14 ?
C6 C7 1.382(7) . ?
C7 C8 1.320(8) . ?
C7 H7A 0.9300 . ?
C8 C9 1.408(6) . ?
C8 H8A 0.9300 . ?
C9 C8 1.408(6) 14 ?

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 Cu1 O1 166.1(4) 28_655 27 ?
O1 Cu1 O1 89.2(4) 28_655 2_655 ?
O1 Cu1 O1 89.2(4) 27 2_655 ?
O1 Cu1 O1 89.2(4) 28_655 . ?
O1 Cu1 O1 89.2(4) 27 . ?
O1 Cu1 O1 166.2(4) 2_655 . ?
O1 Cu1 O2 96.93(18) 28_655 . ?
O1 Cu1 O2 96.93(18) 27 . ?
O1 Cu1 O2 96.93(18) 2_655 . ?
O1 Cu1 O2 96.92(18) . . ?
O1 Cu1 Cu1 83.07(18) 28_655 13_545 ?
O1 Cu1 Cu1 83.07(18) 27 13_545 ?
O1 Cu1 Cu1 83.07(18) 2_655 13_545 ?
O1 Cu1 Cu1 83.08(18) . 13_545 ?
O2 Cu1 Cu1 180.0 . 13_545 ?
C9 N1 C9 120.0 9 5 ?
C9 N1 C9 120.0 9 . ?
C9 N1 C9 120.000(2) 5 . ?
C1 O1 Cu1 128.5(7) . . ?
O1 C1 O1 116.9(11) 14 . ?
O1 C1 C2 121.6(5) 14 . ?
O1 C1 C2 121.6(5) . . ?
C3 C2 C3 112.0(12) 14 . ?
C3 C2 C1 124.0(6) 14 . ?
C3 C2 C1 124.0(6) . . ?
C2 C3 C4 122.6(10) . . ?
C2 C3 H3A 118.7 . . ?
C4 C3 H3A 118.7 . . ?
C5 C4 C3 128.2(12) . . ?
C5 C4 H4A 115.9 . . ?
C3 C4 H4A 115.9 . . ?
C4 C5 C4 106.4(16) 14 . ?
C4 C5 C6 126.8(8) 14 . ?
C4 C5 C6 126.8(8) . . ?
C7 C6 C7 134.4(15) 14 . ?
C7 C6 C5 112.8(8) 14 . ?
C7 C6 C5 112.8(8) . . ?
C8 C7 C6 109.3(13) . . ?
C8 C7 H7A 125.4 . . ?
C6 C7 H7A 125.4 . . ?
C7 C8 C9 125.6(10) . . ?
C7 C8 H8A 117.2 . . ?
C9 C8 H8A 117.2 . . ?
C8 C9 C8 115.8(10) 14 . ?
C8 C9 N1 122.1(5) 14 . ?
C8 C9 N1 122.1(5) . . ?

_refine_diff_density_max         0.110
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.021

# SQUEEZE RESULTS (Version =  30715)
# 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 -0.003 -0.008 -0.004 39955 6923 '27 DMF molecules per formula unit '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?



_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_chemical_properties_physical    Moisture-sensitive
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_pm3m_a_sqd
_database_code_depnum_ccdc_archive 'CCDC 1480876'
_audit_update_record             
;
2016-05-19 deposited with the CCDC.
2016-08-12 downloaded from the CCDC.
;

_vrf_THETM01_pm3m_a_sqd          
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Because of the weak diffraction of the highly porous crystals
at the higher 2Thetha angles, the dataset was integrated to 2Thetha (max)
23 deg.

;

# SQUEEZE RESULTS
# 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 -0.004 -0.010 -0.004 38676 9958 '38 DMF molecules per formula unit '
_platon_squeeze_details          ?


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        DUT-124
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H48 Cu2 N1.33 O10'
_chemical_formula_weight         1122.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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'
Cu Cu 0.1490 1.8970 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_H-M_alt        'P m -3 n'
_space_group_name_Hall           '-P 4n 2 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   35.400(4)
_cell_length_b                   35.400(4)
_cell_length_c                   35.400(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     44362(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    364
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      21.62

_exptl_crystal_description       octahedron
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.252
_exptl_crystal_F_000             3476
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.288
_shelx_estimated_absorpt_T_min   0.980
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            102331
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.1150
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.449
_diffrn_reflns_theta_max         23.109
_diffrn_reflns_theta_full        23.109
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.948
_reflns_number_total             2666
_reflns_number_gt                2102
_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       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1999P)²+10.3769P] 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         2666
_refine_ls_number_parameters     95
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.1101
_refine_ls_wR_factor_ref         0.3458
_refine_ls_wR_factor_gt          0.3135
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.217
_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 0.0000 0.5000 0.78772(6) 0.1724(13) Uani 1 4 d S T P . .
O1 O 0.03940(15) 0.53921(14) 0.78158(18) 0.202(2) Uani 1 1 d . . . . .
O2 O 0.0000 0.5000 0.8493(3) 0.258(5) Uani 1 4 d S T P . .
N1 N 0.2500 0.7500 0.7500 0.48(3) Uani 1 6 d S T P . .
C1 C 0.0505(2) 0.5505(2) 0.7500 0.183(4) Uani 1 2 d DS TU P . .
C2 C 0.0802(2) 0.5802(2) 0.7500 0.198(3) Uani 1 2 d DS TU P . .
C3 C 0.0958(2) 0.5922(2) 0.7838(3) 0.230(3) Uani 1 1 d D U . . .
H3A H 0.0876 0.5821 0.8066 0.276 Uiso 1 1 calc R U . . .
C4 C 0.1240(2) 0.6193(2) 0.7831(3) 0.257(4) Uani 1 1 d D U . . .
H4A H 0.1351 0.6266 0.8058 0.309 Uiso 1 1 calc R U . . .
C5 C 0.1360(2) 0.6360(2) 0.7500 0.272(4) Uani 1 2 d DS TU P . .
C6 C 0.1655(2) 0.6655(2) 0.7500 0.298(4) Uani 1 2 d DS TU P . .
C7 C 0.1926(3) 0.6671(3) 0.7779(3) 0.333(4) Uani 1 1 d D U . . .
H7A H 0.1929 0.6493 0.7972 0.400 Uiso 1 1 calc R U . . .
C8 C 0.2198(3) 0.6960(3) 0.7768(3) 0.355(4) Uani 1 1 d D U . . .
C9 C 0.2235(3) 0.7235(3) 0.7500 0.362(6) Uani 1 2 d DS TU P . .
C10 C 0.2500 0.6936(3) 0.8064(3) 0.380(6) Uani 1 2 d DS TU P . .
C11 C 0.2695(4) 0.6522(4) 0.8062(4) 0.461(8) Uani 1 1 d D U . . .
H11A H 0.2503 0.6332 0.8077 0.692 Uiso 1 1 calc R U . . .
H11B H 0.2836 0.6490 0.7833 0.692 Uiso 1 1 calc R U . . .
H11C H 0.2862 0.6500 0.8275 0.692 Uiso 1 1 calc R 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 O1 1.980(5) 2_565 ?
Cu1 O1 1.980(5) 28 ?
Cu1 O1 1.980(5) 27_565 ?
Cu1 O1 1.980(5) . ?
Cu1 O2 2.180(12) . ?
Cu1 Cu1 2.671(4) 13_456 ?
O1 C1 1.250(6) . ?
N1 C9 1.324(13) 10_656 ?
N1 C9 1.324(13) 7_665 ?
N1 C9 1.324(13) . ?
C1 O1 1.250(6) 13_456 ?
C1 C2 1.489(13) . ?
C2 C3 1.385(8) . ?
C2 C3 1.385(8) 13_456 ?
C3 C4 1.384(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.381(8) . ?
C4 H4A 0.9300 . ?
C5 C4 1.381(8) 13_456 ?
C5 C6 1.476(12) . ?
C6 C7 1.377(8) 13_456 ?
C6 C7 1.378(8) . ?
C7 C8 1.406(10) . ?
C7 H7A 0.9300 . ?
C8 C9 1.368(9) . ?
C8 C10 1.500(10) . ?
C9 C8 1.368(9) 13_456 ?
C10 C8 1.500(10) 19_566 ?
C10 C11 1.618(12) 19_566 ?
C10 C11 1.618(12) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?

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 Cu1 O1 89.0(3) 2_565 28 ?
O1 Cu1 O1 89.6(3) 2_565 27_565 ?
O1 Cu1 O1 167.4(4) 28 27_565 ?
O1 Cu1 O1 167.4(4) 2_565 . ?
O1 Cu1 O1 89.6(3) 28 . ?
O1 Cu1 O1 89.0(3) 27_565 . ?
O1 Cu1 O2 96.3(2) 2_565 . ?
O1 Cu1 O2 96.3(2) 28 . ?
O1 Cu1 O2 96.3(2) 27_565 . ?
O1 Cu1 O2 96.3(2) . . ?
O1 Cu1 Cu1 83.7(2) 2_565 13_456 ?
O1 Cu1 Cu1 83.7(2) 28 13_456 ?
O1 Cu1 Cu1 83.7(2) 27_565 13_456 ?
O1 Cu1 Cu1 83.7(2) . 13_456 ?
O2 Cu1 Cu1 180.0 . 13_456 ?
C1 O1 Cu1 122.9(7) . . ?
C9 N1 C9 120.000(3) 10_656 7_665 ?
C9 N1 C9 119.999(3) 10_656 . ?
C9 N1 C9 120.001(3) 7_665 . ?
O1 C1 O1 126.9(12) . 13_456 ?
O1 C1 C2 116.6(6) . . ?
O1 C1 C2 116.6(6) 13_456 . ?
C3 C2 C3 120.1(11) . 13_456 ?
C3 C2 C1 119.9(5) . . ?
C3 C2 C1 119.9(5) 13_456 . ?
C4 C3 C2 119.1(9) . . ?
C4 C3 H3A 120.5 . . ?
C2 C3 H3A 120.5 . . ?
C5 C4 C3 122.2(9) . . ?
C5 C4 H4A 118.9 . . ?
C3 C4 H4A 118.9 . . ?
C4 C5 C4 117.2(11) 13_456 . ?
C4 C5 C6 121.4(5) 13_456 . ?
C4 C5 C6 121.4(5) . . ?
C7 C6 C7 117.1(10) 13_456 . ?
C7 C6 C5 121.4(5) 13_456 . ?
C7 C6 C5 121.4(5) . . ?
C6 C7 C8 119.2(9) . . ?
C6 C7 H7A 120.4 . . ?
C8 C7 H7A 120.4 . . ?
C9 C8 C7 127.2(9) . . ?
C9 C8 C10 117.1(9) . . ?
C7 C8 C10 115.4(8) . . ?
N1 C9 C8 125.0(6) . . ?
N1 C9 C8 125.0(6) . 13_456 ?
C8 C9 C8 110.1(11) . 13_456 ?
C8 C10 C8 115.4(12) 19_566 . ?
C8 C10 C11 110.6(7) 19_566 19_566 ?
C8 C10 C11 109.1(7) . 19_566 ?
C8 C10 C11 109.1(7) 19_566 . ?
C8 C10 C11 110.6(7) . . ?
C11 C10 C11 100.9(15) 19_566 . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_refine_diff_density_max         0.262
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.030


_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_chemical_properties_physical    Moisture-sensitive
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_pm3n_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1480877'
_audit_update_record             
;
2016-05-19 deposited with the CCDC.
2016-08-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_pm3n_a_sq           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Because of the absence of meaningful intensities at the
higher Theta angles, the dataset was integrated to a slightly lower
value of sine(theta_max)/wavelength
;
_vrf_PLAT213_pm3n_a_sq           
;
PROBLEM: Atom O2              has ADP max/min Ratio .....        5.9 oblate
RESPONSE: The atom O2 is disordered near the special position and is common
for both parts. Since the second part cannot be localized from the residual
electron density map because of lower occupancy, atom O2 is not splitted into
two positions.
;
_vrf_PLAT241_pm3n_a_sq           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O2 Check 
RESPONSE: The high difference Ueq of O2 compared to neibours is caused by
unresolved disorder
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        DUT-125
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H48 Cu3 N5.33 O10'
_chemical_formula_weight         1290.40


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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'
Cu Cu 0.1490 1.8970 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_H-M_alt        'P m -3 n'
_space_group_name_Hall           '-P 4n 2 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   35.510(4)
_cell_length_b                   35.510(4)
_cell_length_c                   35.510(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     44777(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    685
_cell_measurement_theta_min      3.98
_cell_measurement_theta_max      25.34

_exptl_crystal_description       cubic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.287
_exptl_crystal_F_000             3962
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.418
_shelx_estimated_absorpt_T_min   0.979
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.89500
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            94817
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.021
_diffrn_reflns_theta_max         28.101
_diffrn_reflns_theta_full        28.101
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4827
_reflns_number_gt                3267
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1584P)²+4.8475P] 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         4827
_refine_ls_number_parameters     127
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0673
_refine_ls_wR_factor_ref         0.2455
_refine_ls_wR_factor_gt          0.1999
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.138
_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
Cu1 Cu 0.0000 0.5000 0.71224(2) 0.0701(4) Uani 1 4 d S T P . .
O1 O 0.03881(6) 0.53873(6) 0.71846(6) 0.0965(8) Uani 1 1 d . . . . .
C1 C 0.05043(10) 0.55043(10) 0.7500 0.0875(13) Uani 1 2 d S T P . .
C2 C 0.08019(9) 0.58019(9) 0.7500 0.0992(14) Uani 1 2 d S T P . .
C3 C 0.09576(14) 0.59303(13) 0.78274(11) 0.158(2) Uani 1 1 d . . . . .
H3A H 0.0880 0.5828 0.8056 0.190 Uiso 1 1 calc R U . . .
C4 C 0.12315(15) 0.62115(15) 0.78250(12) 0.180(3) Uani 1 1 d . . . . .
H4A H 0.1327 0.6297 0.8053 0.216 Uiso 1 1 calc R U . . .
C5 C 0.13643(12) 0.63643(12) 0.7500 0.136(2) Uani 1 2 d S T P . .
C6 C 0.16615(12) 0.66615(12) 0.7500 0.158(3) Uani 1 2 d S T P . .
C7 C 0.17812(17) 0.68228(17) 0.78259(14) 0.200(3) Uani 1 1 d . . . . .
H7A H 0.1678 0.6746 0.8054 0.239 Uiso 1 1 calc R U . . .
C8 C 0.20539(18) 0.71002(18) 0.78218(16) 0.215(4) Uani 1 1 d . . . . .
H8A H 0.2128 0.7211 0.8047 0.258 Uiso 1 1 calc R U . . .
C9 C 0.22125(13) 0.72125(13) 0.7500 0.188(4) Uani 1 2 d S T P . .
N1 N 0.2500 0.7500 0.7500 0.233(8) Uani 1 6 d S T P . .
Cu2 Cu 0.02462(12) 0.5000 0.5000 0.146(2) Uani 0.32 4 d DS T P . .
N2 N 0.0000 0.5000 0.65282(13) 0.1033(18) Uani 1 4 d DS TU P . .
C12 C 0.0000 0.5000 0.5744(2) 0.258(7) Uani 1 4 d DS TU P . .
O2 O 0.0000 0.5000 0.53822(13) 0.341(7) Uani 1 4 d DS TU P . .
C10 C 0.0303(2) 0.5000 0.63334(18) 0.195(5) Uani 0.64 2 d DS TU P . .
H10A H 0.0532 0.5000 0.6461 0.234 Uiso 0.64 2 calc R U P . .
C11 C 0.0311(2) 0.5000 0.5932(2) 0.277(7) Uani 0.64 2 d DS TU P . .
C13 C 0.0690(4) 0.5000 0.5754(3) 0.424(11) Uani 0.64 2 d DS TU P . .
H13A H 0.0919 0.5000 0.5881 0.508 Uiso 0.64 2 calc R U P . .
N3 N 0.0643(5) 0.5000 0.5363(3) 0.511(12) Uani 0.64 2 d DS TU P . .
C14 C 0.1029(5) 0.5000 0.5199(2) 0.561(16) Uani 0.64 2 d DS TU P . .
H14A H 0.1163 0.5221 0.5288 0.673 Uiso 0.32 1 calc R U P . .
H14B H 0.1163 0.4779 0.5288 0.673 Uiso 0.32 1 calc R U P . .
Cu3 Cu 0.0000 0.5265(3) 0.5000 0.167(5) Uani 0.18 4 d DS T P . .


_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 O1 1.959(2) 2_565 ?
Cu1 O1 1.959(2) 28 ?
Cu1 O1 1.959(2) 27_565 ?
Cu1 O1 1.959(2) . ?
Cu1 N2 2.110(5) . ?
Cu1 Cu1 2.6813(11) 13_456 ?
O1 C1 1.264(3) . ?
C1 O1 1.264(3) 13_456 ?
C1 C2 1.495(6) . ?
C2 C3 1.366(4) . ?
C2 C3 1.366(4) 13_456 ?
C3 C4 1.394(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.360(5) . ?
C4 H4A 0.9300 . ?
C5 C4 1.360(5) 13_456 ?
C5 C6 1.492(8) . ?
C6 C7 1.359(5) . ?
C6 C7 1.359(5) 13_456 ?
C7 C8 1.381(6) . ?
C7 H7A 0.9300 . ?
C8 C9 1.335(6) . ?
C8 H8A 0.9300 . ?
C9 C8 1.335(6) 13_456 ?
C9 N1 1.444(7) . ?
N1 C9 1.444(7) 10_656 ?
N1 C9 1.444(7) 7_665 ?
Cu2 Cu3 1.285(6) 25_566 ?
Cu2 Cu3 1.285(6) . ?
Cu2 O2 1.614(5) 25_566 ?
Cu2 O2 1.614(5) . ?
Cu2 Cu2 1.748(9) 25_566 ?
Cu2 N3 1.910(15) . ?
Cu2 N3 1.910(15) 26_556 ?
N2 C10 1.279(7) 2_565 ?
N2 C10 1.279(7) . ?
C12 O2 1.284(9) . ?
C12 C11 1.289(9) . ?
C12 C11 1.289(9) 2_565 ?
O2 Cu2 1.614(5) 25_566 ?
O2 Cu3 1.652(6) 25_566 ?
O2 Cu3 1.652(6) . ?
C10 C11 1.426(9) . ?
C10 H10A 0.9300 . ?
C11 C13 1.488(13) . ?
C13 N3 1.396(13) . ?
C13 H13A 0.9300 . ?
N3 C14 1.490(15) . ?
C14 C14 1.414(16) 26_556 ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
Cu3 Cu2 1.285(6) 25_566 ?
Cu3 O2 1.652(6) 25_566 ?
Cu3 Cu3 1.885(19) 25_566 ?

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 Cu1 O1 89.15(13) 2_565 28 ?
O1 Cu1 O1 89.39(13) 2_565 27_565 ?
O1 Cu1 O1 167.06(12) 28 27_565 ?
O1 Cu1 O1 167.06(12) 2_565 . ?
O1 Cu1 O1 89.39(14) 28 . ?
O1 Cu1 O1 89.15(13) 27_565 . ?
O1 Cu1 N2 96.47(6) 2_565 . ?
O1 Cu1 N2 96.47(6) 28 . ?
O1 Cu1 N2 96.47(6) 27_565 . ?
O1 Cu1 N2 96.47(6) . . ?
O1 Cu1 Cu1 83.53(6) 2_565 13_456 ?
O1 Cu1 Cu1 83.53(6) 28 13_456 ?
O1 Cu1 Cu1 83.53(6) 27_565 13_456 ?
O1 Cu1 Cu1 83.53(6) . 13_456 ?
N2 Cu1 Cu1 180.0 . 13_456 ?
C1 O1 Cu1 124.1(2) . . ?
O1 C1 O1 124.8(4) . 13_456 ?
O1 C1 C2 117.6(2) . . ?
O1 C1 C2 117.6(2) 13_456 . ?
C3 C2 C3 117.0(5) . 13_456 ?
C3 C2 C1 121.5(3) . . ?
C3 C2 C1 121.5(3) 13_456 . ?
C2 C3 C4 121.1(4) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 122.2(4) . . ?
C5 C4 H4A 118.9 . . ?
C3 C4 H4A 118.9 . . ?
C4 C5 C4 116.3(6) . 13_456 ?
C4 C5 C6 121.8(3) . . ?
C4 C5 C6 121.8(3) 13_456 . ?
C7 C6 C7 117.5(6) . 13_456 ?
C7 C6 C5 121.3(3) . . ?
C7 C6 C5 121.3(3) 13_456 . ?
C6 C7 C8 120.7(5) . . ?
C6 C7 H7A 119.6 . . ?
C8 C7 H7A 119.6 . . ?
C9 C8 C7 121.2(6) . . ?
C9 C8 H8A 119.4 . . ?
C7 C8 H8A 119.4 . . ?
C8 C9 C8 118.7(7) . 13_456 ?
C8 C9 N1 120.6(3) . . ?
C8 C9 N1 120.6(3) 13_456 . ?
C9 N1 C9 120.000(1) 10_656 7_665 ?
C9 N1 C9 120.000(1) 10_656 . ?
C9 N1 C9 120.000(1) 7_665 . ?
Cu3 Cu2 Cu3 94.3(8) 25_566 . ?
Cu3 Cu2 O2 68.4(2) 25_566 25_566 ?
Cu3 Cu2 O2 68.4(2) . 25_566 ?
Cu3 Cu2 O2 68.4(2) 25_566 . ?
Cu3 Cu2 O2 68.4(2) . . ?
O2 Cu2 O2 114.4(3) 25_566 . ?
Cu3 Cu2 Cu2 47.1(4) 25_566 25_566 ?
Cu3 Cu2 Cu2 47.1(4) . 25_566 ?
O2 Cu2 Cu2 57.22(16) 25_566 25_566 ?
O2 Cu2 Cu2 57.22(16) . 25_566 ?
Cu3 Cu2 N3 120.1(3) 25_566 . ?
Cu3 Cu2 N3 120.1(3) . . ?
O2 Cu2 N3 165.3(4) 25_566 . ?
O2 Cu2 N3 80.3(4) . . ?
Cu2 Cu2 N3 137.5(4) 25_566 . ?
Cu3 Cu2 N3 120.1(3) 25_566 26_556 ?
Cu3 Cu2 N3 120.1(3) . 26_556 ?
O2 Cu2 N3 80.3(4) 25_566 26_556 ?
O2 Cu2 N3 165.3(4) . 26_556 ?
Cu2 Cu2 N3 137.5(4) 25_566 26_556 ?
N3 Cu2 N3 85.0(8) . 26_556 ?
C10 N2 C10 114.5(7) 2_565 . ?
C10 N2 Cu1 122.8(4) 2_565 . ?
C10 N2 Cu1 122.8(4) . . ?
O2 C12 C11 121.2(4) . . ?
O2 C12 C11 121.2(4) . 2_565 ?
C11 C12 C11 117.6(9) . 2_565 ?
C12 O2 Cu2 147.22(16) . 25_566 ?
C12 O2 Cu2 147.22(16) . . ?
Cu2 O2 Cu2 65.6(3) 25_566 . ?
C12 O2 Cu3 145.2(3) . 25_566 ?
Cu2 O2 Cu3 46.32(19) 25_566 25_566 ?
Cu2 O2 Cu3 46.32(19) . 25_566 ?
C12 O2 Cu3 145.2(3) . . ?
Cu2 O2 Cu3 46.32(19) 25_566 . ?
Cu2 O2 Cu3 46.32(19) . . ?
Cu3 O2 Cu3 69.5(6) 25_566 . ?
N2 C10 C11 123.9(6) . . ?
N2 C10 H10A 118.1 . . ?
C11 C10 H10A 118.1 . . ?
C12 C11 C10 120.1(6) . . ?
C12 C11 C13 123.6(8) . . ?
C10 C11 C13 116.3(7) . . ?
N3 C13 C11 108.3(13) . . ?
N3 C13 H13A 125.8 . . ?
C11 C13 H13A 125.8 . . ?
C13 N3 C14 106.2(12) . . ?
C13 N3 Cu2 139.4(12) . . ?
C14 N3 Cu2 114.5(8) . . ?
C14 C14 N3 113.0(6) 26_556 . ?
C14 C14 H14A 109.0 26_556 . ?
N3 C14 H14A 109.0 . . ?
C14 C14 H14B 109.0 26_556 . ?
N3 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
Cu2 Cu3 Cu2 85.7(8) 25_566 . ?
Cu2 Cu3 O2 65.3(3) 25_566 25_566 ?
Cu2 Cu3 O2 65.3(3) . 25_566 ?
Cu2 Cu3 O2 65.3(3) 25_566 . ?
Cu2 Cu3 O2 65.3(3) . . ?
O2 Cu3 O2 110.5(6) 25_566 . ?
Cu2 Cu3 Cu3 42.9(4) 25_566 25_566 ?
Cu2 Cu3 Cu3 42.9(4) . 25_566 ?
O2 Cu3 Cu3 55.2(3) 25_566 25_566 ?
O2 Cu3 Cu3 55.2(3) . 25_566 ?

_refine_diff_density_max         0.370
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.048



_exptl_crystal_recrystallization_method 'post-synthetic functionalization'
_chemical_properties_physical    Moisture-sensitive
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_DUT-128
_database_code_depnum_ccdc_archive 'CCDC 1480878'
_audit_update_record             
;
2016-05-19 deposited with the CCDC.
2016-08-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_DUT-128             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The dataset was measured to 2Thetha (max) of 22.5 deg. because
of poor scattering of the single crystal. 
;
_vrf_PLAT213_DUT-128             
;
PROBLEM: Atom O2              has ADP max/min Ratio .....        7.7 prolat
RESPONSE: Large ADP max/min ratios are explained by unresolved disorder 
and room temperature measurement
;
_vrf_PLAT241_DUT-128             
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O2 Check 
RESPONSE: High Ueq of the O2 is due to the unresolved disorder at the
special position
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        DUT-128
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C82 H64 Cu3 N7.33 O10'
_chemical_formula_weight         1502.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.1490 1.8970 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_H-M_alt        'P m -3 n'
_space_group_name_Hall           '-P 4n 2 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   35.490(4)
_cell_length_b                   35.490(4)
_cell_length_c                   35.490(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     44701(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    213
_cell_measurement_theta_min      3.65
_cell_measurement_theta_max      19.43

_exptl_crystal_description       cubic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.335
_exptl_crystal_F_000             4646
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.423
_shelx_estimated_absorpt_T_min   0.987
_shelx_estimated_absorpt_T_max   0.992
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.89500
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            23231
_diffrn_reflns_av_unetI/netI     0.1113
_diffrn_reflns_av_R_equivalents  0.2472
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.022
_diffrn_reflns_theta_max         22.511
_diffrn_reflns_theta_full        22.511
_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             2632
_reflns_number_gt                1493
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1800P)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         2632
_refine_ls_number_parameters     141
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.0998
_refine_ls_wR_factor_ref         0.3243
_refine_ls_wR_factor_gt          0.2748
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.205
_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 0.28769(5) 0.5000 1.0000 0.0516(9) Uani 1 4 d S T P . .
Cu2A Cu 0.5000 0.5256(2) 1.0000 0.142(4) Uani 0.32 4 d S T P A .
Cu2B Cu 0.5000 0.5000 1.0203(7) 0.142(4) Uani 0.18 4 d S T P A .
N1 N 0.2500 0.2500 0.7500 0.192(15) Uani 1 6 d DS T P . .
N2 N 0.3484(3) 0.5000 1.0000 0.111(6) Uani 1 4 d DS TU P . .
O1 O 0.28152(14) 0.46077(16) 0.96102(16) 0.0738(19) Uani 1 1 d . . . . .
C1 C 0.2500 0.4503(3) 0.9503(3) 0.073(3) Uani 1 2 d S TU P . .
C2 C 0.2500 0.4196(3) 0.9196(3) 0.089(4) Uani 1 2 d DS TU P . .
C3 C 0.2164(2) 0.4064(3) 0.9053(3) 0.119(3) Uani 1 1 d D U . . .
H3A H 0.1937 0.4159 0.9142 0.143 Uiso 1 1 calc R U . . .
C4 C 0.2169(2) 0.3788(3) 0.8778(3) 0.148(4) Uani 1 1 d D U . . .
H4A H 0.1940 0.3700 0.8683 0.178 Uiso 1 1 calc R U . . .
C5 C 0.2500 0.3637(3) 0.8637(3) 0.151(5) Uani 1 2 d S TU P . .
C6 C 0.2500 0.3338(3) 0.8338(3) 0.178(6) Uani 1 2 d DS TU P . .
C7 C 0.2225(3) 0.3328(4) 0.8065(4) 0.212(5) Uani 1 1 d D U . . .
H7A H 0.2046 0.3519 0.8055 0.254 Uiso 1 1 calc R U . . .
C8 C 0.2211(4) 0.3036(4) 0.7804(4) 0.235(6) Uani 1 1 d D U . . .
C9 C 0.2500 0.2783(3) 0.7783(3) 0.225(8) Uani 1 2 d DS TU P . .
C10 C 0.1923(4) 0.3077(4) 0.7500 0.262(8) Uani 1 2 d DS TU P . .
C13 C 0.3664(4) 0.4682(3) 1.0000 0.222(9) Uani 1 2 d DS TU P A .
H13A H 0.3532 0.4455 1.0000 0.267 Uiso 1 2 calc R U P . .
C14 C 0.4046(4) 0.4680(3) 1.0000 0.332(11) Uani 1 2 d DS TU P . .
C15 C 0.4243(5) 0.5000 1.0000 0.349(13) Uani 1 4 d DS TU P A .
O2 O 0.4617(5) 0.5000 1.0000 0.402(13) Uani 1 4 d DS TU P . .
C16 C 0.4222(7) 0.4333(8) 0.9822(14) 0.433(14) Uani 0.5 1 d D U P A -1
H16A H 0.4122 0.4154 0.9659 0.520 Uiso 0.5 1 calc R U P A -1
N3 N 0.4631(7) 0.4370(10) 1.0000 0.524(14) Uani 1 2 d DS TU P . .
C17 C 0.4794(3) 0.3955(10) 1.0000 0.58(2) Uani 1 2 d DS TU P . .
H17A H 0.4704 0.3823 1.0221 0.692 Uiso 0.5 1 calc R U P . .
H17B H 0.4704 0.3823 0.9779 0.692 Uiso 0.5 1 calc R U P . .
C11 C 0.1525(5) 0.3065(5) 0.7690(5) 0.344(11) Uani 1 1 d D U . . .
H11A H 0.1334 0.3091 0.7501 0.516 Uiso 1 1 calc R U . . .
H11B H 0.1494 0.2830 0.7819 0.516 Uiso 1 1 calc R U . . .
H11C H 0.1504 0.3268 0.7868 0.516 Uiso 1 1 calc R 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 O1 1.975(5) . ?
Cu1 O1 1.975(5) 4_567 ?
Cu1 O1 1.975(5) 27_565 ?
Cu1 O1 1.975(5) 26_557 ?
Cu1 N2 2.153(12) . ?
Cu1 Cu1 2.675(3) 41_676 ?
Cu2A Cu2B 1.160(15) . ?
Cu2A Cu2B 1.160(15) 25_667 ?
Cu2A O2 1.635(14) . ?
Cu2A O2 1.635(14) 25_667 ?
Cu2A N3 1.86(3) 25_667 ?
Cu2A N3 1.86(3) 27_565 ?
Cu2A Cu2A 1.819(15) 25_667 ?
Cu2A C17 2.89(3) 25_667 ?
Cu2A C17 2.89(3) 27_565 ?
Cu2B Cu2A 1.160(15) 25_667 ?
Cu2B O2 1.537(19) . ?
Cu2B O2 1.537(19) 25_667 ?
Cu2B Cu2B 1.44(5) 25_667 ?
Cu2B N3 2.69(3) 25_667 ?
Cu2B N3 2.69(3) 3_657 ?
Cu2B N3 2.69(3) 27_565 ?
Cu2B N3 2.69(3) . ?
N1 C9 1.422(13) . ?
N1 C9 1.422(13) 8_656 ?
N1 C9 1.422(13) 11_566 ?
N2 C13 1.299(12) 27_565 ?
N2 C13 1.299(12) . ?
O1 C1 1.239(7) . ?
C1 O1 1.239(7) 18_545 ?
C1 C2 1.537(17) . ?
C2 C3 1.378(8) . ?
C2 C3 1.378(8) 18_545 ?
C3 C4 1.385(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.385(11) . ?
C4 H4A 0.9300 . ?
C5 C4 1.385(11) 18_545 ?
C5 C6 1.50(2) . ?
C6 C7 1.376(10) . ?
C6 C7 1.376(10) 18_545 ?
C7 C8 1.393(12) . ?
C7 H7A 0.9300 . ?
C8 C9 1.365(10) . ?
C8 C10 1.492(12) . ?
C9 C8 1.365(10) 18_545 ?
C10 C11 1.565(14) . ?
C10 C11 1.565(14) 14_556 ?
C10 C8 1.492(12) 14_556 ?
C13 C14 1.356(15) . ?
C13 H13A 0.9300 . ?
C14 C15 1.335(11) . ?
C14 C16 1.518(18) . ?
C15 O2 1.327(16) . ?
C15 C14 1.335(11) 27_565 ?
O2 Cu2B 1.537(19) 25_667 ?
O2 Cu2A 1.635(14) 25_667 ?
C16 N3 1.587(18) . ?
C16 H16A 0.9300 . ?
N3 C17 1.581(18) . ?
N3 Cu2A 1.86(3) 25_667 ?
N3 Cu2B 2.69(3) 25_667 ?
C17 C17 1.462(19) 3_657 ?
C17 Cu2A 2.89(3) 25_667 ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?

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 Cu1 O1 167.3(3) . 4_567 ?
O1 Cu1 O1 89.7(4) . 27_565 ?
O1 Cu1 O1 88.9(4) 4_567 27_565 ?
O1 Cu1 O1 88.9(4) . 26_557 ?
O1 Cu1 O1 89.7(4) 4_567 26_557 ?
O1 Cu1 O1 167.3(3) 27_565 26_557 ?
O1 Cu1 N2 96.37(15) . . ?
O1 Cu1 N2 96.37(15) 4_567 . ?
O1 Cu1 N2 96.37(15) 27_565 . ?
O1 Cu1 N2 96.37(15) 26_557 . ?
O1 Cu1 Cu1 83.63(15) . 41_676 ?
O1 Cu1 Cu1 83.63(15) 4_567 41_676 ?
O1 Cu1 Cu1 83.63(15) 27_565 41_676 ?
O1 Cu1 Cu1 83.63(15) 26_557 41_676 ?
N2 Cu1 Cu1 180.0 . 41_676 ?
Cu2B Cu2A Cu2B 77(2) . 25_667 ?
Cu2B Cu2A O2 64.1(6) . . ?
Cu2B Cu2A O2 64.1(6) 25_667 . ?
Cu2B Cu2A O2 64.1(6) . 25_667 ?
Cu2B Cu2A O2 64.1(6) 25_667 25_667 ?
O2 Cu2A O2 112.4(8) . 25_667 ?
Cu2B Cu2A N3 123.9(8) . 25_667 ?
Cu2B Cu2A N3 123.9(8) 25_667 25_667 ?
O2 Cu2A N3 168.5(10) . 25_667 ?
O2 Cu2A N3 79.1(9) 25_667 25_667 ?
Cu2B Cu2A N3 123.9(8) . 27_565 ?
Cu2B Cu2A N3 123.9(8) 25_667 27_565 ?
O2 Cu2A N3 79.1(9) . 27_565 ?
O2 Cu2A N3 168.5(10) 25_667 27_565 ?
N3 Cu2A N3 89.3(17) 25_667 27_565 ?
Cu2B Cu2A Cu2A 38.3(11) . 25_667 ?
Cu2B Cu2A Cu2A 38.3(11) 25_667 25_667 ?
O2 Cu2A Cu2A 56.2(4) . 25_667 ?
O2 Cu2A Cu2A 56.2(4) 25_667 25_667 ?
N3 Cu2A Cu2A 135.3(9) 25_667 25_667 ?
N3 Cu2A Cu2A 135.3(9) 27_565 25_667 ?
Cu2B Cu2A C17 139.4(10) . 25_667 ?
Cu2B Cu2A C17 139.4(10) 25_667 25_667 ?
O2 Cu2A C17 138.4(5) . 25_667 ?
O2 Cu2A C17 109.2(5) 25_667 25_667 ?
N3 Cu2A C17 30.0(7) 25_667 25_667 ?
N3 Cu2A C17 59.3(10) 27_565 25_667 ?
Cu2A Cu2A C17 165.4(3) 25_667 25_667 ?
Cu2B Cu2A C17 139.4(10) . 27_565 ?
Cu2B Cu2A C17 139.4(10) 25_667 27_565 ?
O2 Cu2A C17 109.2(5) . 27_565 ?
O2 Cu2A C17 138.4(5) 25_667 27_565 ?
N3 Cu2A C17 59.3(10) 25_667 27_565 ?
N3 Cu2A C17 30.0(8) 27_565 27_565 ?
Cu2A Cu2A C17 165.4(3) 25_667 27_565 ?
C17 Cu2A C17 29.3(5) 25_667 27_565 ?
Cu2A Cu2B Cu2A 103(2) . 25_667 ?
Cu2A Cu2B O2 73.1(9) . . ?
Cu2A Cu2B O2 73.1(9) 25_667 . ?
Cu2A Cu2B O2 73.1(9) . 25_667 ?
Cu2A Cu2B O2 73.1(9) 25_667 25_667 ?
O2 Cu2B O2 124.2(17) . 25_667 ?
Cu2A Cu2B Cu2B 51.7(11) . 25_667 ?
Cu2A Cu2B Cu2B 51.7(11) 25_667 25_667 ?
O2 Cu2B Cu2B 62.1(9) . 25_667 ?
O2 Cu2B Cu2B 62.1(9) 25_667 25_667 ?
Cu2A Cu2B N3 35.1(4) . 25_667 ?
Cu2A Cu2B N3 119.1(14) 25_667 25_667 ?
O2 Cu2B N3 107.8(8) . 25_667 ?
O2 Cu2B N3 56.2(6) 25_667 25_667 ?
Cu2B Cu2B N3 74.5(5) 25_667 25_667 ?
Cu2A Cu2B N3 119.1(14) . 3_657 ?
Cu2A Cu2B N3 35.1(4) 25_667 3_657 ?
O2 Cu2B N3 107.8(8) . 3_657 ?
O2 Cu2B N3 56.2(6) 25_667 3_657 ?
Cu2B Cu2B N3 74.5(5) 25_667 3_657 ?
N3 Cu2B N3 112.5(11) 25_667 3_657 ?
Cu2A Cu2B N3 35.1(4) . 27_565 ?
Cu2A Cu2B N3 119.1(14) 25_667 27_565 ?
O2 Cu2B N3 56.2(6) . 27_565 ?
O2 Cu2B N3 107.8(8) 25_667 27_565 ?
Cu2B Cu2B N3 74.5(5) 25_667 27_565 ?
N3 Cu2B N3 58.3(11) 25_667 27_565 ?
N3 Cu2B N3 149.0(11) 3_657 27_565 ?
Cu2A Cu2B N3 119.1(14) . . ?
Cu2A Cu2B N3 35.1(4) 25_667 . ?
O2 Cu2B N3 56.2(6) . . ?
O2 Cu2B N3 107.8(8) 25_667 . ?
Cu2B Cu2B N3 74.5(6) 25_667 . ?
N3 Cu2B N3 149.0(11) 25_667 . ?
N3 Cu2B N3 58.3(11) 3_657 . ?
N3 Cu2B N3 112.5(11) 27_565 . ?
C9 N1 C9 120.000(2) . 8_656 ?
C9 N1 C9 120.000(3) . 11_566 ?
C9 N1 C9 120.000(2) 8_656 11_566 ?
C13 N2 C13 120.9(12) 27_565 . ?
C13 N2 Cu1 119.6(6) 27_565 . ?
C13 N2 Cu1 119.6(6) . . ?
C1 O1 Cu1 121.9(7) . . ?
O1 C1 O1 129.0(13) 18_545 . ?
O1 C1 C2 115.5(6) 18_545 . ?
O1 C1 C2 115.5(6) . . ?
C3 C2 C3 119.7(12) . 18_545 ?
C3 C2 C1 120.1(6) . . ?
C3 C2 C1 120.1(6) 18_545 . ?
C2 C3 C4 119.5(8) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 122.5(8) . . ?
C3 C4 H4A 118.8 . . ?
C5 C4 H4A 118.8 . . ?
C4 C5 C4 116.3(13) 18_545 . ?
C4 C5 C6 121.9(7) 18_545 . ?
C4 C5 C6 121.9(7) . . ?
C7 C6 C7 117.9(13) . 18_545 ?
C7 C6 C5 121.0(7) . . ?
C7 C6 C5 121.0(7) 18_545 . ?
C6 C7 C8 120.9(8) . . ?
C6 C7 H7A 119.6 . . ?
C8 C7 H7A 119.6 . . ?
C9 C8 C7 119.9(8) . . ?
C9 C8 C10 122.7(12) . . ?
C7 C8 C10 115.7(9) . . ?
C8 C9 C8 119.7(13) . 18_545 ?
C8 C9 N1 120.2(6) . . ?
C8 C9 N1 120.2(6) 18_545 . ?
C11 C10 C8 107.7(10) . . ?
C11 C10 C11 104(2) . 14_556 ?
C8 C10 C11 112.4(10) . 14_556 ?
C11 C10 C8 112.4(10) . 14_556 ?
C8 C10 C8 112.8(16) . 14_556 ?
C11 C10 C8 107.7(10) 14_556 14_556 ?
N2 C13 C14 119.9(8) . . ?
N2 C13 H13A 120.1 . . ?
C14 C13 H13A 120.1 . . ?
C15 C14 C13 121.3(11) . . ?
C15 C14 C16 118.4(16) . . ?
C13 C14 C16 114.5(12) . . ?
O2 C15 C14 121.6(9) . . ?
O2 C15 C14 121.6(9) . 27_565 ?
C14 C15 C14 116.8(18) . 27_565 ?
C15 O2 Cu2B 152.1(9) . . ?
C15 O2 Cu2B 152.1(9) . 25_667 ?
Cu2B O2 Cu2B 55.8(17) . 25_667 ?
C15 O2 Cu2A 146.2(4) . . ?
Cu2B O2 Cu2A 42.7(6) . . ?
Cu2B O2 Cu2A 42.7(6) 25_667 . ?
C15 O2 Cu2A 146.2(4) . 25_667 ?
Cu2B O2 Cu2A 42.7(6) . 25_667 ?
Cu2B O2 Cu2A 42.7(6) 25_667 25_667 ?
Cu2A O2 Cu2A 67.6(8) . 25_667 ?
C14 C16 N3 98(2) . . ?
C14 C16 H16A 130.9 . . ?
N3 C16 H16A 130.9 . . ?
C17 N3 C16 105(2) . . ?
C17 N3 Cu2A 113.8(17) . 25_667 ?
C16 N3 Cu2A 135(2) . 25_667 ?
C17 N3 Cu2B 126.5(14) . . ?
C16 N3 Cu2B 128(2) . . ?
Cu2A N3 Cu2B 21.0(5) 25_667 . ?
C17 N3 Cu2B 126.5(14) . 25_667 ?
C16 N3 Cu2B 114(2) . 25_667 ?
Cu2A N3 Cu2B 21.0(5) 25_667 25_667 ?
Cu2B N3 Cu2B 31.0(11) . 25_667 ?
C17 C17 N3 111.5(11) 3_657 . ?
C17 C17 Cu2A 75.4(2) 3_657 25_667 ?
N3 C17 Cu2A 36.1(11) . 25_667 ?
C17 C17 H17A 109.3 3_657 . ?
N3 C17 H17A 109.3 . . ?
Cu2A C17 H17A 123.6 25_667 . ?
C17 C17 H17B 109.3 3_657 . ?
N3 C17 H17B 109.3 . . ?
Cu2A C17 H17B 123.6 25_667 . ?
H17A C17 H17B 108.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_refine_diff_density_max         0.526
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.056



_exptl_crystal_recrystallization_method 'post-synthetic functionalization'
_chemical_properties_physical    Moisture-sensitive
_refine_special_details          SQUEEZE
