# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_tt41b
_database_code_depnum_ccdc_archive 'CCDC 1523579'
_audit_update_record             
;
2017-03-11 deposited with the CCDC.
2017-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/8
_shelx_SHELXL_version_number     2014/8
_chemical_name_systematic        T41b
_chemical_name_common            NTU-141
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C61 H40 Cu2 N12 O10'
_chemical_formula_weight         1228.13

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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_H-M_alt        'P 42 21 2'
_space_group_name_Hall           'P 4n 2n'

_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'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, z'
'-y, -x, -z'
'y, x, -z'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   16.0604(4)
_cell_length_b                   16.0604(4)
_cell_length_c                   44.1170(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11379.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    374
_cell_measurement_theta_min      3.28
_cell_measurement_theta_max      71.59

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.717
_exptl_crystal_F_000             2512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.106
_exptl_absorpt_coefficient_mu    0.758
_shelx_estimated_absorpt_T_min   0.903
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22432
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.892
_diffrn_reflns_theta_max         73.158
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             11062
_reflns_number_gt                5610
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_max     0.953
_reflns_Friedel_fraction_full    0.992

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
;
_computing_structure_solution    'SHELXS-2014/8 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_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., SQUEEZE
;
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
1 -0.022 0.008 -0.002 7104.1 1129.1
_platon_squeeze_details          
;
 The unit cell contains 28 DMF molecules, which have been treated as a 
 diffuse contribution to the overall scattering without specific atom 
 positions by SQUEEZE/PLATON. 
 Thus, given the contribution of disordered solvents, the overall 
 formula, formula weight, density, F(000) should be 
 {Cu~2~((C~57~H~36~N~12~)(COO)~4~)(H~2~O)~2??7(DMF)}~n~,
 1739.76,1.016,2794,respectively. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1113P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1723 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11062
_refine_ls_number_parameters     384
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1917
_refine_ls_wR_factor_gt          0.1698
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_restrained_S_all      0.870
_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 1.45842(5) -0.07051(5) 0.71035(2) 0.0772(3) Uani 1 1 d . . . . .
O1 O 1.3897(3) -0.0144(3) 0.68041(8) 0.0943(14) Uani 1 1 d . . . . .
O2 O 1.4666(3) 0.1017(3) 0.67740(8) 0.0933(14) Uani 1 1 d . . . . .
C13 C 1.0341(4) 0.4302(4) 0.48094(8) 0.0646(13) Uani 1 1 d . . . . .
C16 C 1.000000 0.500000 0.46021(13) 0.0622(18) Uani 1 2 d S T P . .
N1 N 1.1979(4) 0.1724(4) 0.57431(11) 0.0967(17) Uani 1 1 d . . . . .
C17 C 0.9310(4) 0.4670(4) 0.43915(9) 0.0646(13) Uani 1 1 d . . . . .
O5 O 1.3897(4) -0.1865(3) 0.71185(12) 0.1355(18) Uani 1 1 d D . . . .
H5A H 1.385429 -0.205456 0.694654 0.203 Uiso 1 1 d DR U . . .
H5B H 1.361405 -0.155204 0.723613 0.203 Uiso 1 1 d DR U . . .
C2 C 1.3497(5) 0.0901(4) 0.64508(11) 0.087(2) Uani 1 1 d . . . . .
C10 C 1.1003(4) 0.3067(4) 0.51919(11) 0.0818(18) Uani 1 1 d . . . . .
N6 N 0.6724(4) 0.3011(5) 0.34772(13) 0.120(2) Uani 1 1 d . . . . .
C9 C 1.1329(5) 0.2430(5) 0.53971(12) 0.091(2) Uani 1 1 d . . . . .
C20 C 0.8056(4) 0.4019(4) 0.40033(11) 0.0806(17) Uani 1 1 d . . . . .
C22 C 0.8444(4) 0.4835(4) 0.44460(11) 0.0848(19) Uani 1 1 d . . . . .
H22 H 0.828747 0.516105 0.461059 0.102 Uiso 1 1 calc R U . . .
C14 C 1.0805(4) 0.4507(4) 0.50565(10) 0.0814(18) Uani 1 1 d . . . . .
H14 H 1.088049 0.506633 0.510338 0.098 Uiso 1 1 calc R U . . .
C1 C 1.4060(5) 0.0566(5) 0.66987(11) 0.085(2) Uani 1 1 d . . . . .
C21 C 0.7836(4) 0.4509(5) 0.42546(13) 0.094(2) Uani 1 1 d . . . . .
H21 H 0.727723 0.461834 0.429352 0.113 Uiso 1 1 calc R U . . .
N3 N 1.1061(5) 0.1611(4) 0.53915(12) 0.116(2) Uani 1 1 d . . . . .
C8 C 1.1919(5) 0.2511(5) 0.56186(14) 0.105(3) Uani 1 1 d . . . . .
H8 H 1.221205 0.298703 0.567312 0.126 Uiso 1 1 calc R U . . .
N2 N 1.1451(5) 0.1178(4) 0.56039(13) 0.119(2) Uani 1 1 d . . . . .
C18 C 0.9483(4) 0.4193(4) 0.41391(10) 0.0813(18) Uani 1 1 d . . . . .
H18 H 1.003694 0.407489 0.409518 0.098 Uiso 1 1 calc R U . . .
C7 C 1.3758(5) 0.1568(5) 0.62855(12) 0.099(2) Uani 1 1 d . . . . .
H7 H 1.425732 0.183523 0.632913 0.118 Uiso 1 1 calc R U . . .
C19 C 0.8884(4) 0.3885(5) 0.39507(11) 0.086(2) Uani 1 1 d . . . . .
H19 H 0.904352 0.357665 0.378197 0.103 Uiso 1 1 calc R U . . .
C24 C 0.7469(5) 0.3158(5) 0.35708(12) 0.098(2) Uani 1 1 d . . . . .
H24 H 0.795863 0.295276 0.348687 0.117 Uiso 1 1 calc R U . . .
C11 C 1.0524(5) 0.2863(4) 0.49454(13) 0.101(2) Uani 1 1 d . . . . .
H11 H 1.041481 0.230658 0.490246 0.121 Uiso 1 1 calc R U . . .
C15 C 1.1171(5) 0.3906(4) 0.52416(11) 0.088(2) Uani 1 1 d . . . . .
H15 H 1.152588 0.406461 0.539771 0.106 Uiso 1 1 calc R U . . .
C12 C 1.0203(5) 0.3480(4) 0.47603(12) 0.091(2) Uani 1 1 d . . . . .
H12 H 0.987923 0.332447 0.459504 0.109 Uiso 1 1 calc R U . . .
C5 C 1.2500(5) 0.1445(5) 0.59887(12) 0.093(2) Uani 1 1 d . . . . .
C3 C 1.2749(5) 0.0488(5) 0.63856(13) 0.103(2) Uani 1 1 d . . . . .
H3 H 1.259214 0.001953 0.649528 0.123 Uiso 1 1 calc R U . . .
C4 C 1.2261(5) 0.0782(5) 0.61613(14) 0.103(2) Uani 1 1 d . . . . .
H4 H 1.175085 0.052847 0.612351 0.124 Uiso 1 1 calc R U . . .
C6 C 1.3237(5) 0.1842(5) 0.60422(14) 0.099(2) Uani 1 1 d . . . . .
H6 H 1.339886 0.228834 0.592133 0.119 Uiso 1 1 calc R U . . .
C23 C 0.7409(5) 0.3656(5) 0.38081(15) 0.105(2) Uani 1 1 d . . . . .
C25 C 0.6437(5) 0.2460(6) 0.32294(15) 0.111(3) Uani 1 1 d . . . . .
N4 N 0.6618(5) 0.3763(7) 0.3858(2) 0.217(6) Uani 1 1 d . . . . .
N5 N 0.6182(5) 0.3396(8) 0.3646(2) 0.225(6) Uani 1 1 d . . . . .
C26 C 0.6945(6) 0.1918(6) 0.31105(17) 0.123(3) Uani 1 1 d . . . . .
H26 H 0.748141 0.185258 0.318636 0.148 Uiso 1 1 calc R U . . .
C27 C 0.6664(5) 0.1434(5) 0.28640(16) 0.116(3) Uani 1 1 d . . . . .
H27 H 0.702665 0.105955 0.277204 0.139 Uiso 1 1 calc R U . . .
C30 C 0.5621(6) 0.2584(7) 0.31252(19) 0.157(4) Uani 1 1 d . . . . .
H30 H 0.526862 0.297022 0.321576 0.188 Uiso 1 1 calc R U . . .
C29 C 0.5363(5) 0.2102(6) 0.28796(18) 0.129(3) Uani 1 1 d . . . . .
H29 H 0.483690 0.219084 0.279778 0.155 Uiso 1 1 calc R U . . .
C28 C 0.5857(5) 0.1507(5) 0.27571(13) 0.096(2) Uani 1 1 d . . . . .
C31 C 0.5539(6) 0.0941(5) 0.25114(13) 0.092(2) Uani 1 1 d . . . . .
O4 O 0.4800(3) 0.1056(3) 0.24306(8) 0.0956(14) Uani 1 1 d . . . . .
O3 O 0.6052(3) 0.0421(3) 0.24041(8) 0.0948(15) Uani 1 1 d . . . . .


_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 1.943(4) . ?
Cu1 O4 1.948(4) 2_645 ?
Cu1 O2 1.953(4) 4_855 ?
Cu1 O3 1.969(4) 7_655 ?
Cu1 O5 2.166(6) . ?
Cu1 Cu1 2.6294(17) 4_855 ?
O1 C1 1.259(9) . ?
O2 C1 1.257(8) . ?
C13 C12 1.355(8) . ?
C13 C14 1.361(7) . ?
C13 C16 1.547(6) . ?
C16 C17 1.540(6) 4_765 ?
C16 C17 1.540(6) . ?
N1 N2 1.365(8) . ?
N1 C8 1.382(9) . ?
N1 C5 1.441(7) . ?
C17 C18 1.380(7) . ?
C17 C22 1.436(8) . ?
O5 H5A 0.8200 . ?
O5 H5B 0.8538 . ?
C2 C7 1.362(9) . ?
C2 C3 1.402(10) . ?
C2 C1 1.517(8) . ?
C10 C11 1.371(8) . ?
C10 C15 1.391(9) . ?
C10 C9 1.464(8) . ?
N6 C24 1.287(9) . ?
N6 N5 1.304(9) . ?
N6 C25 1.480(8) . ?
C9 C8 1.367(9) . ?
C9 N3 1.383(10) . ?
C20 C19 1.368(9) . ?
C20 C21 1.405(8) . ?
C20 C23 1.469(9) . ?
C22 C21 1.393(8) . ?
C22 H22 0.9300 . ?
C14 C15 1.395(8) . ?
C14 H14 0.9300 . ?
C21 H21 0.9300 . ?
N3 N2 1.325(7) . ?
C8 H8 0.9300 . ?
C18 C19 1.364(8) . ?
C18 H18 0.9300 . ?
C7 C6 1.431(8) . ?
C7 H7 0.9300 . ?
C19 H19 0.9300 . ?
C24 C23 1.320(9) . ?
C24 H24 0.9300 . ?
C11 C12 1.384(8) . ?
C11 H11 0.9300 . ?
C15 H15 0.9300 . ?
C12 H12 0.9300 . ?
C5 C4 1.364(10) . ?
C5 C6 1.365(11) . ?
C3 C4 1.348(8) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C6 H6 0.9300 . ?
C23 N4 1.301(10) . ?
C25 C26 1.303(11) . ?
C25 C30 1.403(11) . ?
N4 N5 1.308(9) . ?
C26 C27 1.411(9) . ?
C26 H26 0.9300 . ?
C27 C28 1.385(10) . ?
C27 H27 0.9300 . ?
C30 C29 1.395(10) . ?
C30 H30 0.9300 . ?
C29 C28 1.354(10) . ?
C29 H29 0.9300 . ?
C28 C31 1.504(8) . ?
C31 O4 1.254(9) . ?
C31 O3 1.265(8) . ?

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 O4 90.62(17) . 2_645 ?
O1 Cu1 O2 87.88(17) . 4_855 ?
O4 Cu1 O2 169.5(3) 2_645 4_855 ?
O1 Cu1 O3 167.7(3) . 7_655 ?
O4 Cu1 O3 88.80(18) 2_645 7_655 ?
O2 Cu1 O3 90.45(17) 4_855 7_655 ?
O1 Cu1 O5 97.5(2) . . ?
O4 Cu1 O5 93.8(2) 2_645 . ?
O2 Cu1 O5 96.7(2) 4_855 . ?
O3 Cu1 O5 94.8(2) 7_655 . ?
O1 Cu1 Cu1 83.61(17) . 4_855 ?
O4 Cu1 Cu1 84.82(17) 2_645 4_855 ?
O2 Cu1 Cu1 84.69(17) 4_855 4_855 ?
O3 Cu1 Cu1 84.09(16) 7_655 4_855 ?
O5 Cu1 Cu1 178.25(14) . 4_855 ?
C1 O1 Cu1 123.6(5) . . ?
C1 O2 Cu1 121.8(4) . 4_855 ?
C12 C13 C14 116.9(5) . . ?
C12 C13 C16 123.6(4) . . ?
C14 C13 C16 119.5(5) . . ?
C17 C16 C17 105.8(5) 4_765 . ?
C17 C16 C13 110.5(3) 4_765 . ?
C17 C16 C13 111.2(3) . . ?
C17 C16 C13 111.2(3) 4_765 4_765 ?
C17 C16 C13 110.6(3) . 4_765 ?
C13 C16 C13 107.5(5) . 4_765 ?
N2 N1 C8 111.4(5) . . ?
N2 N1 C5 120.0(6) . . ?
C8 N1 C5 128.6(7) . . ?
C18 C17 C22 115.6(5) . . ?
C18 C17 C16 122.2(5) . . ?
C22 C17 C16 122.2(4) . . ?
Cu1 O5 H5A 109.5 . . ?
Cu1 O5 H5B 77.5 . . ?
H5A O5 H5B 137.4 . . ?
C7 C2 C3 121.7(6) . . ?
C7 C2 C1 118.8(7) . . ?
C3 C2 C1 119.4(7) . . ?
C11 C10 C15 117.7(6) . . ?
C11 C10 C9 121.6(7) . . ?
C15 C10 C9 120.7(6) . . ?
C24 N6 N5 110.5(6) . . ?
C24 N6 C25 129.5(7) . . ?
N5 N6 C25 119.9(7) . . ?
C8 C9 N3 108.6(6) . . ?
C8 C9 C10 128.6(7) . . ?
N3 C9 C10 122.8(6) . . ?
C19 C20 C21 117.8(6) . . ?
C19 C20 C23 121.7(6) . . ?
C21 C20 C23 120.5(6) . . ?
C21 C22 C17 120.6(5) . . ?
C21 C22 H22 119.7 . . ?
C17 C22 H22 119.7 . . ?
C13 C14 C15 122.2(6) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
O2 C1 O1 125.7(6) . . ?
O2 C1 C2 116.6(7) . . ?
O1 C1 C2 117.6(8) . . ?
C22 C21 C20 120.9(6) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
N2 N3 C9 109.9(6) . . ?
C9 C8 N1 104.2(7) . . ?
C9 C8 H8 127.9 . . ?
N1 C8 H8 127.9 . . ?
N3 N2 N1 105.9(6) . . ?
C19 C18 C17 123.4(6) . . ?
C19 C18 H18 118.3 . . ?
C17 C18 H18 118.3 . . ?
C2 C7 C6 117.7(7) . . ?
C2 C7 H7 121.2 . . ?
C6 C7 H7 121.2 . . ?
C18 C19 C20 121.7(5) . . ?
C18 C19 H19 119.1 . . ?
C20 C19 H19 119.1 . . ?
N6 C24 C23 107.4(7) . . ?
N6 C24 H24 126.3 . . ?
C23 C24 H24 126.3 . . ?
C10 C11 C12 120.3(7) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C10 C15 C14 119.8(5) . . ?
C10 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C13 C12 C11 122.8(6) . . ?
C13 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C4 C5 C6 120.9(6) . . ?
C4 C5 N1 119.9(8) . . ?
C6 C5 N1 119.2(6) . . ?
C4 C3 C2 118.9(7) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 121.3(8) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C5 C6 C7 119.5(7) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.2 . . ?
N4 C23 C24 106.6(7) . . ?
N4 C23 C20 122.6(7) . . ?
C24 C23 C20 130.8(8) . . ?
C26 C25 C30 123.2(7) . . ?
C26 C25 N6 120.1(7) . . ?
C30 C25 N6 116.6(8) . . ?
C23 N4 N5 110.0(7) . . ?
N6 N5 N4 105.3(7) . . ?
C25 C26 C27 118.6(8) . . ?
C25 C26 H26 120.7 . . ?
C27 C26 H26 120.7 . . ?
C28 C27 C26 121.0(8) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C29 C30 C25 117.0(9) . . ?
C29 C30 H30 121.5 . . ?
C25 C30 H30 121.5 . . ?
C28 C29 C30 121.8(8) . . ?
C28 C29 H29 119.1 . . ?
C30 C29 H29 119.1 . . ?
C29 C28 C27 118.2(6) . . ?
C29 C28 C31 121.1(7) . . ?
C27 C28 C31 120.8(8) . . ?
O4 C31 O3 127.4(6) . . ?
O4 C31 C28 115.9(7) . . ?
O3 C31 C28 116.6(7) . . ?
C31 O4 Cu1 121.8(5) . 7_564 ?
C31 O3 Cu1 121.2(4) . 2_534 ?

_refine_diff_density_max         0.182
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.057


_exptl_crystal_recrystallization_method 'solvothermal assembly'
_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_t41a
_database_code_depnum_ccdc_archive 'CCDC 1523578'
_audit_update_record             
;
2017-03-11 deposited with the CCDC.
2017-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/8
_shelx_SHELXL_version_number     2014/8
_chemical_name_systematic        T41a
_chemical_name_common            NTU-140
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C61 H40 Cu2 N12 O10'
_chemical_formula_weight         1228.13

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'
Cu Cu -1.9646 0.5888 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_H-M_alt        'P 42 21 2'
_space_group_name_Hall           'P 4n 2n'

_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'
'-y+1/2, x+1/2, z+1/2'
'-x, -y, z'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'-y, -x, -z'

_cell_length_a                   22.8050(5)
_cell_length_b                   22.8050(5)
_cell_length_c                   44.0727(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     22920.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    872
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      73.14

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.356
_exptl_crystal_F_000             2512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.144
_exptl_absorpt_coefficient_mu    0.376
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
; 
 ? 
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            45495
_diffrn_reflns_av_unetI/netI     0.1563
_diffrn_reflns_av_R_equivalents  0.0911
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         3.396
_diffrn_reflns_theta_max         73.332
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             21339
_reflns_number_gt                5470
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_max     0.866
_reflns_Friedel_fraction_full    0.914

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
;
_computing_structure_solution    'SHELXS-2014/8 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_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., SQUEEZE
;
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
1 -0.015 -0.009 -0.001 18890.5 3517.4
_platon_squeeze_details          
;
 The unit cell contains 88 DMF molecules, which have been treated as a 
 diffuse contribution to the overall scattering without specific atom 
 positions by SQUEEZE/PLATON.
 Thus, given the contribution of disordered solvents, the overall 
 formula, formula weight, density, F(000) should be 
 {Cu~2~((C~57~H~36~N~12~)(COO)~4~)(H~2~O)~2??22(DMF)}~n~,
 2836.11,0.822,3391,respectively.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0057P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1105 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.20(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         21339
_refine_ls_number_parameters     384
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1627
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.1370
_refine_ls_wR_factor_gt          0.1125
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_restrained_S_all      0.811
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001

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 0.55582(4) 0.48451(4) 0.36105(2) 0.1079(3) Uani 1 1 d . . . . .
O1 O 0.5322(2) 0.4296(2) 0.33004(10) 0.1241(17) Uani 1 1 d . . . . .
O2 O 0.4347(2) 0.4555(2) 0.32993(11) 0.1273(17) Uani 1 1 d . . . . .
O3 O 0.0703(2) 0.0329(2) -0.10794(13) 0.1258(18) Uani 1 1 d . . . . .
O4 O 0.04305(19) -0.0613(2) -0.10741(7) 0.1107(15) Uani 1 1 d . . . . .
O5 O 0.64690(19) 0.4565(2) 0.36094(14) 0.183(2) Uani 1 1 d . . . . .
H5A H 0.667271 0.485651 0.355317 0.220 Uiso 1 1 d R U . . .
H5B H 0.655842 0.449641 0.379567 0.220 Uiso 1 1 d R U . . .
N1 N 0.4319(4) 0.2544(4) 0.2284(2) 0.192(4) Uani 1 1 d . . . . .
N2 N 0.3766(4) 0.2523(6) 0.2141(3) 0.320(8) Uani 1 1 d . . . . .
N3 N 0.3814(4) 0.2110(6) 0.1940(3) 0.310(8) Uani 1 1 d . . . . .
N4 N 0.2757(5) -0.1085(4) 0.0325(2) 0.227(5) Uani 1 1 d . . . . .
N5 N 0.2337(4) -0.1096(4) 0.0133(2) 0.213(5) Uani 1 1 d . . . . .
N6 N 0.2423(3) -0.0648(4) -0.00407(12) 0.130(2) Uani 1 1 d . U . . .
C1 C 0.4773(3) 0.4246(4) 0.32022(15) 0.123(3) Uani 1 1 d . U . . .
C2 C 0.4652(4) 0.3785(4) 0.29707(18) 0.146(4) Uani 1 1 d . . . . .
C3 C 0.5087(5) 0.3465(5) 0.2869(2) 0.212(6) Uani 1 1 d . . . . .
H3 H 0.545995 0.350996 0.295108 0.254 Uiso 1 1 calc R U . . .
C4 C 0.4998(4) 0.3072(5) 0.2645(2) 0.195(5) Uani 1 1 d . . . . .
H4 H 0.531148 0.284852 0.257481 0.234 Uiso 1 1 calc R U . . .
C5 C 0.4479(5) 0.2997(4) 0.2524(2) 0.153(4) Uani 1 1 d . . . . .
C6 C 0.3993(4) 0.3320(5) 0.2618(2) 0.198(5) Uani 1 1 d . . . . .
H6 H 0.362318 0.327194 0.253277 0.237 Uiso 1 1 calc R U . . .
C7 C 0.4099(4) 0.3716(5) 0.2847(2) 0.183(5) Uani 1 1 d . . . . .
H7 H 0.379140 0.394216 0.292057 0.220 Uiso 1 1 calc R U . . .
C8 C 0.4665(4) 0.2153(5) 0.2137(2) 0.165(4) Uani 1 1 d . . . . .
H8 H 0.506471 0.210211 0.216958 0.198 Uiso 1 1 calc R U . . .
C9 C 0.4331(5) 0.1845(5) 0.1933(2) 0.158(4) Uani 1 1 d . . . . .
C10 C 0.4523(4) 0.1393(5) 0.17346(18) 0.143(3) Uani 1 1 d . U . . .
C11 C 0.5078(4) 0.1146(4) 0.17375(19) 0.145(3) Uani 1 1 d . . . . .
H11 H 0.535605 0.127821 0.187587 0.174 Uiso 1 1 calc R U . . .
C12 C 0.5213(4) 0.0727(4) 0.15458(16) 0.133(3) Uani 1 1 d . . . . .
H12 H 0.558821 0.056874 0.155500 0.159 Uiso 1 1 calc R U . . .
C13 C 0.4815(3) 0.0499(3) 0.13228(18) 0.121(3) Uani 1 1 d . . . . .
C14 C 0.4266(3) 0.0744(4) 0.1325(2) 0.156(4) Uani 1 1 d . . . . .
H14 H 0.397669 0.059484 0.119773 0.188 Uiso 1 1 calc R U . . .
C15 C 0.4137(4) 0.1223(5) 0.1519(2) 0.179(4) Uani 1 1 d . . . . .
H15 H 0.378338 0.142187 0.149818 0.215 Uiso 1 1 calc R U . . .
C16 C 0.500000 0.000000 0.1101(3) 0.114(3) Uani 1 2 d S T P . .
C17 C 0.4483(3) -0.0171(4) 0.08983(15) 0.111(2) Uani 1 1 d . . . . .
C18 C 0.4234(4) -0.0713(4) 0.08913(18) 0.150(4) Uani 1 1 d . . . . .
H18 H 0.437284 -0.099255 0.102708 0.180 Uiso 1 1 calc R U . . .
C19 C 0.3791(4) -0.0876(4) 0.06981(19) 0.162(4) Uani 1 1 d . . . . .
H19 H 0.364480 -0.125652 0.070414 0.194 Uiso 1 1 calc R U . . .
C20 C 0.3568(4) -0.0484(4) 0.0499(2) 0.134(3) Uani 1 1 d . . . . .
C21 C 0.3809(3) 0.0095(4) 0.04813(15) 0.140(3) Uani 1 1 d . . . . .
H21 H 0.366101 0.037746 0.034992 0.168 Uiso 1 1 calc R U . . .
C22 C 0.4291(3) 0.0208(3) 0.06786(14) 0.121(3) Uani 1 1 d . . . . .
H22 H 0.448753 0.056310 0.065692 0.145 Uiso 1 1 calc R U . . .
C23 C 0.3055(4) -0.0597(4) 0.0290(2) 0.136(3) Uani 1 1 d . . . . .
C24 C 0.2831(3) -0.0299(4) 0.00668(15) 0.141(3) Uani 1 1 d . . . . .
H24 H 0.293619 0.007233 -0.000092 0.169 Uiso 1 1 calc R U . . .
C25 C 0.2006(5) -0.0560(4) -0.0269(2) 0.153(4) Uani 1 1 d . . . . .
C26 C 0.1620(4) -0.0963(3) -0.03865(19) 0.149(3) Uani 1 1 d . . . . .
H26 H 0.162526 -0.133839 -0.030435 0.179 Uiso 1 1 calc R U . . .
C27 C 0.1218(3) -0.0852(4) -0.06223(13) 0.138(3) Uani 1 1 d . . . . .
H27 H 0.097574 -0.114881 -0.069415 0.166 Uiso 1 1 calc R U . . .
C28 C 0.1190(4) -0.0304(3) -0.07431(17) 0.123(3) Uani 1 1 d . . . . .
C29 C 0.1576(3) 0.0130(4) -0.06457(19) 0.152(3) Uani 1 1 d . . . . .
H29 H 0.157498 0.049626 -0.073851 0.182 Uiso 1 1 calc R U . . .
C30 C 0.1971(3) 0.0011(4) -0.04027(18) 0.152(4) Uani 1 1 d . . . . .
H30 H 0.221165 0.030905 -0.033022 0.182 Uiso 1 1 calc R U . . .
C31 C 0.0751(3) -0.0198(4) -0.09830(15) 0.128(3) Uani 1 1 d . . . . .


_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 1.931(4) . ?
Cu1 O3 1.925(6) 4 ?
Cu1 O4 1.931(3) 2 ?
Cu1 O2 1.949(5) 3_665 ?
Cu1 O5 2.173(4) . ?
Cu1 Cu1 2.6420(17) 3_665 ?
O1 C1 1.329(7) . ?
O2 C1 1.273(8) . ?
O3 C31 1.279(9) . ?
O4 C31 1.261(8) . ?
O5 H5A 0.8485 . ?
O5 H5B 0.8602 . ?
N1 C8 1.354(10) . ?
N1 N2 1.411(11) . ?
N1 C5 1.522(11) . ?
N2 N3 1.294(11) . ?
N3 C9 1.327(13) . ?
N4 C23 1.313(10) . ?
N4 N5 1.277(9) . ?
N5 N6 1.291(9) . ?
N6 C24 1.314(8) . ?
N6 C25 1.397(10) . ?
C1 C2 1.491(10) . ?
C2 C3 1.311(12) . ?
C2 C7 1.383(11) . ?
C3 C4 1.350(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.308(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(11) . ?
C6 C7 1.373(11) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.374(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.419(12) . ?
C10 C15 1.351(10) . ?
C10 C11 1.386(11) . ?
C11 C12 1.312(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.435(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(9) . ?
C13 C16 1.558(9) . ?
C14 C15 1.421(11) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.530(8) 3_655 ?
C16 C17 1.530(8) . ?
C17 C22 1.371(9) . ?
C17 C18 1.360(10) . ?
C18 C19 1.371(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.353(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.432(10) . ?
C20 C23 1.509(10) . ?
C21 C22 1.425(8) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.300(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.373(10) . ?
C25 C30 1.433(11) . ?
C26 C27 1.409(9) . ?
C26 H26 0.9300 . ?
C27 C28 1.360(10) . ?
C27 H27 0.9300 . ?
C28 C29 1.391(9) . ?
C28 C31 1.477(9) . ?
C29 C30 1.427(9) . ?
C29 H29 0.9300 . ?
C30 H30 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 O3 90.31(19) . 4 ?
O1 Cu1 O4 167.4(2) . 2 ?
O3 Cu1 O4 87.4(2) 4 2 ?
O1 Cu1 O2 89.3(2) . 3_665 ?
O3 Cu1 O2 170.3(2) 4 3_665 ?
O4 Cu1 O2 90.80(18) 2 3_665 ?
O1 Cu1 O5 94.3(2) . . ?
O3 Cu1 O5 94.0(2) 4 . ?
O4 Cu1 O5 98.3(2) 2 . ?
O2 Cu1 O5 95.7(2) 3_665 . ?
O1 Cu1 Cu1 84.52(15) . 3_665 ?
O3 Cu1 Cu1 84.95(14) 4 3_665 ?
O4 Cu1 Cu1 82.95(15) 2 3_665 ?
O2 Cu1 Cu1 85.37(15) 3_665 3_665 ?
O5 Cu1 Cu1 178.39(14) . 3_665 ?
C1 O1 Cu1 123.2(5) . . ?
C1 O2 Cu1 122.7(5) . 3_665 ?
C31 O3 Cu1 123.1(4) . 2_544 ?
C31 O4 Cu1 125.6(5) . 4_454 ?
Cu1 O5 H5A 107.0 . . ?
Cu1 O5 H5B 106.1 . . ?
H5A O5 H5B 106.9 . . ?
C8 N1 N2 106.5(9) . . ?
C8 N1 C5 129.7(10) . . ?
N2 N1 C5 123.2(10) . . ?
N3 N2 N1 104.8(9) . . ?
N2 N3 C9 115.1(10) . . ?
C23 N4 N5 109.2(9) . . ?
N6 N5 N4 105.3(8) . . ?
N5 N6 C24 111.8(6) . . ?
N5 N6 C25 115.9(8) . . ?
C24 N6 C25 131.0(9) . . ?
O2 C1 O1 124.2(7) . . ?
O2 C1 C2 118.6(7) . . ?
O1 C1 C2 117.1(8) . . ?
C3 C2 C7 119.4(9) . . ?
C3 C2 C1 119.2(10) . . ?
C7 C2 C1 121.3(9) . . ?
C2 C3 C4 120.5(11) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 121.4(11) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 121.9(10) . . ?
C4 C5 N1 126.0(11) . . ?
C6 C5 N1 112.1(9) . . ?
C5 C6 C7 115.2(9) . . ?
C5 C6 H6 122.5 . . ?
C7 C6 H6 122.4 . . ?
C2 C7 C6 121.7(9) . . ?
C2 C7 H7 119.1 . . ?
C6 C7 H7 119.2 . . ?
C9 C8 N1 109.1(9) . . ?
C9 C8 H8 125.4 . . ?
N1 C8 H8 125.5 . . ?
C8 C9 N3 104.0(10) . . ?
C8 C9 C10 127.2(12) . . ?
N3 C9 C10 128.4(10) . . ?
C15 C10 C11 119.0(9) . . ?
C15 C10 C9 116.1(10) . . ?
C11 C10 C9 124.8(9) . . ?
C12 C11 C10 120.3(10) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 123.8(9) . . ?
C11 C12 H12 118.1 . . ?
C13 C12 H12 118.1 . . ?
C14 C13 C12 115.2(8) . . ?
C14 C13 C16 123.3(7) . . ?
C12 C13 C16 121.5(7) . . ?
C13 C14 C15 120.5(8) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C10 C15 C14 120.7(10) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C17 108.6(9) 3_655 . ?
C17 C16 C13 112.9(4) 3_655 . ?
C17 C16 C13 110.1(4) . . ?
C17 C16 C13 110.1(4) 3_655 3_655 ?
C17 C16 C13 112.9(4) . 3_655 ?
C13 C16 C13 102.3(9) . 3_655 ?
C22 C17 C18 115.1(7) . . ?
C22 C17 C16 119.8(7) . . ?
C18 C17 C16 124.6(7) . . ?
C17 C18 C19 124.6(8) . . ?
C17 C18 H18 117.7 . . ?
C19 C18 H18 117.7 . . ?
C20 C19 C18 120.1(9) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 119.9(8) . . ?
C19 C20 C23 125.1(9) . . ?
C21 C20 C23 114.9(9) . . ?
C20 C21 C22 115.5(8) . . ?
C20 C21 H21 122.3 . . ?
C22 C21 H21 122.2 . . ?
C17 C22 C21 124.2(7) . . ?
C17 C22 H22 117.9 . . ?
C21 C22 H22 117.9 . . ?
N4 C23 C24 109.0(8) . . ?
N4 C23 C20 118.4(9) . . ?
C24 C23 C20 132.6(10) . . ?
N6 C24 C23 103.7(8) . . ?
N6 C24 H24 128.2 . . ?
C23 C24 H24 128.2 . . ?
C26 C25 C30 114.6(9) . . ?
C26 C25 N6 127.8(9) . . ?
C30 C25 N6 117.6(8) . . ?
C25 C26 C27 125.2(9) . . ?
C25 C26 H26 117.4 . . ?
C27 C26 H26 117.5 . . ?
C28 C27 C26 119.0(8) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C27 C28 C29 120.2(8) . . ?
C27 C28 C31 117.6(8) . . ?
C29 C28 C31 122.2(8) . . ?
C28 C29 C30 119.7(8) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.2 . . ?
C25 C30 C29 121.2(8) . . ?
C25 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
O4 C31 O3 123.3(6) . . ?
O4 C31 C28 119.9(8) . . ?
O3 C31 C28 116.7(7) . . ?

_refine_diff_density_max         0.276
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.021


_exptl_crystal_recrystallization_method 'solvothermal assemably'
_chemical_properties_physical    ', Moisture-sensitive'
