# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_swy1
_database_code_depnum_ccdc_archive 'CCDC 1028540'
_audit_update_record             
;
2017-07-15 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H28 Cu3 N2 O13, 13(C3 H7 N O)'
_chemical_formula_sum            'C85 H119 Cu3 N15 O26'
_chemical_formula_weight         1957.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   19.387(4)
_cell_length_b                   19.387(4)
_cell_length_c                   60.831(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     22864(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1601
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      17.05

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_F_000             8232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.360
_exptl_absorpt_coefficient_mu    0.620
_shelx_estimated_absorpt_T_min   0.789
_shelx_estimated_absorpt_T_max   0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6017
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31263
_diffrn_reflns_av_unetI/netI     0.1723
_diffrn_reflns_av_R_equivalents  0.2468
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_theta_min         1.102
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5792
_reflns_number_gt                2204
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0292P)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_number_reflns         5792
_refine_ls_number_parameters     165
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1370
_refine_ls_wR_factor_gt          0.1217
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.046
_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 0.43246(4) 0.49767(2) 0.0486(3) Uani 1 2 d S T P A .
Cu2 Cu 0.5000 0.2500 0.60331(2) 0.0480(3) Uani 1 4 d S T P . .
O1 O 0.07017(18) 0.55393(18) 0.52481(5) 0.0664(11) Uani 1 1 d . . . . .
O2 O 0.07126(18) 0.44070(18) 0.52075(5) 0.0676(10) Uani 1 1 d . . . . .
O3 O 0.42981(17) 0.32005(17) 0.60648(5) 0.0690(10) Uani 1 1 d . . . . .
O4 O 0.5000 0.2500 0.56721(11) 0.125(3) Uani 1 4 d S TU P . .
H4A H 0.4706 0.2793 0.5596 0.150 Uiso 0.25 1 d R U P . .
H4B H 0.5294 0.2207 0.5596 0.150 Uiso 0.25 1 d R U P . .
N1 N 0.0000 0.3189(3) 0.49722(10) 0.0664(16) Uani 1 2 d DS TU P . .
C1 C 0.0899(3) 0.4959(4) 0.53032(8) 0.0619(15) Uani 1 1 d . . . . .
C2 C 0.1375(3) 0.4863(3) 0.54919(8) 0.0683(17) Uani 1 1 d . . . . .
C3 C 0.1608(3) 0.4223(3) 0.55521(9) 0.117(3) Uani 1 1 d . . . . .
H3 H 0.1485 0.3840 0.5469 0.140 Uiso 1 1 calc R U . . .
C4 C 0.1562(3) 0.5417(3) 0.56174(10) 0.097(2) Uani 1 1 d . . . . .
H4 H 0.1411 0.5857 0.5581 0.116 Uiso 1 1 calc R U . . .
C5 C 0.2030(4) 0.4137(3) 0.57372(10) 0.136(3) Uani 1 1 d . . . . .
H5 H 0.2188 0.3700 0.5776 0.163 Uiso 1 1 calc R U . . .
C6 C 0.1979(3) 0.5320(3) 0.57998(9) 0.105(2) Uani 1 1 d . . . . .
H6 H 0.2104 0.5703 0.5883 0.126 Uiso 1 1 calc R U . . .
C7 C 0.2211(3) 0.4699(3) 0.58619(9) 0.096(2) Uani 1 1 d . . . . .
C8 C 0.2650(3) 0.4582(3) 0.60569(9) 0.088(2) Uani 1 1 d . . . . .
C9 C 0.2533(3) 0.4967(3) 0.6250 0.105(3) Uani 1 2 d S T P . .
H9 H 0.2193 0.5307 0.6250 0.127 Uiso 1 2 calc R U P . .
C10 C 0.3156(3) 0.4093(3) 0.60609(8) 0.0821(19) Uani 1 1 d . . . . .
H10 H 0.3249 0.3841 0.5934 0.099 Uiso 1 1 calc R U . . .
C11 C 0.3535(2) 0.3965(2) 0.6250 0.064(2) Uani 1 2 d S T P . .
C12 C 0.4078(3) 0.3422(3) 0.6250 0.065(2) Uani 1 2 d S T P . .
C13A C 0.0000 0.2870(6) 0.5166(2) 0.077(3) Uani 0.5 2 d DS TU P A 1
H13A H 0.0000 0.3119 0.5297 0.092 Uiso 0.5 2 calc R U P A 1
C13B C 0.0000 0.2891(7) 0.4761(2) 0.089(4) Uani 0.5 2 d DS TU P A 1
H13B H 0.0000 0.3152 0.4633 0.106 Uiso 0.5 2 calc R U P A 1
C13C C 0.0594(5) 0.2859(4) 0.49183(17) 0.086(3) Uani 0.5 1 d D U P A 2
H13C H 0.0989 0.3106 0.4882 0.104 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.947(3) 17_566 ?
Cu1 O1 1.947(3) 6_566 ?
Cu1 O2 1.976(3) . ?
Cu1 O2 1.976(3) 22 ?
Cu1 N1 2.202(5) . ?
Cu1 Cu1 2.6341(16) 17_566 ?
Cu2 O3 1.932(3) . ?
Cu2 O3 1.932(3) 22_655 ?
Cu2 O3 1.932(3) 29 ?
Cu2 O3 1.932(3) 10_554 ?
Cu2 O4 2.196(7) . ?
Cu2 Cu2 2.639(2) 27_566 ?
O1 C1 1.235(6) . ?
O1 Cu1 1.946(3) 17_566 ?
O2 C1 1.271(5) . ?
O3 C12 1.279(4) . ?
O4 H4A 0.9300 . ?
O4 H4B 0.9300 . ?
N1 C13A 1.332(11) . ?
N1 C13C 1.357(9) . ?
N1 C13C 1.357(9) 22 ?
N1 C13B 1.405(12) . ?
C1 C2 1.484(6) . ?
C2 C4 1.367(6) . ?
C2 C3 1.371(6) . ?
C3 C5 1.402(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.385(6) . ?
C4 H4 0.9300 . ?
C5 C7 1.373(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.340(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.477(7) . ?
C8 C10 1.363(6) . ?
C8 C9 1.411(6) . ?
C9 C8 1.411(6) 16 ?
C9 H9 0.9300 . ?
C10 C11 1.388(5) . ?
C10 H10 0.9300 . ?
C11 C10 1.388(5) 16 ?
C11 C12 1.488(9) . ?
C12 O3 1.279(4) 16 ?
C13A C13A 1.44(2) 10_454 ?
C13A H13A 0.9300 . ?
C13B C13B 1.52(3) 10_454 ?
C13B H13B 0.9300 . ?
C13C C13C 1.394(16) 29 ?
C13C H13C 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 88.7(2) 17_566 6_566 ?
O1 Cu1 O2 167.58(13) 17_566 . ?
O1 Cu1 O2 89.97(13) 6_566 . ?
O1 Cu1 O2 89.98(13) 17_566 22 ?
O1 Cu1 O2 167.57(13) 6_566 22 ?
O2 Cu1 O2 88.7(2) . 22 ?
O1 Cu1 N1 97.28(15) 17_566 . ?
O1 Cu1 N1 97.28(15) 6_566 . ?
O2 Cu1 N1 95.14(15) . . ?
O2 Cu1 N1 95.14(15) 22 . ?
O1 Cu1 Cu1 86.62(11) 17_566 17_566 ?
O1 Cu1 Cu1 86.62(11) 6_566 17_566 ?
O2 Cu1 Cu1 80.97(10) . 17_566 ?
O2 Cu1 Cu1 80.97(10) 22 17_566 ?
N1 Cu1 Cu1 174.52(16) . 17_566 ?
O3 Cu2 O3 89.5(2) . 22_655 ?
O3 Cu2 O3 89.3(2) . 29 ?
O3 Cu2 O3 168.53(17) 22_655 29 ?
O3 Cu2 O3 168.53(17) . 10_554 ?
O3 Cu2 O3 89.3(2) 22_655 10_554 ?
O3 Cu2 O3 89.5(2) 29 10_554 ?
O3 Cu2 O4 95.74(9) . . ?
O3 Cu2 O4 95.74(9) 22_655 . ?
O3 Cu2 O4 95.74(9) 29 . ?
O3 Cu2 O4 95.74(9) 10_554 . ?
O3 Cu2 Cu2 84.26(9) . 27_566 ?
O3 Cu2 Cu2 84.26(9) 22_655 27_566 ?
O3 Cu2 Cu2 84.26(9) 29 27_566 ?
O3 Cu2 Cu2 84.26(9) 10_554 27_566 ?
O4 Cu2 Cu2 180.0 . 27_566 ?
C1 O1 Cu1 122.0(3) . 17_566 ?
C1 O2 Cu1 126.3(3) . . ?
C12 O3 Cu2 124.0(4) . . ?
Cu2 O4 H4A 120.0 . . ?
Cu2 O4 H4B 120.0 . . ?
H4A O4 H4B 120.0 . . ?
C13C N1 C13C 116.1(10) . 22 ?
C13A N1 C13B 128.2(9) . . ?
C13A N1 Cu1 116.9(6) . . ?
C13C N1 Cu1 118.3(5) . . ?
C13C N1 Cu1 118.3(5) 22 . ?
C13B N1 Cu1 114.9(7) . . ?
O1 C1 O2 123.7(5) . . ?
O1 C1 C2 121.1(5) . . ?
O2 C1 C2 115.2(6) . . ?
C4 C2 C3 118.3(5) . . ?
C4 C2 C1 120.0(5) . . ?
C3 C2 C1 121.7(5) . . ?
C2 C3 C5 121.0(5) . . ?
C2 C3 H3 119.5 . . ?
C5 C3 H3 119.5 . . ?
C2 C4 C6 119.8(6) . . ?
C2 C4 H4 120.1 . . ?
C6 C4 H4 120.1 . . ?
C7 C5 C3 119.8(6) . . ?
C7 C5 H5 120.1 . . ?
C3 C5 H5 120.1 . . ?
C7 C6 C4 122.9(6) . . ?
C7 C6 H6 118.6 . . ?
C4 C6 H6 118.6 . . ?
C6 C7 C5 118.2(5) . . ?
C6 C7 C8 123.9(5) . . ?
C5 C7 C8 117.9(6) . . ?
C10 C8 C9 118.0(5) . . ?
C10 C8 C7 122.4(5) . . ?
C9 C8 C7 119.6(5) . . ?
C8 C9 C8 121.5(7) . 16 ?
C8 C9 H9 119.3 . . ?
C8 C9 H9 119.3 16 . ?
C8 C10 C11 121.4(5) . . ?
C8 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C10 119.8(6) 16 . ?
C10 C11 C12 120.1(3) 16 . ?
C10 C11 C12 120.1(3) . . ?
O3 C12 O3 123.5(7) . 16 ?
O3 C12 C11 118.3(3) . . ?
O3 C12 C11 118.3(3) 16 . ?
N1 C13A C13A 117.6(6) . 10_454 ?
N1 C13A H13A 121.2 . . ?
C13A C13A H13A 121.2 10_454 . ?
N1 C13B C13B 114.2(6) . 10_454 ?
N1 C13B H13B 122.9 . . ?
C13B C13B H13B 122.9 10_454 . ?
N1 C13C C13C 118.1(5) . 29 ?
N1 C13C H13C 121.0 . . ?
C13C C13C H13C 121.0 29 . ?

_refine_diff_density_max         0.528
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.055


# start Validation Reply Form
_vrf_CHEMW03_2                   
;
PROBLEM:  The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    8
           From the CIF: _chemical_formula_weight          1957.56
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   46.00  552.51
           H         1.01   28.00   28.22
           N        14.01    2.00   28.01
           O        16.00   13.00  207.99
           Cu       63.55    3.00  190.64
           Calculated formula weight             1007.37
           
RESPONSE: PLATON SQUEEZE has been employed; the removed solvent has been 
included in the formula and the calculation of derived parameters.
;

_vrf_RINTA01_ALERT_3             
;
PROBLEM:   The value of Rint is greater than 0.18
            Rint given   0.247
RESPONSE:   This problem is mainly due to the poor diffraction from the mofs with high porsity. 
;

_vrf_PLAT026_ALERT_3             
;
PROBLEM:   Ratio Observed / Unique Reflections (too) Low ..         38 %  
RESPONSE:  The crystal diffracted weakly so low sigma values were selected. 
;

_vrf_PLAT430_ALERT_3             
;
PROBLEM:   PLAT430_ALERT_2_B Short Inter D...A Contact  N1     ..  N1      ..       2.67 Ang.  
RESPONSE:  These nitrogens (N1 and N1) correspond to the pyz linker in MOF. The N...N distances 
are comparable to what is observed for typical pyz ligands in other reported crystals.
;

# end Validation Reply Form


####################################################################### 
# 
# 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_swy5
_database_code_depnum_ccdc_archive 'CCDC 1028544'
_audit_update_record             
;
2017-07-15 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H36 Cu3 N2 O17, 8(C3 H7 N O)'
_chemical_formula_sum            'C152 H184 Cu6 N20 O50'
_chemical_formula_weight         3472.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'

_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+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'-y+1/4, -x+1/4, -z+3/4'
'y+1/4, x+3/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'-y+3/4, -x+3/4, -z+5/4'
'y+3/4, x+5/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'y-1/4, x-1/4, z-3/4'
'-y-1/4, -x-3/4, z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'
'y+1/4, x+1/4, z-1/4'
'-y+1/4, -x-1/4, z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'

_cell_length_a                   19.627(2)
_cell_length_b                   19.627
_cell_length_c                   60.175(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     23181(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2658
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      17.24

_exptl_crystal_description       block
_exptl_crystal_colour            dark-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.995
_exptl_crystal_F_000             7240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.603
_shelx_estimated_absorpt_T_min   0.794
_shelx_estimated_absorpt_T_max   0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            66775
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_av_R_equivalents  0.1750
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_theta_min         1.452
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5808
_reflns_number_gt                2920
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+0.0100P] 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_number_reflns         5808
_refine_ls_number_parameters     259
_refine_ls_number_restraints     329
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0738
_refine_ls_wR_factor_ref         0.2157
_refine_ls_wR_factor_gt          0.1863
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.159
_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 0.18392(4) 0.7500 0.24719(2) 0.0535(3) Uani 1 2 d S T P B .
Cu2 Cu 0.0000 0.2500 0.35314(2) 0.0508(3) Uani 1 4 d S T P . .
O1 O 0.29993(17) 0.68079(18) 0.27541(5) 0.0720(10) Uani 1 1 d . U . . .
O2 O 0.18764(17) 0.68021(18) 0.27055(5) 0.0725(10) Uani 1 1 d . U . . .
O3 O 0.0000 0.2500 0.31711(12) 0.131(4) Uani 1 4 d S T P . .
H3A H 0.0265 0.2765 0.3101 0.158 Uiso 0.25 1 d R U P . .
H3B H -0.0265 0.2235 0.3101 0.158 Uiso 0.25 1 d R U P . .
O4 O 0.07031(16) 0.32066(17) 0.35657(5) 0.0700(9) Uani 1 1 d . U . . .
O5A O 0.0000 0.7500 0.1839(3) 0.173(5) Uani 0.5 4 d DS TU P . .
O6A O 0.1025(4) 0.7500 0.1657(4) 0.223(9) Uani 0.25 2 d DS TU P . .
O5B O 0.0000 0.7500 0.3056(3) 0.162(5) Uani 0.5 4 d DS TU P . .
C16B C -0.0657(7) 0.7500 0.3380(4) 0.196(7) Uani 0.25 2 d DS TU P . .
H16G H -0.0600 0.7500 0.3538 0.295 Uiso 0.25 2 d R U P B .
H16H H -0.0905 0.7899 0.3335 0.295 Uiso 0.125 1 d R U P . .
H16I H -0.0905 0.7101 0.3335 0.295 Uiso 0.125 1 d R U P . .
O5C O 0.0000 0.5555(7) 0.2419(3) 0.200(5) Uani 0.5 2 d DS TU P A 2
O6C O 0.0854(13) 0.4857(14) 0.2305(5) 0.253(9) Uani 0.25 1 d D U P A 2
N1 N 0.0719(3) 0.7500 0.24497(13) 0.0979(18) Uani 1 2 d S TU P . .
C1 C 0.2402(3) 0.6607(3) 0.28014(8) 0.0671(13) Uani 1 1 d . U . . .
C2 C 0.2319(3) 0.6141(3) 0.29902(8) 0.0731(13) Uani 1 1 d . U . . .
C3 C 0.1693(3) 0.5892(3) 0.30492(9) 0.0893(16) Uani 1 1 d . U . . .
H3 H 0.1317 0.6002 0.2962 0.107 Uiso 1 1 calc R U . . .
C4 C 0.2885(3) 0.5928(3) 0.31159(9) 0.0870(16) Uani 1 1 d . U . . .
H4 H 0.3321 0.6068 0.3077 0.104 Uiso 1 1 calc R U . . .
C5 C 0.1602(3) 0.5481(3) 0.32335(9) 0.0921(17) Uani 1 1 d . U . . .
H5 H 0.1165 0.5344 0.3273 0.111 Uiso 1 1 calc R U . . .
C6 C 0.2787(3) 0.5505(3) 0.32990(9) 0.0917(17) Uani 1 1 d . U . . .
H6 H 0.3162 0.5375 0.3383 0.110 Uiso 1 1 calc R U . . .
C7 C 0.2147(3) 0.5275(3) 0.33583(9) 0.0812(15) Uani 1 1 d . U . . .
C8 C 0.2048(3) 0.4838(3) 0.35578(8) 0.0794(14) Uani 1 1 d . U . . .
C9 C 0.2443(3) 0.4943(3) 0.3750 0.085(2) Uani 1 2 d S TU P . .
H9 H 0.2779 0.5279 0.3750 0.103 Uiso 1 2 calc R U P . .
C10 C 0.1565(3) 0.4326(3) 0.35626(8) 0.0744(14) Uani 1 1 d . U . . .
H10 H 0.1314 0.4236 0.3435 0.089 Uiso 1 1 calc R U . . .
C11 C 0.1444(2) 0.3944(2) 0.3750 0.0681(17) Uani 1 2 d S TU P . .
C12 C 0.0909(2) 0.3409(2) 0.3750 0.0626(16) Uani 1 2 d S TU P . .
C13A C 0.0362(8) 0.7500 0.2266(3) 0.1004(19) Uani 0.5 2 d DS TU P B 1
H13A H 0.0602 0.7500 0.2127 0.120 Uiso 0.25 2 d R U P B 2
C14A C 0.0475(13) 0.7500 0.2020(3) 0.140(5) Uani 0.25 2 d DS TU P B 1
H14A H 0.0761 0.7894 0.1993 0.168 Uiso 0.125 1 d R U P B 1
H14B H 0.0761 0.7106 0.1993 0.168 Uiso 0.125 1 d R U P B 1
C15A C 0.0376(10) 0.7500 0.1640(4) 0.186(6) Uani 0.25 2 d DS TU P B 1
C16A C 0.0000 0.7500 0.1447(3) 0.192(7) Uani 0.5 4 d DS TU P B 1
H16A H 0.0212 0.7797 0.1341 0.289 Uiso 0.125 1 d R U P B 1
H16B H -0.0454 0.7657 0.1477 0.289 Uiso 0.125 1 d R U P B 1
H16C H 0.0000 0.7046 0.1388 0.289 Uiso 0.25 2 d R U P B 1
C13B C 0.0348(8) 0.7500 0.2665(3) 0.1000(19) Uani 0.5 2 d DS TU P B 1
H13B H 0.0595 0.7500 0.2803 0.120 Uiso 0.25 2 d R U P B 2
C14B C 0.0559(10) 0.7500 0.2904(3) 0.131(4) Uani 0.25 2 d DS TU P B 1
H14C H 0.0836 0.7100 0.2932 0.157 Uiso 0.125 1 d R U P B 1
H14D H 0.0836 0.7900 0.2932 0.157 Uiso 0.125 1 d R U P B 1
C15B C 0.0000 0.7500 0.3276(3) 0.187(6) Uani 0.5 4 d DS TU P B 1
O6B O 0.0553(8) 0.7500 0.3388(4) 0.203(7) Uani 0.25 2 d DS TU P B 1
C13C C 0.0409(6) 0.6956(7) 0.2445(2) 0.1013(19) Uani 0.5 1 d D U P A 2
H13C H 0.0667 0.6541 0.2442 0.122 Uiso 0.25 1 d R U P A 1
C14C C 0.0203(4) 0.6244(7) 0.24322(18) 0.168(5) Uani 0.25 1 d D U P A 2
H14E H 0.0645 0.6119 0.2372 0.202 Uiso 0.25 1 d R U P A 2
H14F H 0.0254 0.6202 0.2592 0.202 Uiso 0.25 1 d R U P A 2
C15C C 0.0637(13) 0.5225(13) 0.2467(4) 0.211(6) Uani 0.25 1 d D U P A 2
C16C C 0.0543(18) 0.4891(16) 0.2688(4) 0.221(9) Uani 0.25 1 d D U P A 2
H16D H 0.0854 0.4515 0.2698 0.331 Uiso 0.25 1 d R U P A 2
H16E H 0.0126 0.4777 0.2763 0.331 Uiso 0.25 1 d R U P A 2
H16F H 0.0742 0.5286 0.2757 0.331 Uiso 0.25 1 d R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.948(3) 12_545 ?
Cu1 O1 1.948(3) 25_565 ?
Cu1 O2 1.964(3) 20_575 ?
Cu1 O2 1.964(3) . ?
Cu1 N1 2.202(7) . ?
Cu1 Cu1 2.6160(15) 25_565 ?
Cu2 O4 1.967(3) . ?
Cu2 O4 1.967(3) 2 ?
Cu2 O4 1.967(3) 20_565 ?
Cu2 O4 1.967(3) 19 ?
Cu2 O3 2.168(7) . ?
Cu2 Cu2 2.6305(19) 5 ?
O1 C1 1.270(5) . ?
O1 Cu1 1.948(3) 25_565 ?
O2 C1 1.242(5) . ?
O3 H3A 0.8499 . ?
O3 H3B 0.8499 . ?
O4 C12 1.246(4) . ?
O5A C15A 1.404(17) 2_565 ?
O5A C15A 1.404(17) . ?
O5A C14A 1.436(10) . ?
O5A C14A 1.436(10) 2_565 ?
O6A C15A 1.278(19) . ?
O5B C15B 1.327(13) . ?
O5B C14B 1.428(10) . ?
O5B C14B 1.429(10) 2_565 ?
C16B O6B 0.21(3) 2_565 ?
C16B C15B 1.431(9) . ?
C16B H16G 0.9598 . ?
C16B H16H 0.9602 . ?
C16B H16I 0.9602 . ?
O5C C14C 1.412(9) . ?
O5C C14C 1.412(9) 19 ?
O5C C15C 1.439(18) . ?
O5C C15C 1.439(18) 19 ?
O6C C15C 1.285(18) . ?
N1 C13C 1.230(12) . ?
N1 C13C 1.230(12) 20_575 ?
N1 C13A 1.309(18) . ?
N1 C13B 1.486(18) . ?
C1 C2 1.468(7) . ?
C2 C3 1.370(7) . ?
C2 C4 1.407(7) . ?
C3 C5 1.382(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.392(7) . ?
C4 H4 0.9300 . ?
C5 C7 1.369(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.383(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.488(7) . ?
C8 C10 1.382(7) . ?
C8 C9 1.408(6) . ?
C9 C8 1.408(6) 14_445 ?
C9 H9 0.9300 . ?
C10 C11 1.375(6) . ?
C10 H10 0.9300 . ?
C11 C10 1.375(6) 14_445 ?
C11 C12 1.483(9) . ?
C12 O4 1.246(4) 14_445 ?
C13A C13A 1.42(3) 2_565 ?
C13A C14A 1.495(10) . ?
C14A C14A 1.86(5) 2_565 ?
C14A H14A 0.9700 . ?
C14A H14B 0.9700 . ?
C15A C16A 1.38(2) . ?
C15A C15A 1.47(4) 2_565 ?
C16A C15A 1.38(2) 2_565 ?
C16A H16A 0.9600 . ?
C16A H16B 0.9600 . ?
C16A H16C 0.9593 . ?
C13B C13B 1.37(3) 2_565 ?
C13B C14B 1.494(10) . ?
C14B H14C 0.9700 . ?
C14B H14D 0.9700 . ?
C15B O6B 1.278(9) . ?
C15B O6B 1.278(9) 2_565 ?
C15B C16B 1.431(9) 2_565 ?
O6B C16B 0.21(3) 2_565 ?
C13C C14C 1.456(9) . ?
C13C C13C 1.60(2) 19 ?
C13C C14C 1.844(12) 19 ?
C14C C14C 0.797(14) 19 ?
C14C C13C 1.844(12) 19 ?
C14C H14E 0.9700 . ?
C14C H14F 0.9700 . ?
C15C C16C 1.494(14) . ?
C16C H16D 0.9600 . ?
C16C H16E 0.9600 . ?
C16C H16F 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 88.4(2) 12_545 25_565 ?
O1 Cu1 O2 168.47(15) 12_545 20_575 ?
O1 Cu1 O2 90.40(15) 25_565 20_575 ?
O1 Cu1 O2 90.41(15) 12_545 . ?
O1 Cu1 O2 168.48(15) 25_565 . ?
O2 Cu1 O2 88.4(2) 20_575 . ?
O1 Cu1 N1 96.90(17) 12_545 . ?
O1 Cu1 N1 96.90(17) 25_565 . ?
O2 Cu1 N1 94.62(17) 20_575 . ?
O2 Cu1 N1 94.62(18) . . ?
O1 Cu1 Cu1 85.92(10) 12_545 25_565 ?
O1 Cu1 Cu1 85.92(10) 25_565 25_565 ?
O2 Cu1 Cu1 82.56(10) 20_575 25_565 ?
O2 Cu1 Cu1 82.56(10) . 25_565 ?
N1 Cu1 Cu1 176.1(2) . 25_565 ?
O4 Cu2 O4 167.96(18) . 2 ?
O4 Cu2 O4 89.6(2) . 20_565 ?
O4 Cu2 O4 89.1(2) 2 20_565 ?
O4 Cu2 O4 89.1(2) . 19 ?
O4 Cu2 O4 89.6(2) 2 19 ?
O4 Cu2 O4 167.96(18) 20_565 19 ?
O4 Cu2 O3 96.02(9) . . ?
O4 Cu2 O3 96.02(9) 2 . ?
O4 Cu2 O3 96.02(9) 20_565 . ?
O4 Cu2 O3 96.02(9) 19 . ?
O4 Cu2 Cu2 83.98(9) . 5 ?
O4 Cu2 Cu2 83.98(9) 2 5 ?
O4 Cu2 Cu2 83.98(9) 20_565 5 ?
O4 Cu2 Cu2 83.98(9) 19 5 ?
O3 Cu2 Cu2 180.0 . 5 ?
C1 O1 Cu1 121.5(3) . 25_565 ?
C1 O2 Cu1 125.3(3) . . ?
Cu2 O3 H3A 120.0 . . ?
Cu2 O3 H3B 120.0 . . ?
H3A O3 H3B 120.0 . . ?
C12 O4 Cu2 123.1(4) . . ?
C15A O5A C15A 63.3(19) 2_565 . ?
C15A O5A C14A 171.2(17) 2_565 . ?
C15A O5A C14A 107.9(15) . . ?
C15A O5A C14A 107.9(15) 2_565 2_565 ?
C15A O5A C14A 171.2(17) . 2_565 ?
C14A O5A C14A 81(3) . 2_565 ?
C15B O5B C14B 129.9(11) . . ?
C15B O5B C14B 129.9(11) . 2_565 ?
C14B O5B C14B 100(2) . 2_565 ?
O6B C16B C15B 40(5) 2_565 . ?
O6B C16B H16G 68.9 2_565 . ?
C15B C16B H16G 109.1 . . ?
O6B C16B H16H 124.0 2_565 . ?
C15B C16B H16H 109.6 . . ?
H16G C16B H16H 109.5 . . ?
O6B C16B H16I 124.0 2_565 . ?
C15B C16B H16I 109.6 . . ?
H16G C16B H16I 109.5 . . ?
H16H C16B H16I 109.5 . . ?
C14C O5C C14C 32.8(6) . 19 ?
C14C O5C C15C 100.1(13) . . ?
C14C O5C C15C 131.8(13) 19 . ?
C14C O5C C15C 131.8(13) . 19 ?
C14C O5C C15C 100.1(13) 19 19 ?
C15C O5C C15C 121(2) . 19 ?
C13C N1 C13C 120.4(13) . 20_575 ?
C13A N1 C13B 118.2(11) . . ?
C13C N1 Cu1 119.8(6) . . ?
C13C N1 Cu1 119.8(7) 20_575 . ?
C13A N1 Cu1 125.9(9) . . ?
C13B N1 Cu1 115.9(7) . . ?
O2 C1 O1 124.6(5) . . ?
O2 C1 C2 117.4(5) . . ?
O1 C1 C2 117.9(5) . . ?
C3 C2 C4 117.6(5) . . ?
C3 C2 C1 121.4(5) . . ?
C4 C2 C1 121.0(5) . . ?
C2 C3 C5 122.1(5) . . ?
C2 C3 H3 118.9 . . ?
C5 C3 H3 118.9 . . ?
C6 C4 C2 119.6(5) . . ?
C6 C4 H4 120.2 . . ?
C2 C4 H4 120.2 . . ?
C7 C5 C3 120.8(6) . . ?
C7 C5 H5 119.6 . . ?
C3 C5 H5 119.6 . . ?
C7 C6 C4 121.6(5) . . ?
C7 C6 H6 119.2 . . ?
C4 C6 H6 119.2 . . ?
C5 C7 C6 118.2(5) . . ?
C5 C7 C8 120.7(5) . . ?
C6 C7 C8 121.0(5) . . ?
C10 C8 C9 117.9(5) . . ?
C10 C8 C7 121.7(5) . . ?
C9 C8 C7 120.4(5) . . ?
C8 C9 C8 120.8(7) 14_445 . ?
C8 C9 H9 119.6 14_445 . ?
C8 C9 H9 119.6 . . ?
C11 C10 C8 122.2(5) . . ?
C11 C10 H10 118.9 . . ?
C8 C10 H10 118.9 . . ?
C10 C11 C10 118.9(7) 14_445 . ?
C10 C11 C12 120.6(3) 14_445 . ?
C10 C11 C12 120.6(3) . . ?
O4 C12 O4 125.8(6) 14_445 . ?
O4 C12 C11 117.1(3) 14_445 . ?
O4 C12 C11 117.1(3) . . ?
N1 C13A C13A 122.4(8) . 2_565 ?
N1 C13A C14A 139.1(15) . . ?
C13A C13A C14A 98.5(12) 2_565 . ?
O5A C14A C13A 131(2) . . ?
O5A C14A C14A 49.6(13) . 2_565 ?
C13A C14A C14A 81.5(12) . 2_565 ?
O5A C14A H14A 104.4 . . ?
C13A C14A H14A 104.5 . . ?
C14A C14A H14A 125.4 2_565 . ?
O5A C14A H14B 104.4 . . ?
C13A C14A H14B 104.5 . . ?
C14A C14A H14B 125.4 2_565 . ?
H14A C14A H14B 105.8 . . ?
O6A C15A C16A 126.9(16) . . ?
O6A C15A O5A 117.1(18) . . ?
C16A C15A O5A 115.9(14) . . ?
O6A C15A C15A 175.4(11) . 2_565 ?
C16A C15A C15A 57.6(8) . 2_565 ?
O5A C15A C15A 58.3(9) . 2_565 ?
C15A C16A C15A 64.8(15) . 2_565 ?
C15A C16A H16A 109.4 . . ?
C15A C16A H16A 142.6 2_565 . ?
C15A C16A H16B 109.6 . . ?
C15A C16A H16B 48.9 2_565 . ?
H16A C16A H16B 109.5 . . ?
C15A C16A H16C 108.2 . . ?
C15A C16A H16C 108.2 2_565 . ?
H16A C16A H16C 108.5 . . ?
H16B C16A H16C 111.7 . . ?
C13B C13B N1 119.4(7) 2_565 . ?
C13B C13B C14B 106.0(9) 2_565 . ?
N1 C13B C14B 134.6(13) . . ?
O5B C14B C13B 113.8(18) . . ?
O5B C14B H14C 108.5 . . ?
C13B C14B H14C 108.9 . . ?
O5B C14B H14D 108.5 . . ?
C13B C14B H14D 108.9 . . ?
H14C C14B H14D 107.9 . . ?
O6B C15B O6B 116(2) . 2_565 ?
O6B C15B O5B 121.8(10) . . ?
O6B C15B O5B 121.8(10) 2_565 . ?
O6B C15B C16B 122.4(11) . . ?
O6B C15B C16B 6.1(16) 2_565 . ?
O5B C15B C16B 115.8(9) . . ?
O6B C15B C16B 6.1(16) . 2_565 ?
O6B C15B C16B 122.4(11) 2_565 2_565 ?
O5B C15B C16B 115.8(9) . 2_565 ?
C16B C15B C16B 128.5(19) . 2_565 ?
C16B O6B C15B 134(7) 2_565 . ?
N1 C13C C14C 166.2(9) . . ?
N1 C13C C13C 119.7(6) . 19 ?
C14C C13C C13C 73.9(3) . 19 ?
N1 C13C C14C 169.0(11) . 19 ?
C14C C13C C14C 24.6(3) . 19 ?
C13C C13C C14C 49.4(5) 19 19 ?
C14C C14C O5C 73.6(3) 19 . ?
C14C C14C C13C 106.1(3) 19 . ?
O5C C14C C13C 179.6(5) . . ?
C14C C14C C13C 49.4(5) 19 19 ?
O5C C14C C13C 123.0(8) . 19 ?
C13C C14C C13C 56.7(7) . 19 ?
C14C C14C H14E 153.3 19 . ?
O5C C14C H14E 89.3 . . ?
C13C C14C H14E 90.9 . . ?
C13C C14C H14E 142.1 19 . ?
C14C C14C H14F 95.9 19 . ?
O5C C14C H14F 90.2 . . ?
C13C C14C H14F 90.1 . . ?
C13C C14C H14F 95.2 19 . ?
H14E C14C H14F 104.7 . . ?
O6C C15C O5C 112.9(17) . . ?
O6C C15C C16C 118.1(16) . . ?
O5C C15C C16C 105.6(13) . . ?
C15C C16C H16D 108.3 . . ?
C15C C16C H16E 128.7 . . ?
H16D C16C H16E 109.5 . . ?
C15C C16C H16F 88.8 . . ?
H16D C16C H16F 109.5 . . ?
H16E C16C H16F 109.5 . . ?

_refine_diff_density_max         0.696
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.081

# start Validation Reply Form
_vrf_CHEMW03_2                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    8
           From the CIF: _chemical_formula_weight          1736.21
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   52.00  624.57
           H         1.01   36.00   36.29
           N        14.01    2.00   28.01
           O        16.00   17.00  271.98
           Cu       63.55    3.00  190.64
           Calculated formula weight             1151.49

RESPONSE: PLATON SQUEEZE has been employed; the removed solvent has been 
included in the formula and the calculation of derived parameters.
;

# end Validation Reply Form




####################################################################### 
# 
# 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_swy4
_database_code_depnum_ccdc_archive 'CCDC 1028543'
_audit_update_record             
;
2017-07-15 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H28 Cu3 O15, 12 C3 H7 N O'
_chemical_formula_sum            'C78 H112 Cu3 N12 O27'
_chemical_formula_weight         1840.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'

_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+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'-y+1/4, -x+1/4, -z+3/4'
'y+1/4, x+3/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'-y+3/4, -x+3/4, -z+5/4'
'y+3/4, x+5/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'y-1/4, x-1/4, z-3/4'
'-y-1/4, -x-3/4, z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'
'y+1/4, x+1/4, z-1/4'
'-y+1/4, -x-1/4, z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'

_cell_length_a                   20.009(1)
_cell_length_b                   20.009
_cell_length_c                   59.029(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     23633(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5960
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      19.29

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_F_000             7736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    0.596
_shelx_estimated_absorpt_T_min   0.755
_shelx_estimated_absorpt_T_max   0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5268
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?

_diffrn_reflns_number            79082
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_av_R_equivalents  0.1584
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_theta_min         1.380
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7172
_reflns_number_gt                3095
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1122P)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_number_reflns         7172
_refine_ls_number_parameters     140
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0643
_refine_ls_wR_factor_ref         0.2414
_refine_ls_wR_factor_gt          0.2132
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.233
_refine_ls_shift/su_max          0.058
_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 1.0000 0.93485(4) 1.00347(2) 0.0622(3) Uani 1 2 d S TU P . .
Cu2 Cu 0.5000 0.7500 0.89737(2) 0.0552(3) Uani 1 4 d S TU P . .
O1 O 0.93206(17) 0.93276(18) 0.97972(5) 0.0870(10) Uani 1 1 d . . . . .
O2 O 0.93205(17) 1.04575(18) 0.97380(5) 0.0832(10) Uani 1 1 d . . . . .
O3 O 0.56880(15) 0.81880(15) 0.89398(5) 0.0737(9) Uani 1 1 d . . . . .
O4 O 0.5000 0.7500 0.93333(14) 0.1266(12) Uani 1 4 d S TU P . .
H4A H 0.5261 0.7759 0.9405 0.152 Uiso 0.25 1 d R U P . .
H4B H 0.4739 0.7240 0.9405 0.152 Uiso 0.25 1 d R U P . .
O5 O 1.0000 0.8320(3) 1.00989(9) 0.1266(12) Uani 1 2 d S TU P . .
H5A H 0.9740 0.8063 1.0025 0.152 Uiso 0.5 1 d R U P . .
H5B H 1.0260 0.8159 1.0199 0.152 Uiso 0.5 1 d R U P . .
C1 C 0.9133(3) 0.9864(3) 0.96954(8) 0.0801(15) Uani 1 1 d . . . . .
C2 C 0.8622(2) 0.9776(3) 0.95076(7) 0.0812(14) Uani 1 1 d . . . . .
C3 C 0.8413(3) 1.0314(3) 0.93873(8) 0.0952(17) Uani 1 1 d . . . . .
H3 H 0.8559 1.0740 0.9427 0.114 Uiso 1 1 calc R U . . .
C4 C 0.7978(3) 1.0230(3) 0.92034(9) 0.1040(19) Uani 1 1 d . U . . .
H4 H 0.7845 1.0603 0.9121 0.125 Uiso 1 1 calc R U . . .
C5 C 0.7742(3) 0.9607(3) 0.91413(8) 0.0844(15) Uani 1 1 d . U . . .
C6 C 0.7957(3) 0.9065(3) 0.92724(8) 0.0989(18) Uani 1 1 d . . . . .
H6 H 0.7800 0.8640 0.9238 0.119 Uiso 1 1 calc R U . . .
C7 C 0.8395(3) 0.9142(3) 0.94524(8) 0.0985(18) Uani 1 1 d . . . . .
H7 H 0.8536 0.8772 0.9535 0.118 Uiso 1 1 calc R U . . .
C8 C 0.7312(3) 0.9509(3) 0.89404(8) 0.0791(14) Uani 1 1 d . . . . .
C9 C 0.7389(2) 0.9889(2) 0.8750 0.087(2) Uani 1 2 d S T P . .
H9 H 0.7717 1.0217 0.8750 0.104 Uiso 1 2 calc R U P . .
C10 C 0.6825(2) 0.9036(3) 0.89394(7) 0.0790(14) Uani 1 1 d . . . . .
H10 H 0.6756 0.8777 0.9068 0.095 Uiso 1 1 calc R U . . .
C11 C 0.6431(2) 0.8931(2) 0.8750 0.0690(17) Uani 1 2 d S T P . .
C12 C 0.5897(2) 0.8397(2) 0.8750 0.0697(17) Uani 1 2 d S 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 O2 1.949(3) 17_777 ?
Cu1 O2 1.949(3) 3_577 ?
Cu1 O1 1.953(3) 19_755 ?
Cu1 O1 1.953(3) . ?
Cu1 O5 2.093(5) . ?
Cu1 Cu1 2.6391(15) 17_777 ?
Cu2 O3 1.957(3) 2_665 ?
Cu2 O3 1.957(3) 20_575 ?
Cu2 O3 1.957(3) 19_655 ?
Cu2 O3 1.957(3) . ?
Cu2 O4 2.123(8) . ?
Cu2 Cu2 2.6408(18) 5_666 ?
O1 C1 1.286(6) . ?
O2 C1 1.271(6) . ?
O2 Cu1 1.949(3) 17_777 ?
O3 C12 1.267(4) . ?
O4 H4A 0.8500 . ?
O4 H4B 0.8500 . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8501 . ?
C1 C2 1.518(6) . ?
C2 C3 1.357(7) . ?
C2 C7 1.385(7) . ?
C3 C4 1.402(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.399(7) . ?
C5 C8 1.478(6) . ?
C6 C7 1.387(7) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C10 1.359(6) . ?
C8 C9 1.365(5) . ?
C9 C8 1.365(5) 14_446 ?
C9 H9 0.9300 . ?
C10 C11 1.384(5) . ?
C10 H10 0.9300 . ?
C11 C10 1.384(5) 14_446 ?
C11 C12 1.513(8) . ?
C12 O3 1.267(4) 14_446 ?

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
O2 Cu1 O2 88.4(2) 17_777 3_577 ?
O2 Cu1 O1 90.75(14) 17_777 19_755 ?
O2 Cu1 O1 169.67(15) 3_577 19_755 ?
O2 Cu1 O1 169.67(15) 17_777 . ?
O2 Cu1 O1 90.75(14) 3_577 . ?
O1 Cu1 O1 88.2(2) 19_755 . ?
O2 Cu1 O5 94.08(15) 17_777 . ?
O2 Cu1 O5 94.08(15) 3_577 . ?
O1 Cu1 O5 96.25(16) 19_755 . ?
O1 Cu1 O5 96.25(16) . . ?
O2 Cu1 Cu1 84.85(11) 17_777 17_777 ?
O2 Cu1 Cu1 84.85(11) 3_577 17_777 ?
O1 Cu1 Cu1 84.82(11) 19_755 17_777 ?
O1 Cu1 Cu1 84.82(11) . 17_777 ?
O5 Cu1 Cu1 178.50(16) . 17_777 ?
O3 Cu2 O3 89.40(18) 2_665 20_575 ?
O3 Cu2 O3 89.41(18) 2_665 19_655 ?
O3 Cu2 O3 168.28(17) 20_575 19_655 ?
O3 Cu2 O3 168.27(17) 2_665 . ?
O3 Cu2 O3 89.40(19) 20_575 . ?
O3 Cu2 O3 89.40(18) 19_655 . ?
O3 Cu2 O4 95.86(8) 2_665 . ?
O3 Cu2 O4 95.86(8) 20_575 . ?
O3 Cu2 O4 95.86(8) 19_655 . ?
O3 Cu2 O4 95.87(8) . . ?
O3 Cu2 Cu2 84.14(8) 2_665 5_666 ?
O3 Cu2 Cu2 84.14(8) 20_575 5_666 ?
O3 Cu2 Cu2 84.14(8) 19_655 5_666 ?
O3 Cu2 Cu2 84.13(8) . 5_666 ?
O4 Cu2 Cu2 180.0 . 5_666 ?
C1 O1 Cu1 121.4(3) . . ?
C1 O2 Cu1 121.9(3) . 17_777 ?
C12 O3 Cu2 123.7(3) . . ?
Cu2 O4 H4A 120.0 . . ?
Cu2 O4 H4B 120.0 . . ?
H4A O4 H4B 120.0 . . ?
Cu1 O5 H5A 120.1 . . ?
Cu1 O5 H5B 119.9 . . ?
H5A O5 H5B 120.0 . . ?
O2 C1 O1 126.9(5) . . ?
O2 C1 C2 116.9(5) . . ?
O1 C1 C2 116.2(5) . . ?
C3 C2 C7 120.2(5) . . ?
C3 C2 C1 119.8(5) . . ?
C7 C2 C1 119.9(5) . . ?
C2 C3 C4 120.1(5) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 121.7(5) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 116.5(5) . . ?
C4 C5 C8 122.0(5) . . ?
C6 C5 C8 121.4(5) . . ?
C7 C6 C5 122.2(5) . . ?
C7 C6 H6 118.9 . . ?
C5 C6 H6 118.9 . . ?
C2 C7 C6 119.3(5) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C10 C8 C9 117.7(5) . . ?
C10 C8 C5 120.8(4) . . ?
C9 C8 C5 121.5(5) . . ?
C8 C9 C8 123.6(7) . 14_446 ?
C8 C9 H9 118.2 . . ?
C8 C9 H9 118.2 14_446 . ?
C8 C10 C11 121.1(4) . . ?
C8 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C10 118.8(6) 14_446 . ?
C10 C11 C12 120.6(3) 14_446 . ?
C10 C11 C12 120.6(3) . . ?
O3 C12 O3 124.4(6) . 14_446 ?
O3 C12 C11 117.8(3) . . ?
O3 C12 C11 117.8(3) 14_446 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O2 C1 O1 3.8(7) 17_777 . . . ?
Cu1 O2 C1 C2 -177.4(3) 17_777 . . . ?
Cu1 O1 C1 O2 -3.6(7) . . . . ?
Cu1 O1 C1 C2 177.6(3) . . . . ?
O2 C1 C2 C3 3.1(7) . . . . ?
O1 C1 C2 C3 -178.0(5) . . . . ?
O2 C1 C2 C7 180.0(5) . . . . ?
O1 C1 C2 C7 -1.1(7) . . . . ?
C7 C2 C3 C4 -1.3(9) . . . . ?
C1 C2 C3 C4 175.5(5) . . . . ?
C2 C3 C4 C5 1.0(10) . . . . ?
C3 C4 C5 C6 0.4(9) . . . . ?
C3 C4 C5 C8 -176.7(6) . . . . ?
C4 C5 C6 C7 -1.4(9) . . . . ?
C8 C5 C6 C7 175.7(5) . . . . ?
C3 C2 C7 C6 0.3(9) . . . . ?
C1 C2 C7 C6 -176.5(5) . . . . ?
C5 C6 C7 C2 1.1(9) . . . . ?
C4 C5 C8 C10 -145.9(6) . . . . ?
C6 C5 C8 C10 37.2(8) . . . . ?
C4 C5 C8 C9 34.1(8) . . . . ?
C6 C5 C8 C9 -142.7(5) . . . . ?
C10 C8 C9 C8 -0.7(4) . . . 14_446 ?
C5 C8 C9 C8 179.2(6) . . . 14_446 ?
C9 C8 C10 C11 1.5(7) . . . . ?
C5 C8 C10 C11 -178.5(4) . . . . ?
C8 C10 C11 C10 -0.8(4) . . . 14_446 ?
C8 C10 C11 C12 179.2(4) . . . . ?
Cu2 O3 C12 O3 0.00(13) . . . 14_446 ?
Cu2 O3 C12 C11 180.00(13) . . . . ?
C10 C11 C12 O3 -159.9(3) 14_446 . . . ?
C10 C11 C12 O3 20.1(3) . . . . ?
C10 C11 C12 O3 20.1(3) 14_446 . . 14_446 ?
C10 C11 C12 O3 -159.9(3) . . . 14_446 ?

_refine_diff_density_max         0.517
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.067

# start Validation Reply Form
_vrf_CHEMW03_2                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    8
           From the CIF: _chemical_formula_weight          1840.41
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   42.00  504.46
           H         1.01   28.00   28.22
           O        16.00   15.00  239.99
           N        14.01    0.00    0.00
           Cu       63.55    3.00  190.64
           Calculated formula weight              963.31

RESPONSE: PLATON SQUEEZE has been employed; the removed solvent has been 
included in the formula and the calculation of derived parameters.
;
_vrf_PLAT420_2                   
;
PROBLEM: D-H Without Acceptor       O5     -- *H5A    ...     Please Check 
         D-H Without Acceptor       O5     -- *H5B    ...     Please Check 

RESPONSE: The H-bond acceptor of O -- H should be  disordered solvent molecules (DMF),
which have been squeezed by PLATON.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_swy3
_database_code_depnum_ccdc_archive 'CCDC 1028542'
_audit_update_record             
;
2017-07-15 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H30 Cu3 N2 O13, 12(C3 H7 N O)'
_chemical_formula_sum            'C86 H114 Cu3 N14 O25'
_chemical_formula_weight         1934.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   19.730(4)
_cell_length_b                   19.730(4)
_cell_length_c                   60.060(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     23380(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5236
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      19.41

_exptl_crystal_description       pillar
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_F_000             8120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.605
_shelx_estimated_absorpt_T_min   0.794
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8121
_exptl_absorpt_correction_T_max  0.9176
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and \ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            78053
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_av_R_equivalents  0.1490
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_theta_min         1.086
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7116
_reflns_number_gt                3705
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0587P)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         7116
_refine_ls_number_parameters     168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1468
_refine_ls_wR_factor_gt          0.1334
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.002
_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 0.56611(2) 0.49679(2) 0.03062(16) Uani 1 2 d S T P . .
Cu2 Cu 1.0000 0.7500 0.60305(2) 0.0305(2) Uani 1 4 d S T P . .
O1 O 0.56887(11) 0.56744(11) 0.52051(4) 0.0482(6) Uani 1 1 d . . . . .
O2 O 0.56903(11) 0.45535(11) 0.52552(4) 0.0480(6) Uani 1 1 d . . . . .
O3 O 0.92988(11) 0.68036(11) 0.60656(4) 0.0481(6) Uani 1 1 d . . . . .
O4 O 1.0000 0.7500 0.56634(9) 0.105(2) Uani 1 4 d S T P . .
H4A H 1.0290 0.7788 0.5586 0.126 Uiso 0.25 1 calc R U P . .
H4B H 0.9710 0.7212 0.5586 0.126 Uiso 0.25 1 calc R U P . .
N1 N 0.5000 0.67810(17) 0.49240(6) 0.0397(9) Uani 1 2 d S T P . .
C1 C 0.58831(17) 0.51523(18) 0.53028(5) 0.0415(8) Uani 1 1 d . . . . .
C2 C 0.63620(17) 0.52291(17) 0.54919(5) 0.0447(9) Uani 1 1 d . . . . .
C3 C 0.6568(2) 0.46645(19) 0.56095(6) 0.0649(12) Uani 1 1 d . . . . .
H3 H 0.6427 0.4235 0.5566 0.078 Uiso 1 1 calc R U . . .
C4 C 0.6987(2) 0.47417(19) 0.57933(7) 0.0709(13) Uani 1 1 d . . . . .
H4 H 0.7117 0.4360 0.5873 0.085 Uiso 1 1 calc R U . . .
C5 C 0.72191(19) 0.53805(19) 0.58620(6) 0.0567(10) Uani 1 1 d . . . . .
C6 C 0.7020(2) 0.59294(19) 0.57321(7) 0.0703(13) Uani 1 1 d . . . . .
H6 H 0.7175 0.6360 0.5769 0.084 Uiso 1 1 calc R U . . .
C7 C 0.6600(2) 0.58535(18) 0.55499(6) 0.0632(12) Uani 1 1 d . . . . .
H7 H 0.6478 0.6231 0.5466 0.076 Uiso 1 1 calc R U . . .
C8 C 0.76511(18) 0.54696(18) 0.60661(6) 0.0546(10) Uani 1 1 d . . . . .
C9 C 0.75702(17) 0.50702(17) 0.6250 0.0577(15) Uani 1 2 d S T P . .
H9 H 0.7237 0.4737 0.6250 0.069 Uiso 1 2 calc R U P . .
C10 C 0.81700(18) 0.59555(18) 0.60667(6) 0.0530(10) Uani 1 1 d . . . . .
H10 H 0.8248 0.6211 0.5939 0.064 Uiso 1 1 calc R U . . .
C11 C 0.85611(16) 0.60611(16) 0.6250 0.0437(12) Uani 1 2 d S T P . .
C12 C 0.90968(16) 0.65968(16) 0.6250 0.0395(11) Uani 1 2 d S T P . .
C13 C 0.5000 0.7133(2) 0.51097(9) 0.0613(16) Uani 1 2 d S T P . .
H13 H 0.5000 0.6904 0.5245 0.074 Uiso 1 2 calc R U P . .
C14 C 0.5000 0.7139(2) 0.47266(8) 0.0492(13) Uani 1 2 d S T P . .
C15 C 0.5000 0.6786(3) 0.45238(9) 0.086(2) Uani 1 2 d S T P . .
H15 H 0.5000 0.6314 0.4520 0.103 Uiso 1 2 calc R U P . .
C16 C 0.5000 0.7147(3) 0.43366(10) 0.155(4) Uani 1 2 d S T P . .
H16 H 0.5000 0.6920 0.4201 0.186 Uiso 1 2 calc R U 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 O2 1.957(2) 17_666 ?
Cu1 O2 1.957(2) 6_566 ?
Cu1 O1 1.969(2) . ?
Cu1 O1 1.969(2) 22_655 ?
Cu1 N1 2.225(3) . ?
Cu1 Cu1 2.6372(11) 17_666 ?
Cu2 O3 1.961(2) 10_664 ?
Cu2 O3 1.961(2) . ?
Cu2 O3 1.961(2) 22_755 ?
Cu2 O3 1.961(2) 29_565 ?
Cu2 O4 2.205(5) . ?
Cu2 Cu2 2.6368(15) 27_576 ?
O1 C1 1.246(4) . ?
O2 C1 1.273(4) . ?
O2 Cu1 1.957(2) 17_666 ?
O3 C12 1.246(3) . ?
O4 H4A 0.9300 . ?
O4 H4B 0.9300 . ?
N1 C13 1.314(6) . ?
N1 C14 1.380(6) . ?
C1 C2 1.485(4) . ?
C2 C7 1.363(4) . ?
C2 C3 1.380(5) . ?
C3 C4 1.387(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.403(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(5) . ?
C5 C8 1.504(4) . ?
C6 C7 1.381(5) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.366(4) . ?
C8 C10 1.403(5) . ?
C9 C8 1.366(4) 7_546 ?
C9 H9 0.9300 . ?
C10 C11 1.360(4) . ?
C10 H10 0.9300 . ?
C11 C10 1.361(4) 7_546 ?
C11 C12 1.495(6) . ?
C12 O3 1.246(3) 7_546 ?
C13 C13 1.448(9) 10_564 ?
C13 H13 0.9300 . ?
C14 C15 1.403(6) . ?
C14 C14 1.424(9) 10_564 ?
C15 C16 1.332(7) . ?
C15 H15 0.9300 . ?
C16 C16 1.392(12) 10_564 ?
C16 H16 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
O2 Cu1 O2 88.20(14) 17_666 6_566 ?
O2 Cu1 O1 168.13(9) 17_666 . ?
O2 Cu1 O1 91.04(10) 6_566 . ?
O2 Cu1 O1 91.04(10) 17_666 22_655 ?
O2 Cu1 O1 168.13(9) 6_566 22_655 ?
O1 Cu1 O1 87.28(14) . 22_655 ?
O2 Cu1 N1 97.68(10) 17_666 . ?
O2 Cu1 N1 97.68(10) 6_566 . ?
O1 Cu1 N1 94.16(9) . . ?
O1 Cu1 N1 94.16(9) 22_655 . ?
O2 Cu1 Cu1 83.45(7) 17_666 17_666 ?
O2 Cu1 Cu1 83.45(7) 6_566 17_666 ?
O1 Cu1 Cu1 84.69(7) . 17_666 ?
O1 Cu1 Cu1 84.70(7) 22_655 17_666 ?
N1 Cu1 Cu1 178.42(10) . 17_666 ?
O3 Cu2 O3 167.65(13) 10_664 . ?
O3 Cu2 O3 88.95(14) 10_664 22_755 ?
O3 Cu2 O3 89.72(14) . 22_755 ?
O3 Cu2 O3 89.72(14) 10_664 29_565 ?
O3 Cu2 O3 88.95(14) . 29_565 ?
O3 Cu2 O3 167.65(13) 22_755 29_565 ?
O3 Cu2 O4 96.18(6) 10_664 . ?
O3 Cu2 O4 96.17(6) . . ?
O3 Cu2 O4 96.18(6) 22_755 . ?
O3 Cu2 O4 96.18(6) 29_565 . ?
O3 Cu2 Cu2 83.82(6) 10_664 27_576 ?
O3 Cu2 Cu2 83.83(6) . 27_576 ?
O3 Cu2 Cu2 83.82(6) 22_755 27_576 ?
O3 Cu2 Cu2 83.82(6) 29_565 27_576 ?
O4 Cu2 Cu2 180.0 . 27_576 ?
C1 O1 Cu1 122.8(2) . . ?
C1 O2 Cu1 124.2(2) . 17_666 ?
C12 O3 Cu2 123.4(2) . . ?
Cu2 O4 H4A 120.0 . . ?
Cu2 O4 H4B 120.0 . . ?
H4A O4 H4B 120.0 . . ?
C13 N1 C14 117.3(4) . . ?
C13 N1 Cu1 115.1(3) . . ?
C14 N1 Cu1 127.6(3) . . ?
O1 C1 O2 124.7(3) . . ?
O1 C1 C2 118.1(3) . . ?
O2 C1 C2 117.1(3) . . ?
C7 C2 C3 119.8(3) . . ?
C7 C2 C1 120.4(3) . . ?
C3 C2 C1 119.8(3) . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C5 121.8(3) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C6 C5 C4 116.3(3) . . ?
C6 C5 C8 121.7(3) . . ?
C4 C5 C8 122.0(3) . . ?
C7 C6 C5 122.0(3) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C2 C7 C6 120.5(3) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C9 C8 C10 118.5(3) . . ?
C9 C8 C5 121.7(3) . . ?
C10 C8 C5 119.7(3) . . ?
C8 C9 C8 121.2(5) . 7_546 ?
C8 C9 H9 119.4 . . ?
C8 C9 H9 119.4 7_546 . ?
C11 C10 C8 121.4(3) . . ?
C11 C10 H10 119.3 . . ?
C8 C10 H10 119.3 . . ?
C10 C11 C10 118.8(4) . 7_546 ?
C10 C11 C12 120.6(2) . . ?
C10 C11 C12 120.6(2) 7_546 . ?
O3 C12 O3 125.5(4) 7_546 . ?
O3 C12 C11 117.3(2) 7_546 . ?
O3 C12 C11 117.2(2) . . ?
N1 C13 C13 121.9(3) . 10_564 ?
N1 C13 H13 119.0 . . ?
C13 C13 H13 119.0 10_564 . ?
N1 C14 C15 119.4(4) . . ?
N1 C14 C14 120.8(2) . 10_564 ?
C15 C14 C14 119.8(3) . 10_564 ?
C16 C15 C14 117.8(5) . . ?
C16 C15 H15 121.1 . . ?
C14 C15 H15 121.1 . . ?
C15 C16 C16 122.4(4) . 10_564 ?
C15 C16 H16 118.8 . . ?
C16 C16 H16 118.8 10_564 . ?

_refine_diff_density_max         0.414
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.063

# start Validation Reply Form
_vrf_CHEMW03_2                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    8
           From the CIF: _chemical_formula_weight          1934.53
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   50.00  600.55
           H         1.01   30.00   30.24
           N        14.01    2.00   28.01
           O        16.00   13.00  207.99
           Cu       63.55    3.00  190.64
           Calculated formula weight             1057.43

RESPONSE: PLATON SQUEEZE has been employed; the removed solvent has been 
included in the formula and the calculation of derived parameters.
;
# end Validation Reply Form



####################################################################### 
# 
# 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_swy2
_database_code_depnum_ccdc_archive 'CCDC 1028541'
_audit_update_record             
;
2017-07-15 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C96 H64 Cu6 N4 O26, 24 (C3 H7 N O)'
_chemical_formula_sum            'C168 H232 Cu6 N28 O50'
_chemical_formula_weight         3825.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'

_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+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'-y+1/4, -x+1/4, -z+3/4'
'y+1/4, x+3/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'-y+3/4, -x+3/4, -z+5/4'
'y+3/4, x+5/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'y-1/4, x-1/4, z-3/4'
'-y-1/4, -x-3/4, z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'
'y+1/4, x+1/4, z-1/4'
'-y+1/4, -x-1/4, z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'

_cell_length_a                   19.511(2)
_cell_length_b                   19.511(2)
_cell_length_c                   60.340(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     22970(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4706
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_F_000             8040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.340
_exptl_absorpt_coefficient_mu    0.615
_shelx_estimated_absorpt_T_min   0.791
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6381
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?

_diffrn_reflns_number            89079
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_av_R_equivalents  0.2180
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_theta_min         1.097
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5810
_reflns_number_gt                3170
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1491P)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_number_reflns         5810
_refine_ls_number_parameters     186
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0737
_refine_ls_wR_factor_ref         0.2569
_refine_ls_wR_factor_gt          0.2229
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.039
_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 0.31676(3) 0.2500 0.24729(2) 0.0539(3) Uani 1 2 d S T P A .
Cu2 Cu 0.5000 0.7500 0.35318(2) 0.0578(4) Uani 1 4 d S T P . .
O1 O 0.19877(18) 0.3197(2) 0.27526(5) 0.0733(11) Uani 1 1 d . . . . .
O2 O 0.31233(18) 0.3198(2) 0.27048(5) 0.0730(11) Uani 1 1 d . . . . .
O3 O 0.4302(2) 0.6799(2) 0.35658(6) 0.0792(12) Uani 1 1 d . . . . .
O4 O 0.5000 0.7500 0.31777(13) 0.133(4) Uani 1 4 d S T P . .
H4A H 0.4734 0.7232 0.3107 0.160 Uiso 0.25 1 d R U P . .
H4B H 0.5266 0.7768 0.3107 0.160 Uiso 0.25 1 d R U P . .
N1 N 0.4307(3) 0.2500 0.24492(9) 0.0656(17) Uani 1 2 d DS T P . .
C1 C 0.2581(3) 0.3389(3) 0.28013(8) 0.0681(15) Uani 1 1 d . . . . .
C2 C 0.2669(3) 0.3864(3) 0.29925(8) 0.0744(16) Uani 1 1 d . . . . .
C3 C 0.3315(3) 0.4095(4) 0.30546(10) 0.100(2) Uani 1 1 d . . . . .
H3 H 0.3695 0.3966 0.2971 0.120 Uiso 1 1 calc R U . . .
C4 C 0.2113(3) 0.4073(4) 0.31139(10) 0.096(2) Uani 1 1 d . . . . .
H4 H 0.1673 0.3939 0.3073 0.115 Uiso 1 1 calc R U . . .
C5 C 0.3407(3) 0.4510(4) 0.32357(10) 0.103(2) Uani 1 1 d . . . . .
H5 H 0.3844 0.4653 0.3275 0.124 Uiso 1 1 calc R U . . .
C6 C 0.2208(4) 0.4481(4) 0.32955(11) 0.110(3) Uani 1 1 d . . . . .
H6 H 0.1828 0.4606 0.3379 0.132 Uiso 1 1 calc R U . . .
C7 C 0.2845(4) 0.4714(4) 0.33592(10) 0.091(2) Uani 1 1 d . . . . .
C8 C 0.2957(4) 0.5142(4) 0.35625(9) 0.091(2) Uani 1 1 d . . . . .
C9 C 0.2551(3) 0.5051(3) 0.3750 0.091(3) Uani 1 2 d S T P . .
H9 H 0.2214 0.4714 0.3750 0.109 Uiso 1 2 calc R U P . .
C10 C 0.3443(3) 0.5666(3) 0.35628(9) 0.090(2) Uani 1 1 d . . . . .
H10 H 0.3693 0.5753 0.3435 0.108 Uiso 1 1 calc R U . . .
C11 C 0.3562(3) 0.6062(3) 0.3750 0.079(2) Uani 1 2 d S T P . .
C12 C 0.4097(3) 0.6597(3) 0.3750 0.069(2) Uani 1 2 d S T P . .
C13A C 0.4649(7) 0.2500 0.2661(2) 0.080(4) Uani 0.5 2 d DS TU P A 1
H13A H 0.4393 0.2500 0.2797 0.095 Uiso 0.25 2 d R U P A 2
C14A C 0.4513(17) 0.2500 0.2910(4) 0.088(6) Uani 0.25 2 d DS TU P A 1
H14A H 0.5000 0.2500 0.2992 0.131 Uiso 0.5 4 d R U P A 1
H14B H 0.4253 0.2902 0.2946 0.131 Uiso 0.125 1 d R U P A 1
H14C H 0.4253 0.2098 0.2946 0.131 Uiso 0.125 1 d R U P A 1
C13B C 0.4656(7) 0.2500 0.2268(2) 0.076(4) Uani 0.5 2 d DS TU P A 1
H13B H 0.4420 0.2500 0.2128 0.091 Uiso 0.25 2 d R U P A 2
C14B C 0.4453(17) 0.2500 0.2027(4) 0.092(8) Uani 0.25 2 d DS TU P A 1
H14D H 0.4803 0.2500 0.1915 0.137 Uiso 0.25 2 d R U P A 1
H14E H 0.4173 0.2098 0.2010 0.137 Uiso 0.125 1 d R U P A 1
H14F H 0.4173 0.2902 0.2010 0.137 Uiso 0.125 1 d R U P A 1
C13C C 0.4650(5) 0.3089(5) 0.24384(14) 0.052(2) Uani 0.5 1 d D U P A 3
H13C H 0.4405 0.3516 0.2432 0.062 Uiso 0.25 1 d R U P A 4
C14C C 0.4418(10) 0.3837(9) 0.2449(4) 0.073(5) Uani 0.25 1 d D U P A 3
H14G H 0.4798 0.4148 0.2440 0.109 Uiso 0.25 1 d R U P A 3
H14H H 0.4117 0.3909 0.2325 0.109 Uiso 0.25 1 d R U P A 3
H14I H 0.4172 0.3916 0.2584 0.109 Uiso 0.25 1 d R U P A 3


_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 1.948(4) 25 ?
Cu1 O1 1.948(4) 12_545 ?
Cu1 O2 1.954(3) . ?
Cu1 O2 1.954(3) 20_565 ?
Cu1 N1 2.227(5) . ?
Cu1 Cu1 2.6254(14) 25 ?
Cu2 O3 1.940(4) . ?
Cu2 O3 1.940(4) 2_665 ?
Cu2 O3 1.940(4) 20_575 ?
Cu2 O3 1.940(4) 19_655 ?
Cu2 O4 2.137(8) . ?
Cu2 Cu2 2.6330(19) 5_665 ?
O1 C1 1.251(6) . ?
O1 Cu1 1.948(4) 25 ?
O2 C1 1.264(6) . ?
O3 C12 1.245(5) . ?
N1 C13B 1.289(13) . ?
N1 C13C 1.333(9) . ?
N1 C13C 1.333(9) 20_565 ?
N1 C13A 1.441(13) . ?
C1 C2 1.489(7) . ?
C2 C4 1.371(7) . ?
C2 C3 1.392(8) . ?
C3 C5 1.371(8) . ?
C4 C6 1.367(8) . ?
C5 C7 1.384(9) . ?
C6 C7 1.378(9) . ?
C7 C8 1.500(8) . ?
C8 C9 1.393(7) . ?
C8 C10 1.394(8) . ?
C9 C8 1.393(7) 14_445 ?
C10 C11 1.387(7) . ?
C11 C10 1.387(7) 14_445 ?
C11 C12 1.478(11) . ?
C12 O3 1.245(5) 14_445 ?
C13A C13A 1.37(3) 2_655 ?
C13A C14A 1.524(18) . ?
C14A C14A 1.90(7) 2_655 ?
C13B C13B 1.34(3) 2_655 ?
C13B C14B 1.509(17) . ?
C13C C13C 1.366(18) 19_655 ?
C13C C14C 1.528(15) . ?

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 88.6(2) 25 12_545 ?
O1 Cu1 O2 168.50(15) 25 . ?
O1 Cu1 O2 90.37(16) 12_545 . ?
O1 Cu1 O2 90.37(16) 25 20_565 ?
O1 Cu1 O2 168.50(15) 12_545 20_565 ?
O2 Cu1 O2 88.3(2) . 20_565 ?
O1 Cu1 N1 96.33(15) 25 . ?
O1 Cu1 N1 96.33(15) 12_545 . ?
O2 Cu1 N1 95.16(15) . . ?
O2 Cu1 N1 95.16(15) 20_565 . ?
O1 Cu1 Cu1 86.15(11) 25 25 ?
O1 Cu1 Cu1 86.15(11) 12_545 25 ?
O2 Cu1 Cu1 82.36(10) . 25 ?
O2 Cu1 Cu1 82.36(10) 20_565 25 ?
N1 Cu1 Cu1 176.52(15) . 25 ?
O3 Cu2 O3 167.9(2) . 2_665 ?
O3 Cu2 O3 89.6(2) . 20_575 ?
O3 Cu2 O3 89.1(2) 2_665 20_575 ?
O3 Cu2 O3 89.1(2) . 19_655 ?
O3 Cu2 O3 89.6(2) 2_665 19_655 ?
O3 Cu2 O3 167.9(2) 20_575 19_655 ?
O3 Cu2 O4 96.06(10) . . ?
O3 Cu2 O4 96.05(10) 2_665 . ?
O3 Cu2 O4 96.05(10) 20_575 . ?
O3 Cu2 O4 96.05(10) 19_655 . ?
O3 Cu2 Cu2 83.94(10) . 5_665 ?
O3 Cu2 Cu2 83.95(10) 2_665 5_665 ?
O3 Cu2 Cu2 83.95(10) 20_575 5_665 ?
O3 Cu2 Cu2 83.95(10) 19_655 5_665 ?
O4 Cu2 Cu2 180.0 . 5_665 ?
C1 O1 Cu1 121.1(3) . 25 ?
C1 O2 Cu1 124.9(3) . . ?
C12 O3 Cu2 122.9(4) . . ?
C13C N1 C13C 119.3(9) . 20_565 ?
C13B N1 C13A 120.5(10) . . ?
C13B N1 Cu1 125.6(7) . . ?
C13C N1 Cu1 120.3(4) . . ?
C13C N1 Cu1 120.3(4) 20_565 . ?
C13A N1 Cu1 114.0(7) . . ?
O1 C1 O2 125.3(5) . . ?
O1 C1 C2 118.3(5) . . ?
O2 C1 C2 116.4(5) . . ?
C4 C2 C3 118.5(5) . . ?
C4 C2 C1 120.6(5) . . ?
C3 C2 C1 121.0(5) . . ?
C5 C3 C2 121.6(6) . . ?
C6 C4 C2 119.6(6) . . ?
C3 C5 C7 119.7(6) . . ?
C4 C6 C7 122.6(6) . . ?
C6 C7 C5 118.0(6) . . ?
C6 C7 C8 122.9(6) . . ?
C5 C7 C8 119.0(6) . . ?
C9 C8 C10 118.6(6) . . ?
C9 C8 C7 120.7(6) . . ?
C10 C8 C7 120.6(5) . . ?
C8 C9 C8 121.0(8) . 14_445 ?
C11 C10 C8 121.5(6) . . ?
C10 C11 C10 118.5(8) 14_445 . ?
C10 C11 C12 120.7(4) 14_445 . ?
C10 C11 C12 120.7(4) . . ?
O3 C12 O3 126.4(8) . 14_445 ?
O3 C12 C11 116.8(4) . . ?
O3 C12 C11 116.8(4) 14_445 . ?
C13A C13A N1 117.6(6) 2_655 . ?
C13A C13A C14A 100.0(14) 2_655 . ?
N1 C13A C14A 142.3(17) . . ?
C13A C14A C14A 80.0(14) . 2_655 ?
N1 C13B C13B 121.9(7) . 2_655 ?
N1 C13B C14B 132.9(18) . . ?
C13B C13B C14B 105.2(15) 2_655 . ?
N1 C13C C13C 120.2(4) . 19_655 ?
N1 C13C C14C 132.3(10) . . ?
C13C C13C C14C 107.2(8) 19_655 . ?

_refine_diff_density_max         1.267
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.083

# start Validation Reply Form
_vrf_CHEMW03_2                   
;
PROBLEM:  The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight          3825.04
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   96.00 1153.06
           H         1.01   64.00   64.51
           N        14.01    4.00   56.03
           O        16.00   26.00  415.97
           Cu       63.55    6.00  381.28
           Calculated formula weight             2070.85
           
RESPONSE: PLATON SQUEEZE has been employed; the removed solvent has been 
included in the formula and the calculation of derived parameters.
;

_vrf_RINTA01_ALERT_3             
;
PROBLEM:    The value of Rint is greater than 0.18
            Rint given   0.218
RESPONSE:   This problem is mainly due to the poor diffraction from the mofs with high porsity. 
;

_vrf_PLAT020_ALERT_3             
;
PROBLEM:    The value of Rint is greater than 0.12 .........      0.218 Report
RESPONSE:   This problem is mainly due to the poor diffraction from the mofs with high porsity. 
;

# end Validation Reply Form


####################################################################### 
# 
# 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_swy6
_database_code_depnum_ccdc_archive 'CCDC 1028545'
_audit_update_record             
;
2017-07-15 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C92 H58 Cu6 N6 O26, 24(C3 H7 N O)'
_chemical_formula_sum            'C164 H226 Cu6 N30 O50'
_chemical_formula_weight         3798.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'

_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+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'-y+1/4, -x+1/4, -z+3/4'
'y+1/4, x+3/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'-y+3/4, -x+3/4, -z+5/4'
'y+3/4, x+5/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'y-1/4, x-1/4, z-3/4'
'-y-1/4, -x-3/4, z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'
'y+1/4, x+1/4, z-1/4'
'-y+1/4, -x-1/4, z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'

_cell_length_a                   19.525(5)
_cell_length_b                   19.525
_cell_length_c                   60.38(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     23018(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2653
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      27.51

_exptl_crystal_description       pillar
_exptl_crystal_colour            light-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_F_000             7976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.614
_shelx_estimated_absorpt_T_min   0.791
_shelx_estimated_absorpt_T_max   0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5711
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            59272
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_av_R_equivalents  0.2023
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_theta_min         1.096
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_full        25.048
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5434
_reflns_number_gt                3041
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0794P)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_number_reflns         5434
_refine_ls_number_parameters     180
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1613
_refine_ls_wR_factor_gt          0.1542
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.002
_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 0.68294(3) 0.7500 0.75272(2) 0.0351(2) Uani 1 2 d S T P A .
Cu2 Cu 0.5000 0.2500 0.60332(2) 0.0355(3) Uani 1 4 d S T P . .
O1 O 0.80009(14) 0.68092(14) 0.72455(4) 0.0534(8) Uani 1 1 d . . . . .
O2 O 0.68755(14) 0.68005(15) 0.72942(4) 0.0553(8) Uani 1 1 d . . . . .
O3 O 0.57053(14) 0.32015(14) 0.60653(4) 0.0517(7) Uani 1 1 d . . . . .
O4 O 0.5000 0.2500 0.56713(10) 0.106(3) Uani 1 4 d S T P . .
H4A H 0.4672 0.2172 0.5618 0.160 Uiso 0.25 1 d R U P . .
H4B H 0.4880 0.2948 0.5618 0.160 Uiso 0.25 1 d R U P . .
N1 N 0.5714(2) 0.7500 0.75472(8) 0.0477(12) Uani 1 2 d DS T P . .
C1 C 0.7413(2) 0.6616(2) 0.71968(7) 0.0469(11) Uani 1 1 d . . . . .
C2 C 0.7330(2) 0.6142(2) 0.70048(7) 0.0540(12) Uani 1 1 d . . . . .
C3 C 0.6686(2) 0.5916(2) 0.69431(7) 0.0670(14) Uani 1 1 d . . . . .
H3A H 0.6304 0.6051 0.7024 0.080 Uiso 1 1 calc R U . . .
C4 C 0.7882(2) 0.5937(3) 0.68822(8) 0.0702(14) Uani 1 1 d . . . . .
H4 H 0.8320 0.6082 0.6921 0.084 Uiso 1 1 calc R U . . .
C5 C 0.6603(3) 0.5492(3) 0.67617(8) 0.0764(16) Uani 1 1 d . . . . .
H5 H 0.6166 0.5343 0.6723 0.092 Uiso 1 1 calc R U . . .
C6 C 0.7790(3) 0.5514(3) 0.67008(8) 0.0778(17) Uani 1 1 d . . . . .
H6 H 0.8172 0.5380 0.6619 0.093 Uiso 1 1 calc R U . . .
C7 C 0.7155(2) 0.5285(2) 0.66370(7) 0.0592(13) Uani 1 1 d . . . . .
C8 C 0.7057(2) 0.4858(2) 0.64407(7) 0.0597(13) Uani 1 1 d . . . . .
C9 C 0.7454(2) 0.4954(2) 0.6250 0.070(2) Uani 1 2 d S T P . .
H9 H 0.7791 0.5291 0.6250 0.083 Uiso 1 2 calc R U P . .
C10 C 0.6562(2) 0.4335(2) 0.64376(7) 0.0576(12) Uani 1 1 d . . . . .
H10 H 0.6305 0.4246 0.6564 0.069 Uiso 1 1 calc R U . . .
C11 C 0.6454(2) 0.3954(2) 0.6250 0.0504(15) Uani 1 2 d S T P . .
C12 C 0.5908(2) 0.3408(2) 0.6250 0.0454(14) Uani 1 2 d S T P . .
C13A C 0.5354(5) 0.7500 0.73558(18) 0.057(4) Uani 0.5 2 d S T P A 1
H13A H 0.5587 0.7500 0.7221 0.069 Uiso 0.5 2 calc R U P A 1
C13B C 0.5358(6) 0.7500 0.77390(19) 0.051(3) Uani 0.5 2 d S TU P A 1
H13B H 0.5589 0.7500 0.7874 0.061 Uiso 0.25 2 d R U P A 4
N2B N 0.5668(15) 0.7500 0.7942(5) 0.126(10) Uani 0.25 2 d S TU P B 5
H2B1 H 0.6108 0.7500 0.7942 0.151 Uiso 0.25 2 d R U P B 5
H2B2 H 0.5446 0.7500 0.8065 0.151 Uiso 0.25 2 d R U P B 5
C13C C 0.5397(6) 0.6967(7) 0.7567(2) 0.127(5) Uani 0.5 1 d D U P A 2
H13C H 0.5633 0.6556 0.7582 0.152 Uiso 0.375 1 calc R U P A 2
N2C N 0.559(2) 0.6254(11) 0.7586(6) 0.135(7) Uani 0.125 1 d D U P C 3
H2C1 H 0.6068 0.6203 0.7572 0.163 Uiso 0.125 1 d R U P C 3
H2C2 H 0.5338 0.5884 0.7590 0.163 Uiso 0.125 1 d R U P C 3


_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 1.953(3) 25_666 ?
Cu1 O1 1.953(3) 12_646 ?
Cu1 O2 1.962(3) 20_575 ?
Cu1 O2 1.963(3) . ?
Cu1 N1 2.181(5) . ?
Cu1 Cu1 2.6390(14) 25_666 ?
Cu2 O3 1.952(3) 2_655 ?
Cu2 O3 1.952(3) 20_565 ?
Cu2 O3 1.952(3) 19_655 ?
Cu2 O3 1.952(3) . ?
Cu2 O4 2.185(6) . ?
Cu2 Cu2 2.6185(19) 13 ?
O1 C1 1.243(5) . ?
O1 Cu1 1.953(3) 25_666 ?
O2 C1 1.256(4) . ?
O3 C12 1.250(3) . ?
N1 C13C 1.218(14) . ?
N1 C13C 1.218(14) 20_575 ?
N1 C13B 1.351(12) . ?
N1 C13A 1.353(11) . ?
C1 C2 1.492(5) . ?
C2 C4 1.368(6) . ?
C2 C3 1.384(6) . ?
C3 C5 1.383(6) . ?
C4 C6 1.384(6) . ?
C5 C7 1.376(6) . ?
C6 C7 1.373(6) . ?
C7 C8 1.461(5) . ?
C8 C9 1.401(5) . ?
C8 C10 1.407(6) . ?
C9 C8 1.401(5) 6_546 ?
C10 C11 1.371(5) . ?
C11 C10 1.371(5) 6_546 ?
C11 C12 1.508(7) . ?
C12 O3 1.250(3) 6_546 ?
C13A C13A 1.38(2) 2_665 ?
C13B C13B 1.40(2) 2_665 ?
C13C C13C 1.55(2) 19_655 ?

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 87.39(17) 25_666 12_646 ?
O1 Cu1 O2 90.87(12) 25_666 20_575 ?
O1 Cu1 O2 167.60(12) 12_646 20_575 ?
O1 Cu1 O2 167.60(12) 25_666 . ?
O1 Cu1 O2 90.87(12) 12_646 . ?
O2 Cu1 O2 88.20(17) 20_575 . ?
O1 Cu1 N1 97.49(12) 25_666 . ?
O1 Cu1 N1 97.49(12) 12_646 . ?
O2 Cu1 N1 94.91(12) 20_575 . ?
O2 Cu1 N1 94.91(12) . . ?
O1 Cu1 Cu1 85.35(9) 25_666 25_666 ?
O1 Cu1 Cu1 85.35(9) 12_646 25_666 ?
O2 Cu1 Cu1 82.27(9) 20_575 25_666 ?
O2 Cu1 Cu1 82.27(9) . 25_666 ?
N1 Cu1 Cu1 176.04(13) . 25_666 ?
O3 Cu2 O3 89.74(17) 2_655 20_565 ?
O3 Cu2 O3 89.13(17) 2_655 19_655 ?
O3 Cu2 O3 168.59(15) 20_565 19_655 ?
O3 Cu2 O3 168.59(15) 2_655 . ?
O3 Cu2 O3 89.13(17) 20_565 . ?
O3 Cu2 O3 89.74(17) 19_655 . ?
O3 Cu2 O4 95.71(8) 2_655 . ?
O3 Cu2 O4 95.71(8) 20_565 . ?
O3 Cu2 O4 95.71(8) 19_655 . ?
O3 Cu2 O4 95.70(8) . . ?
O3 Cu2 Cu2 84.29(8) 2_655 13 ?
O3 Cu2 Cu2 84.29(8) 20_565 13 ?
O3 Cu2 Cu2 84.29(8) 19_655 13 ?
O3 Cu2 Cu2 84.30(8) . 13 ?
O4 Cu2 Cu2 180.0 . 13 ?
C1 O1 Cu1 122.2(3) . 25_666 ?
C1 O2 Cu1 125.0(3) . . ?
C12 O3 Cu2 122.6(3) . . ?
C13C N1 C13C 117.6(13) . 20_575 ?
C13B N1 C13A 117.7(8) . . ?
C13C N1 Cu1 120.9(6) . . ?
C13C N1 Cu1 120.9(6) 20_575 . ?
C13B N1 Cu1 124.2(6) . . ?
C13A N1 Cu1 118.2(5) . . ?
O1 C1 O2 125.0(4) . . ?
O1 C1 C2 118.2(4) . . ?
O2 C1 C2 116.8(4) . . ?
C4 C2 C3 118.5(4) . . ?
C4 C2 C1 121.1(4) . . ?
C3 C2 C1 120.4(4) . . ?
C5 C3 C2 120.7(4) . . ?
C2 C4 C6 120.1(4) . . ?
C7 C5 C3 121.2(4) . . ?
C7 C6 C4 122.2(4) . . ?
C6 C7 C5 117.3(4) . . ?
C6 C7 C8 122.1(4) . . ?
C5 C7 C8 120.6(4) . . ?
C9 C8 C10 117.8(4) . . ?
C9 C8 C7 121.2(4) . . ?
C10 C8 C7 121.0(4) . . ?
C8 C9 C8 121.8(6) . 6_546 ?
C11 C10 C8 120.7(4) . . ?
C10 C11 C10 121.1(5) 6_546 . ?
C10 C11 C12 119.5(3) 6_546 . ?
C10 C11 C12 119.5(3) . . ?
O3 C12 O3 126.3(5) 6_546 . ?
O3 C12 C11 116.9(3) 6_546 . ?
O3 C12 C11 116.9(3) . . ?
N1 C13A C13A 121.3(5) . 2_665 ?
N1 C13B C13B 121.0(5) . 2_665 ?
N1 C13C C13C 120.6(6) . 19_655 ?

_refine_diff_density_max         0.642
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.067

# start Validation Reply Form
_vrf_CHEMW03_2                   
;
PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight          3798.97
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   92.00 1105.01
           H         1.01   58.00   58.46
           N        14.01    6.00   84.04
           O        16.00   26.00  415.97
           Cu       63.55    6.00  381.28
           Calculated formula weight             2044.77

RESPONSE: PLATON SQUEEZE has been employed; the removed solvent has been 
included in the formula and the calculation of derived parameters.
;
_vrf_RINTA01_ALERT_3             
;
PROBLEM: The value of Rint is greater than 0.18
            Rint given   0.202

RESPONSE: This problem is mainly due to the poor diffraction from the mofs with high porsity.
;
# end Validation Reply Form



#====END
