# Electronic Supplementary Material (ESI) for Materials Chemistry Frontiers.
# This journal is © the Partner Organisations 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_ST-14
_database_code_depnum_ccdc_archive 'CCDC 1573691'
_audit_update_record             
;
2017-09-09 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_audit_creation_date             2017-09-05
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.17(C252 H168 Cu12 N60 O48)'
_chemical_formula_sum            'C42 H28 Cu2 N10 O8'
_chemical_formula_weight         927.82
_chemical_absolute_configuration syn
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   27.6887(13)
_cell_length_b                   27.6887(13)
_cell_length_c                   27.6887(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     21228(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9227
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      42.824
_cell_measurement_theta_min      3.904
_shelx_estimated_absorpt_T_max   0.929
_shelx_estimated_absorpt_T_min   0.929
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.7484
_exptl_absorpt_correction_T_min  0.5677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1502 before and 0.0781 after correction. The Ratio of minimum to maximum transmission is 0.7586. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             2832
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68406
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        42.909
_diffrn_reflns_theta_max         42.909
_diffrn_reflns_theta_min         2.257
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    1.001
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2330
_reflns_number_total             2572
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.093
_refine_diff_density_rms         0.012
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2572
_refine_ls_number_restraints     134
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0200
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0241P)²+2.6021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0535
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.50(4)
 0.50(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained distances
 C11-C11_$6
 1.48 with sigma of 0.01
 N1-C10 \\sim N1-C10_$1 \\sim C10-C10_$1 \\sim C11-C9 \\sim C11-C9_$1 \\sim
C9_$1-C9
 with sigma of 0.02
 N1-C13 \\sim N1-C13_$1 \\sim C13-C13_$1 \\sim C12-C11 \\sim C11-C12_$1 \\sim
C12-C12_$1
 with sigma of 0.02
 N3_$4-N3 \\sim N3_$4-N3_$5 \\sim N3_$5-N3 \\sim C8-C8_$5 \\sim C8_$4-C8 \\sim
C8_$4-C8_$5
 with sigma of 0.02
 O2-C1 \\sim O1-C1
 with sigma of 0.02
 N1-C13 \\sim C13-C13_$1 \\sim C13_$1-N1 \\sim C12-C11 \\sim C11-C12_$1 \\sim
C12_$1-C12
 with sigma of 0.02
 N1-C12 \\sim N1-C12_$1 \\sim C13_$1-C12_$1 \\sim C13_$1-C11 \\sim C13-C11
\\sim C13-C12
 with sigma of 0.02
 N3_$4-C8 \\sim N3-C8 \\sim N3-C8_$5 \\sim N3_$5-C8_$5 \\sim N3_$5-C8_$4 \\sim
N3_$4-C8_$4
 with sigma of 0.02
 N3_$4-C8 \\sim N3_$4-C8_$4 \\sim N3_$5-C8_$4 \\sim N3_$5-C8_$5 \\sim N3-C8_$5
\\sim N3-C8
 with sigma of 0.02
 N1-C12 \\sim C13-C12 \\sim C13-C11 \\sim C13_$1-C11 \\sim C13_$1-C12_$1 \\sim
N1-C12_$1
 with sigma of 0.02
 N1-C9 \\sim C9-C10 \\sim C11-C10 \\sim C11-C10_$1 \\sim C9_$1-C10_$1 \\sim
N1-C9_$1
 with sigma of 0.02
4. Restrained planarity
 N1, C12, C12_$1, C13, C13_$1, C11
 with sigma of 0.1
 N1, C9_$1, C9, C10_$1, C10, C11
 with sigma of 0.1
 N2_$1, N2_$3, N2_$2, N3_$1, N3_$2, N3_$3, C8_$1, C8_$2, C8_$3
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(O1)
Uanis(C9) = Uanis(C10) = Uanis(C13) = Uanis(C12)
Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C7) = Uanis(C6) = Uanis(C5) =
Uanis(C1)
6. Rigid body (RIGU) restrains
 N1, C12, C9, C10, C13, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=1-FVAR(1)
 Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=FVAR(1)
8.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C6(H6), C4(H4), C3(H3), C9(H9), C12(H12), C10(H10), C13(H13)
8.b Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.20326(2) 0.0000 0.0529(2) Uani 1 2 d S T P A .
O1 O 0.52378(7) 0.20792(8) 0.06621(7) 0.0722(4) Uani 1 1 d D . . . .
O2 O 0.52543(7) 0.28866(8) 0.06681(8) 0.0722(4) Uani 1 1 d D . . . .
N1 N 0.5000 0.12537(10) 0.0000 0.0488(8) Uani 1 2 d DS TU P . .
N2 N 0.62945(11) 0.24758(11) 0.26665(10) 0.1018(11) Uani 1 1 d . . . . .
H2 H 0.6184 0.2272 0.2884 0.122 Uiso 1 1 calc R . . . .
N3 N 0.68003(14) 0.31100(15) 0.25619(10) 0.0817(9) Uani 1 1 d D . . . .
C1 C 0.53170(11) 0.24844(15) 0.08378(12) 0.0716(4) Uani 1 1 d D . . . .
C2 C 0.55492(7) 0.24869(8) 0.13437(6) 0.0716(4) Uani 1 1 d . . . . .
C7 C 0.57114(7) 0.29182(6) 0.15429(7) 0.0716(4) Uani 1 1 d G . . . .
H7 H 0.5655 0.3215 0.1379 0.086 Uiso 1 1 calc R . . . .
C6 C 0.59560(7) 0.29158(6) 0.19813(7) 0.0716(4) Uani 1 1 d G . . . .
H6 H 0.6067 0.3211 0.2117 0.086 Uiso 1 1 calc R . . . .
C5 C 0.60383(7) 0.24822(7) 0.22205(6) 0.0716(4) Uani 1 1 d G . . . .
C4 C 0.58761(7) 0.20509(6) 0.20213(7) 0.0716(4) Uani 1 1 d G . . . .
H4 H 0.5932 0.1755 0.2185 0.086 Uiso 1 1 calc R . . . .
C3 C 0.56315(7) 0.20532(6) 0.15828(7) 0.0716(4) Uani 1 1 d G . . . .
H3 H 0.5521 0.1758 0.1447 0.086 Uiso 1 1 calc R . . . .
C8 C 0.66678(13) 0.27271(18) 0.2799(2) 0.0803(11) Uani 1 1 d D . . . .
C9 C 0.4878(3) 0.10177(18) -0.0413(3) 0.0642(17) Uani 0.719(14) 1 d D U . A 1
H9 H 0.4788 0.1192 -0.0694 0.077 Uiso 0.719(14) 1 calc R . . A 1
C12 C 0.4694(5) 0.1007(4) -0.0272(5) 0.0642(17) Uani 0.281(14) 1 d D U . A 2
H12 H 0.4473 0.1175 -0.0473 0.077 Uiso 0.281(14) 1 calc R . . A 2
C10 C 0.4889(3) 0.05228(17) -0.0414(3) 0.0642(17) Uani 0.719(14) 1 d D U . A 1
H10 H 0.4819 0.0350 -0.0702 0.077 Uiso 0.719(14) 1 calc R . . A 1
C13 C 0.4691(6) 0.0525(4) -0.0269(6) 0.0642(17) Uani 0.281(14) 1 d D U . A 2
H13 H 0.4464 0.0356 -0.0462 0.077 Uiso 0.281(14) 1 calc R . . A 2
C11 C 0.5000 0.02805(11) 0.0000 0.0560(10) Uani 1 2 d DS TU 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 Cu1 2.5881(9) 22 ?
Cu1 O1 1.952(2) . ?
Cu1 O1 1.952(2) 3_655 ?
Cu1 O2 1.992(2) 22 ?
Cu1 O2 1.992(2) 24_554 ?
Cu1 N1 2.157(3) . ?
O1 C1 1.243(4) . ?
O2 Cu1 1.992(2) 22 ?
O2 C1 1.221(4) . ?
N1 C9 1.359(5) . ?
N1 C9 1.359(5) 3_655 ?
N1 C12 1.324(9) 3_655 ?
N1 C12 1.324(9) . ?
N2 H2 0.8800 . ?
N2 C5 1.424(3) . ?
N2 C8 1.299(4) . ?
N3 C8 1.350(4) 7_665 ?
N3 C8 1.299(4) . ?
C1 C2 1.541(4) . ?
C2 C7 1.3900 . ?
C2 C3 1.3900 . ?
C7 H7 0.9500 . ?
C7 C6 1.3900 . ?
C6 H6 0.9500 . ?
C6 C5 1.3900 . ?
C5 C4 1.3900 . ?
C4 H4 0.9500 . ?
C4 C3 1.3900 . ?
C3 H3 0.9500 . ?
C8 N3 1.350(4) 10_656 ?
C9 H9 0.9500 . ?
C9 C10 1.371(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.332(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.364(5) . ?
C13 H13 0.9500 . ?
C13 C11 1.322(9) . ?
C11 C10 1.364(5) 3_655 ?
C11 C13 1.322(9) 3_655 ?
C11 C11 1.554(6) 2_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 Cu1 86.22(6) . 22 ?
O1 Cu1 Cu1 86.22(6) 3_655 22 ?
O1 Cu1 O1 172.43(13) 3_655 . ?
O1 Cu1 O2 90.65(9) 3_655 24_554 ?
O1 Cu1 O2 88.51(9) 3_655 22 ?
O1 Cu1 O2 90.65(9) . 22 ?
O1 Cu1 O2 88.50(9) . 24_554 ?
O1 Cu1 N1 93.78(6) 3_655 . ?
O1 Cu1 N1 93.78(6) . . ?
O2 Cu1 Cu1 83.55(6) 22 22 ?
O2 Cu1 Cu1 83.55(6) 24_554 22 ?
O2 Cu1 O2 167.11(12) 22 24_554 ?
O2 Cu1 N1 96.45(6) 22 . ?
O2 Cu1 N1 96.45(6) 24_554 . ?
N1 Cu1 Cu1 180.0 . 22 ?
C1 O1 Cu1 119.1(2) . . ?
C1 O2 Cu1 120.7(2) . 22 ?
C9 N1 Cu1 118.7(3) 3_655 . ?
C9 N1 Cu1 118.7(3) . . ?
C9 N1 C9 122.5(5) . 3_655 ?
C12 N1 Cu1 121.1(5) . . ?
C12 N1 Cu1 121.1(5) 3_655 . ?
C12 N1 C12 117.8(10) . 3_655 ?
C5 N2 H2 115.3 . . ?
C8 N2 H2 115.3 . . ?
C8 N2 C5 129.3(3) . . ?
C8 N3 C8 115.7(4) . 7_665 ?
O1 C1 C2 115.7(3) . . ?
O2 C1 O1 130.4(3) . . ?
O2 C1 C2 113.9(3) . . ?
C7 C2 C1 120.0(2) . . ?
C7 C2 C3 120.0 . . ?
C3 C2 C1 119.8(2) . . ?
C2 C7 H7 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C5 N2 120.37(18) . . ?
C4 C5 N2 119.63(18) . . ?
C4 C5 C6 120.0 . . ?
C5 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
N2 C8 N3 121.3(5) . . ?
N2 C8 N3 114.4(5) . 10_656 ?
N3 C8 N3 124.3(4) . 10_656 ?
N1 C9 H9 120.7 . . ?
N1 C9 C10 118.6(4) . . ?
C10 C9 H9 120.7 . . ?
N1 C12 H12 119.4 . . ?
N1 C12 C13 121.2(7) . . ?
C13 C12 H12 119.4 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.6(4) . . ?
C11 C10 H10 120.2 . . ?
C12 C13 H13 119.6 . . ?
C11 C13 C12 120.8(7) . . ?
C11 C13 H13 119.6 . . ?
C10 C11 C10 121.1(5) 3_655 . ?
C10 C11 C11 119.5(3) 3_655 2_655 ?
C10 C11 C11 119.5(3) . 2_655 ?
C13 C11 C13 118.3(10) 3_655 . ?
C13 C11 C11 120.9(5) . 2_655 ?
C13 C11 C11 120.9(5) 3_655 2_655 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.954 -0.591 -0.588 16673.3 4655.6 ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.50(4)
2 0.50(4)

# start Validation Reply Form
_vrf_THETM01_ST-14               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Due to the highly porous nature of the crystal, 
diffractions at higher 2-theta angles were too weak to be incorporated
for structure determination. A resolution cut-off was applied at 1.1 angstrom.
;
# 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_ST-15
_database_code_depnum_ccdc_archive 'CCDC 1573692'
_audit_update_record             
;
2017-09-09 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_audit_creation_date             2017-09-05
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.17(C252 H168 N60 O48 Zn12)'
_chemical_formula_sum            'C42 H28 N10 O8 Zn2'
_chemical_formula_weight         931.48
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   28.1049(10)
_cell_length_b                   28.1049(10)
_cell_length_c                   28.1049(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     22200(2)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      42.78
_cell_measurement_theta_min      3.14
_shelx_estimated_absorpt_T_max   0.926
_shelx_estimated_absorpt_T_min   0.926
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.7485
_exptl_absorpt_correction_T_min  0.6136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0728 before and 0.0543 after correction. The Ratio of minimum to maximum transmission is 0.8198. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.418
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             2844
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32606
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        42.990
_diffrn_reflns_theta_max         42.990
_diffrn_reflns_theta_min         3.145
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2478
_reflns_number_total             2690
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.023
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2690
_refine_ls_number_restraints     134
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0514P)²+2.3804P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0826
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.54(5)
 0.46(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained distances
 C11-C11_$6
 1.48 with sigma of 0.01
 N1-C10 \\sim N1-C10_$1 \\sim C10-C10_$1 \\sim C11-C9 \\sim C11-C9_$1 \\sim
C9_$1-C9
 with sigma of 0.02
 N1-C13 \\sim N1-C13_$1 \\sim C13-C13_$1 \\sim C12-C11 \\sim C11-C12_$1 \\sim
C12-C12_$1
 with sigma of 0.02
 N3_$4-N3 \\sim N3_$4-N3_$5 \\sim N3_$5-N3 \\sim C8-C8_$5 \\sim C8_$4-C8 \\sim
C8_$4-C8_$5
 with sigma of 0.02
 O2-C1 \\sim O1-C1
 with sigma of 0.02
 N1-C13 \\sim C13-C13_$1 \\sim C13_$1-N1 \\sim C12-C11 \\sim C11-C12_$1 \\sim
C12_$1-C12
 with sigma of 0.02
 N1-C12 \\sim N1-C12_$1 \\sim C13_$1-C12_$1 \\sim C13_$1-C11 \\sim C13-C11
\\sim C13-C12
 with sigma of 0.02
 N3_$4-C8 \\sim N3-C8 \\sim N3-C8_$5 \\sim N3_$5-C8_$5 \\sim N3_$5-C8_$4 \\sim
N3_$4-C8_$4
 with sigma of 0.02
 N3_$4-C8 \\sim N3_$4-C8_$4 \\sim N3_$5-C8_$4 \\sim N3_$5-C8_$5 \\sim N3-C8_$5
\\sim N3-C8
 with sigma of 0.02
 N1-C12 \\sim C13-C12 \\sim C13-C11 \\sim C13_$1-C11 \\sim C13_$1-C12_$1 \\sim
N1-C12_$1
 with sigma of 0.02
 N1-C9 \\sim C9-C10 \\sim C11-C10 \\sim C11-C10_$1 \\sim C9_$1-C10_$1 \\sim
N1-C9_$1
 with sigma of 0.02
4. Restrained planarity
 N1, C12, C12_$1, C13, C13_$1, C11
 with sigma of 0.1
 N1, C9_$1, C9, C10_$1, C10, C11
 with sigma of 0.1
 N2_$1, N2_$3, N2_$2, N3_$1, N3_$2, N3_$3, C8_$1, C8_$2, C8_$3
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(O1)
Uanis(C9) = Uanis(C10) = Uanis(C13) = Uanis(C12)
Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C7) = Uanis(C6) = Uanis(C5) =
Uanis(C1)
6. Rigid body (RIGU) restrains
 N1, C12, C9, C10, C13, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=1-FVAR(1)
 Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=FVAR(1)
8.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C6(H6), C4(H4), C3(H3), C9(H9), C12(H12), C10(H10), C13(H13)
8.b Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Zn1 Zn 0.5000 0.19774(2) 0.0000 0.0284(3) Uani 1 2 d S T P A .
O1 O 0.52723(9) 0.20800(11) 0.06849(10) 0.0439(6) Uani 1 1 d D . . . .
O2 O 0.52764(9) 0.28538(10) 0.06535(10) 0.0439(6) Uani 1 1 d D . . . .
N1 N 0.5000 0.12541(14) 0.0000 0.0415(12) Uani 1 2 d DS TU P . .
N2 N 0.63200(14) 0.24484(13) 0.26257(12) 0.0477(11) Uani 1 1 d . . . . .
H2 H 0.6201 0.2246 0.2833 0.057 Uiso 1 1 calc R . . . .
N3 N 0.6851(2) 0.3070(3) 0.25345(12) 0.0518(11) Uani 1 1 d D . . . .
C1 C 0.53480(15) 0.2473(2) 0.08677(17) 0.0475(5) Uani 1 1 d D . . . .
C2 C 0.55938(9) 0.24842(11) 0.13320(8) 0.0475(5) Uani 1 1 d . . . . .
C7 C 0.57473(10) 0.29090(9) 0.15334(10) 0.0475(5) Uani 1 1 d G . . . .
H7 H 0.5685 0.3202 0.1378 0.057 Uiso 1 1 calc R . . . .
C6 C 0.59924(10) 0.29046(9) 0.19630(10) 0.0475(5) Uani 1 1 d G . . . .
H6 H 0.6097 0.3195 0.2101 0.057 Uiso 1 1 calc R . . . .
C5 C 0.60840(9) 0.24754(11) 0.21911(8) 0.0475(5) Uani 1 1 d G . . . .
C4 C 0.59304(10) 0.20506(9) 0.19897(10) 0.0475(5) Uani 1 1 d G . . . .
H4 H 0.5993 0.1757 0.2146 0.057 Uiso 1 1 calc R . . . .
C3 C 0.56854(10) 0.20550(9) 0.15601(10) 0.0475(5) Uani 1 1 d G . . . .
H3 H 0.5580 0.1765 0.1422 0.057 Uiso 1 1 calc R . . . .
C8 C 0.66955(15) 0.2685(3) 0.2765(3) 0.0458(14) Uani 1 1 d D . . . .
C9 C 0.5305(3) 0.1001(3) -0.0272(3) 0.0267(12) Uani 0.368(4) 1 d D U . A 1
H9 H 0.5540 0.1166 -0.0450 0.032 Uiso 0.368(4) 1 calc R . . A 1
C12 C 0.4899(2) 0.0997(2) -0.03897(19) 0.0267(12) Uani 0.632(4) 1 d D U . A 2
H12 H 0.4814 0.1160 -0.0673 0.032 Uiso 0.632(4) 1 calc R . . A 2
C10 C 0.5286(4) 0.0522(3) -0.0299(3) 0.0267(12) Uani 0.368(4) 1 d D U . A 1
H10 H 0.5474 0.0361 -0.0530 0.032 Uiso 0.368(4) 1 calc R . . A 1
C13 C 0.4911(2) 0.05224(19) -0.03966(19) 0.0267(12) Uani 0.632(4) 1 d D U . A 2
H13 H 0.4856 0.0361 -0.0688 0.032 Uiso 0.632(4) 1 calc R . . A 2
C11 C 0.5000 0.02643(14) 0.0000 0.0399(15) Uani 1 2 d DS TU 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
Zn1 Zn1 2.9378(13) 22 ?
Zn1 O1 2.091(3) . ?
Zn1 O1 2.091(3) 3_655 ?
Zn1 O2 2.050(3) 24_554 ?
Zn1 O2 2.050(3) 22 ?
Zn1 N1 2.033(4) . ?
O1 C1 1.238(5) . ?
O2 Zn1 2.050(3) 22 ?
O2 C1 1.243(5) . ?
N1 C9 1.350(8) 3_655 ?
N1 C9 1.350(8) . ?
N1 C12 1.343(5) 3_655 ?
N1 C12 1.343(5) . ?
N2 H2 0.8800 . ?
N2 C5 1.392(4) . ?
N2 C8 1.307(5) . ?
N3 C8 1.335(5) 7_665 ?
N3 C8 1.333(5) . ?
C1 C2 1.477(5) . ?
C2 C7 1.3900 . ?
C2 C3 1.3900 . ?
C7 H7 0.9500 . ?
C7 C6 1.3900 . ?
C6 H6 0.9500 . ?
C6 C5 1.3900 . ?
C5 C4 1.3900 . ?
C4 H4 0.9500 . ?
C4 C3 1.3900 . ?
C3 H3 0.9500 . ?
C8 N3 1.335(5) 10_656 ?
C9 H9 0.9500 . ?
C9 C10 1.350(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.335(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.371(8) . ?
C13 H13 0.9500 . ?
C13 C11 1.353(5) . ?
C11 C10 1.371(8) 3_655 ?
C11 C13 1.353(5) 3_655 ?
C11 C11 1.486(8) 2_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 Zn1 Zn1 82.07(9) 3_655 22 ?
O1 Zn1 Zn1 82.07(9) . 22 ?
O1 Zn1 O1 164.14(17) 3_655 . ?
O2 Zn1 Zn1 76.61(8) 24_554 22 ?
O2 Zn1 Zn1 76.61(8) 22 22 ?
O2 Zn1 O1 89.37(11) 22 . ?
O2 Zn1 O1 89.37(11) 24_554 3_655 ?
O2 Zn1 O1 86.97(11) 22 3_655 ?
O2 Zn1 O1 86.97(11) 24_554 . ?
O2 Zn1 O2 153.23(16) 22 24_554 ?
N1 Zn1 Zn1 180.0 . 22 ?
N1 Zn1 O1 97.93(9) . . ?
N1 Zn1 O1 97.93(9) . 3_655 ?
N1 Zn1 O2 103.39(8) . 22 ?
N1 Zn1 O2 103.39(8) . 24_554 ?
C1 O1 Zn1 124.6(3) . . ?
C1 O2 Zn1 134.0(3) . 22 ?
C9 N1 Zn1 121.7(4) . . ?
C9 N1 Zn1 121.7(4) 3_655 . ?
C9 N1 C9 116.5(8) 3_655 . ?
C12 N1 Zn1 122.5(3) . . ?
C12 N1 Zn1 122.5(3) 3_655 . ?
C12 N1 C12 114.9(6) . 3_655 ?
C5 N2 H2 115.9 . . ?
C8 N2 H2 115.9 . . ?
C8 N2 C5 128.3(5) . . ?
C8 N3 C8 120.8(4) . 7_665 ?
O1 C1 O2 122.6(5) . . ?
O1 C1 C2 117.7(5) . . ?
O2 C1 C2 119.1(5) . . ?
C7 C2 C1 121.5(3) . . ?
C7 C2 C3 120.0 . . ?
C3 C2 C1 118.4(3) . . ?
C2 C7 H7 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C5 N2 122.7(3) . . ?
C4 C5 N2 117.3(3) . . ?
C4 C5 C6 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
N2 C8 N3 118.7(9) . 10_656 ?
N2 C8 N3 122.1(9) . . ?
N3 C8 N3 119.2(4) . 10_656 ?
N1 C9 H9 118.9 . . ?
N1 C9 C10 122.2(7) . . ?
C10 C9 H9 118.9 . . ?
N1 C12 H12 118.5 . . ?
C13 C12 N1 123.0(5) . . ?
C13 C12 H12 118.5 . . ?
C9 C10 H10 119.5 . . ?
C9 C10 C11 121.0(6) . . ?
C11 C10 H10 119.5 . . ?
C12 C13 H13 119.0 . . ?
C12 C13 C11 121.9(5) . . ?
C11 C13 H13 119.0 . . ?
C10 C11 C10 116.2(8) . 3_655 ?
C10 C11 C11 121.9(4) 3_655 2_655 ?
C10 C11 C11 121.9(4) . 2_655 ?
C13 C11 C13 115.2(6) 3_655 . ?
C13 C11 C11 122.4(3) . 2_655 ?
C13 C11 C11 122.4(3) 3_655 2_655 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.490 -0.317 -0.423 17587.3 3176.8 ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.54(5)
2 0.46(5)

# start Validation Reply Form
_vrf_THETM01_ST-15               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Due to the highly porous nature of the crystal, 
diffractions at higher 2-theta angles were too weak to be incorporated
for structure determination. A resolution cut-off was applied at 1.1 angstrom.
;
# end Validation Reply Form
