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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dlk16_sq
_database_code_depnum_ccdc_archive 'CCDC 1482580'
_audit_update_record             
;
2016-05-29 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;

_audit_creation_date             2016-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C96 N12 O52 Zn16)'
_chemical_formula_sum            'C76.60 H78.20 N3 O13 Zn4'
_chemical_formula_weight         1510.30
_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 0.0030 0.0010 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3260 1.3880 '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           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, -y+1/2, -z+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-x, y+1/2, -z+1/2'
'-z, y+1/2, x+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -z, y+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -z+1/2, y'
'x+1/2, -y+1/2, -z'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-x+1/2, y+1/2, -z'
'-z+1/2, y+1/2, x'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-x, z+1/2, -y+1/2'
'-x, y+1/2, z+1/2'
'-x, -z+1/2, y+1/2'
'-z, -y+1/2, x+1/2'
'x, -y+1/2, z+1/2'
'z, -y+1/2, -x+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y, z+1/2, -x+1/2'
'-z, x+1/2, y+1/2'
'y, -z+1/2, x+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, z+1/2, x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-z, y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'y+1/2, -x, -z+1/2'
'x+1/2, y, -z+1/2'
'-y+1/2, x, -z+1/2'
'-x+1/2, z, -y+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -z, y+1/2'
'-z+1/2, -y, x+1/2'
'x+1/2, -y, z+1/2'
'z+1/2, -y, -x+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x, y+1/2'
'y+1/2, -z, x+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, z, x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'y+1/2, -x+1/2, -z'
'x+1/2, y+1/2, -z'
'-y+1/2, x+1/2, -z'
'-x+1/2, z+1/2, -y'
'-x+1/2, y+1/2, z'
'-x+1/2, -z+1/2, y'
'-z+1/2, -y+1/2, x'
'x+1/2, -y+1/2, z'
'z+1/2, -y+1/2, -x'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/2, z+1/2, -x'
'-z+1/2, x+1/2, y'
'y+1/2, -z+1/2, x'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, z+1/2, x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-z+1/2, y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   25.9940(3)
_cell_length_b                   25.9940(3)
_cell_length_c                   25.9940(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17563.8(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9423

_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.6279
_cell_measurement_theta_min      2.5189
_shelx_estimated_absorpt_T_max   0.903
_shelx_estimated_absorpt_T_min   0.867
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  1.00000

_exptl_absorpt_correction_T_min  0.76334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_exptl_crystal_description       block
_exptl_crystal_F_000             6262
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10

_exptl_special_details           
; 
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43780
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.565
_diffrn_reflns_theta_min         2.519

_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   Synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                748
_reflns_number_total             1064
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         1064
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0550
_refine_ls_restrained_S_all      1.053
_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)+(0.1119P)²+60.7871P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1969


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The optimal data collection strategy with crystals from this family is to 
use large samples, a lot of attenuation (3.75mm of aluminium in this 
instance) and a speedy data collection. This minimises the influence of 
the (extensive) diffuse scattering during integration of the intensities 
and, more importantly, provides the best means of ensuring that the data 
collection completes without catastrophic degradation of the sample by 
the X-ray beam. Thus were the data for this sample obtained, and 
integration gave a pre-squeeze R(int) of 7.34%.
Very high crystallographic symmetry coupled with disorder and a 25% 
PSM conversion meant that only the nitrogen from the pendant group on 
the ligand could be located with any certainty. This atom (N1) is present 
at 12.5% occupancy, which means that the remainder of the functionalised 
group is subject to dynamic disorder around all four carbons of the 
dicarboxylate ligand. This disorder precluded the addition of any 
hydrogen atoms to the model. Some ADP restraints were also applied to 
N1.
The residual electron density in the crystal structure was treated using 
Platon SQUEEZE which indicated a void volume of approximately 12,420 
Å3 per unit cell. This equates to a void space of 1551 Å3 per 4 zinc 
centres. Based on TGA results, 7 molecules of toluene have been included 
in the formula above, in addition to the appropriate ratio of the PSM 
derivatised ligand. The latter conversion rate was based on NMR digestion 
experiments on the crystalline material.
;
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
2. Others
 Fixed Sof: N1(0.125)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_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 0.29340(2) 0.20660(2) 0.20660(2) 0.0501(4) Uani 1 6 d S T P . .
O1 O 0.2500 0.2500 0.2500 0.052(2) Uani 1 24 d S T P . .
O2 O 0.36605(13) 0.21936(11) 0.21936(11) 0.0856(12) Uani 1 2 d S T P . .
C1 C 0.3886(2) 0.2500 0.2500 0.0739(19) Uani 1 4 d S T P . .
C2 C 0.4467(3) 0.2500 0.2500 0.083(2) Uani 1 4 d S T P . .
C3 C 0.4733(2) 0.28193(19) 0.28193(19) 0.120(3) Uani 1 2 d S T P . .
N1 N 0.4504(10) 0.3166(9) 0.3166(9) 0.170(13) Uani 0.25 2 d S TU P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0501(4) 0.0501(4) 0.0501(4) -0.00099(18) 0.00099(18) 0.00099(18)
O1 0.052(2) 0.052(2) 0.052(2) 0.000 0.000 0.000
O2 0.0481(18) 0.1043(18) 0.1043(18) -0.026(2) -0.0014(12) -0.0014(12)
C1 0.045(3) 0.088(3) 0.088(3) 0.001(4) 0.000 0.000
C2 0.049(3) 0.100(4) 0.100(4) -0.015(4) 0.000 0.000
C3 0.057(3) 0.151(5) 0.151(5) -0.074(5) 0.007(2) 0.007(2)
N1 0.072(14) 0.219(19) 0.219(19) -0.10(2) 0.011(10) 0.011(10)

_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 O1 1.9538(8) . ?
Zn1 O2 1.946(3) . ?
Zn1 O2 1.946(3) 88 ?
Zn1 O2 1.946(3) 63 ?
O1 Zn1 1.9536(8) 148 ?
O1 Zn1 1.9536(8) 75 ?
O1 Zn1 1.9536(8) 122 ?
O2 C1 1.270(5) . ?
C1 O2 1.270(5) 30 ?
C1 C2 1.509(9) . ?
C2 C3 1.363(8) . ?
C2 C3 1.363(8) 30 ?
C3 C3 1.387(12) 102_655 ?
C3 N1 1.41(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O1 111.32(13) . . ?
O2 Zn1 O1 111.32(13) 88 . ?
O2 Zn1 O1 111.32(13) 63 . ?
O2 Zn1 O2 107.56(13) . 88 ?
O2 Zn1 O2 107.56(13) . 63 ?
O2 Zn1 O2 107.56(13) 88 63 ?
Zn1 O1 Zn1 109.5 75 122 ?
Zn1 O1 Zn1 109.5 148 . ?
Zn1 O1 Zn1 109.5 148 122 ?
Zn1 O1 Zn1 109.5 122 . ?
Zn1 O1 Zn1 109.5 148 75 ?
Zn1 O1 Zn1 109.5 75 . ?
C1 O2 Zn1 131.5(4) . . ?
O2 C1 O2 125.0(6) 30 . ?
O2 C1 C2 117.5(3) . . ?
O2 C1 C2 117.5(3) 30 . ?
C3 C2 C1 120.6(4) 30 . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 C3 118.9(7) 30 . ?
C2 C3 C3 120.6(4) . 102_655 ?
C2 C3 N1 124.3(13) . . ?
C3 C3 N1 115.1(12) 102_655 . ?

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
Zn1 O2 C1 O2 0.000(0) . . . 30 ?
Zn1 O2 C1 C2 180.000(0) . . . . ?
O2 C1 C2 C3 180.000(0) . . . . ?
O2 C1 C2 C3 0.000(0) . . . 30 ?
O2 C1 C2 C3 180.000(0) 30 . . 30 ?
O2 C1 C2 C3 0.000(1) 30 . . . ?
C1 C2 C3 C3 180.000(0) . . . 102_655 ?
C1 C2 C3 N1 0.000(2) . . . . ?
C3 C2 C3 C3 0.000(1) 30 . . 102_655 ?
C3 C2 C3 N1 180.000(2) 30 . . . ?

_iucr_refine_instructions_details 
;
TITL DLK16 in Fm-3m
CELL 0.6889 25.993964 25.993964 25.993964 90 90 90
ZERR 8 0.000256 0.000256 0.000256 0 0 0
LATT 4
SYMM -Y,+X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X,+Z
SYMM +X,-Z,+Y
SYMM +X,-Y,-Z
SYMM +X,+Z,-Y
SYMM +Z,+Y,-X
SYMM -X,+Y,-Z
SYMM -Z,+Y,+X
SYMM +Z,+X,+Y
SYMM +Y,+Z,+X
SYMM -Y,-Z,+X
SYMM +Z,-X,-Y
SYMM -Y,+Z,-X
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,-Z,-X
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM -X,+Z,+Y
SYMM -X,-Z,-Y
SYMM +Z,-Y,+X
SYMM -Z,-Y,-X
SFAC C H N O Zn
DISP C 0.003 0.001 10.848
DISP H -0 0 0.623
DISP N 0.006 0.003 18.337
DISP O 0.011 0.006 30.192
DISP Zn 0.326 1.388 5404.793
UNIT 612.8 625.6 24 104 32
ISOR 0.02 0.04 N1
 
L.S. 5 0 1
PLAN  -4
SIZE 0.14 0.12 0.1
TEMP -23
GRID
BOND $H
CONF
MORE -1
ABIN
fmap 2
acta
MERG 2
SHEL 20 0.77
OMIT 2 2 2
REM <olex2.extras>
REM <HklSrc "%.\\DLK16a.hkl">
REM </olex2.extras>
 
WGHT    0.111900   60.787102
FVAR       1.12565
ZN1   5    0.293396    0.206604    0.206604    10.16667    0.05009    0.05009 =
         0.05009   -0.00099    0.00099    0.00099
O1    4    0.250000    0.250000    0.250000    10.04167    0.05156    0.05156 =
         0.05156    0.00000    0.00000    0.00000
O2    4    0.366053    0.219363    0.219363    10.50000    0.04810    0.10428 =
         0.10428   -0.02595   -0.00145   -0.00145
C1    1    0.388617    0.250000    0.250000    10.25000    0.04521    0.08828 =
         0.08828    0.00074    0.00000    0.00000
C2    1    0.446656    0.250000    0.250000    10.25000    0.04875    0.09966 =
         0.09966   -0.01515    0.00000    0.00000
C3    1    0.473328    0.281933    0.281933    10.50000    0.05706    0.15113 =
         0.15113   -0.07404    0.00693    0.00693
N1    3    0.450371    0.316603    0.316603    10.12500    0.07234    0.21945 =
         0.21945   -0.09837    0.01087    0.01087
HKLF 4
 
REM  DLK16 in Fm-3m
REM R1 =  0.0550 for     748 Fo > 4sig(Fo)  and  0.0733 for all    1064 data
REM     31 parameters refined using      6 restraints
 
END  
     
WGHT      0.1119     60.7695 

REM Highest difference peak  0.684,  deepest hole -0.428,  1-sigma level  0.063
Q1    1   0.2897  0.2103  0.1688  10.50000  0.05    0.68
Q2    1   0.2942  0.2058  0.2427  10.50000  0.05    0.50
Q3    1   0.3809  0.2082  0.2918  10.50000  0.05    0.43
Q4    1   0.3470  0.2500  0.2500  10.25000  0.05    0.32

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0550 for 748 Fo > 4sig(Fo) and 0.0733 for all 43790 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.68, deepest hole -0.43
  REM Mean Shift 0, Max Shift 0.001.
  
  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0733
  REM R1_gt = 0.0550
  REM wR_ref = 0.1969
  REM GOOF = 1.048
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 43790
  REM Reflections_gt = 748
  REM Parameters = n/a
  REM Hole = -0.43
  REM Peak = 0.68
  REM Flack = n/a
  
  
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 1 1.315
0 0 2 1.519
0 2 2 2.148
2 2 2 2.631
0 0 4 3.038

_platon_squeeze_details          
;
TITL DLK16 in Fm-3m
CELL   25.9940   25.9940   25.9940     90.00     90.00     90.00
SPGR Fm-3m
# Solvent Accessible Volume =   12690.0
# Electrons Found in S.A.V. =     117.5
# Note: Atoms in Void as Cxxx and Qxxx all others
Q101 0.294 0.206 0.206 !       1.32 eA-3
Q102 0.209 0.326 0.215 !       0.84 eA-3
Q103 0.880 0.207 0.207 !       0.80 eA-3
Q104 0.295 0.245 0.202 !       0.74 eA-3
C105 0.136 0.138 0.152 !       0.67 eA-3
Q106 0.155 0.250 0.250 !       0.58 eA-3
C107 0.347 0.403 0.156 !       0.53 eA-3
Q108 0.721 0.283 0.217 !       0.52 eA-3
;
# SQUEEZE RESULTS (Version = 110516)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.031 -0.012 -0.009 12420 251 ' '

_platon_squeeze_void_probe_radius 1.20
####################################################################### 
# 
# 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_dlk29_sq
_database_code_depnum_ccdc_archive 'CCDC 1482581'
_audit_update_record             
;
2016-05-29 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;
_audit_creation_date             2016-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C96 N12 O52 Zn16)'
_chemical_formula_sum            'C79 H83 N3 O13 Zn4'
_chemical_formula_weight         1543.96
_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 0.0030 0.0010 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3260 1.3880 '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           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, -y+1/2, -z+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-x, y+1/2, -z+1/2'
'-z, y+1/2, x+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -z, y+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -z+1/2, y'
'x+1/2, -y+1/2, -z'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-x+1/2, y+1/2, -z'
'-z+1/2, y+1/2, x'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-x, z+1/2, -y+1/2'
'-x, y+1/2, z+1/2'
'-x, -z+1/2, y+1/2'
'-z, -y+1/2, x+1/2'
'x, -y+1/2, z+1/2'
'z, -y+1/2, -x+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y, z+1/2, -x+1/2'
'-z, x+1/2, y+1/2'
'y, -z+1/2, x+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, z+1/2, x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-z, y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'y+1/2, -x, -z+1/2'
'x+1/2, y, -z+1/2'
'-y+1/2, x, -z+1/2'
'-x+1/2, z, -y+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -z, y+1/2'
'-z+1/2, -y, x+1/2'
'x+1/2, -y, z+1/2'
'z+1/2, -y, -x+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x, y+1/2'
'y+1/2, -z, x+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, z, x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'y+1/2, -x+1/2, -z'
'x+1/2, y+1/2, -z'
'-y+1/2, x+1/2, -z'
'-x+1/2, z+1/2, -y'
'-x+1/2, y+1/2, z'
'-x+1/2, -z+1/2, y'
'-z+1/2, -y+1/2, x'
'x+1/2, -y+1/2, z'
'z+1/2, -y+1/2, -x'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/2, z+1/2, -x'
'-z+1/2, x+1/2, y'
'y+1/2, -z+1/2, x'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, z+1/2, x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-z+1/2, y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   25.7627(2)
_cell_length_b                   25.7627(2)
_cell_length_c                   25.7627(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17099.2(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1971

_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      1.5
_shelx_estimated_absorpt_T_max   0.948
_shelx_estimated_absorpt_T_min   0.900
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  1.0000

_exptl_absorpt_correction_T_min  0.7745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_exptl_crystal_description       block
_exptl_crystal_F_000             6416
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05

_exptl_special_details           
; 
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0063
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34745
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         24.200
_diffrn_reflns_theta_min         2.542

_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  
;
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                713
_reflns_number_total             803
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         803
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0365
_refine_ls_restrained_S_all      1.185
_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)+(0.0655P)²+29.8484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1175

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The optimal data collection strategy with crystals from this family 
is to use large samples, a lot of attenuation (3.75mm of aluminium 
in this instance) and a speedy data collection. This minimises the 
influence of the (extensive) diffuse scattering during integration 
of the intensities and, more importantly, provides the best means 
of ensuring that the data collection completes without catastrophic 
degradation of the sample by the X-ray beam. Thus were the data for 
this sample obtained, and integration gave a pre-squeeze R(int) of 
3%.
Very high crystallographic symmetry coupled with disorder meant that 
only the nitrogen from the pendant group on the ligand could be 
located with any certainty. This atom (N1) is present at 12.5% 
occupancy, which means that the pendant group is subject to 
dynamic disorder around all four carbons of the dicarboxylate 
ligand. This disorder precluded the addition of any hydrogen 
atoms to the model.
The residual electron density in the crystal structure was 
treated using Platon SQUEEZE, which indicated a void volume 
of approximately 12003 Å3 per unit cell. This equates to a 
void space of 1500 Å3 per 4 zinc centres. There are 3 ligands 
present per 4 zincs, and 2 atoms per ligand that could not be 
reliably located and included in the model. This equates to 6 
atoms per 4 zincs and, allowing a crude atomic volume of 24 Å3,
 the ?missing? atoms account for 144 Å3 approximately. Based 
on TGA measurements, 7 toluene molecules have also been added 
to the formula per 4 zinc atoms, although the electron count 
via SQUEEZE falls somewhat short. The pre-SQUEEZE Fo-Fc showed 
that the residual electron density is very diffuse -- but 
given the nature of the samples and the well documented 
deficiencies in measuring diffraction data associated 
with MOFs of this type, the composition must be weighted 
in favour of chemical analysis. 

1H NMR analysis of the digested product indicated a 4% 
presence of ABDC versus BDC-NHEt. This (low) percentage has 
not been accounted for in this model.
;
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Others
 Fixed Sof: N1(0.125)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_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 0.29332(2) 0.20668(2) 0.20668(2) 0.0394(3) Uani 1 6 d S T P . .
O1 O 0.2500 0.2500 0.2500 0.0398(13) Uani 1 24 d S T P . .
O2 O 0.36609(8) 0.21950(7) 0.21950(7) 0.0716(7) Uani 1 2 d S T P . .
C1 C 0.38895(15) 0.2500 0.2500 0.0592(11) Uani 1 4 d S T P . .
C2 C 0.44624(17) 0.2500 0.2500 0.0670(13) Uani 1 4 d S T P . .
C3 C 0.47339(15) 0.28210(13) 0.28210(13) 0.1087(19) Uani 1 2 d S T P . .
N1 N 0.4503(7) 0.3180(5) 0.3180(5) 0.160(8) Uani 0.25 2 d S TU P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0394(3) 0.0394(3) 0.0394(3) -0.00144(11) 0.00144(11) 0.00144(11)
O1 0.0398(13) 0.0398(13) 0.0398(13) 0.000 0.000 0.000
O2 0.0368(11) 0.0891(11) 0.0891(11) -0.0230(14) 0.0010(7) 0.0010(7)
C1 0.038(2) 0.0700(17) 0.0700(17) -0.001(2) 0.000 0.000
C2 0.042(2) 0.079(2) 0.079(2) -0.007(2) 0.000 0.000
C3 0.044(2) 0.141(3) 0.141(3) -0.069(3) 0.0025(13) 0.0025(13)
N1 0.082(10) 0.198(11) 0.198(11) -0.103(13) 0.004(6) 0.004(6)

_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 3.1568(8) 75 ?
Zn1 Zn1 3.1568(8) 122 ?
Zn1 Zn1 3.1568(8) 148 ?
Zn1 O1 1.9332(5) . ?
Zn1 O2 1.932(2) 63 ?
Zn1 O2 1.932(2) . ?
Zn1 O2 1.932(2) 88 ?
O1 Zn1 1.9331(5) 148 ?
O1 Zn1 1.9331(5) 122 ?
O1 Zn1 1.9331(5) 75 ?
O2 C1 1.258(3) . ?
C1 O2 1.258(3) 30 ?
C1 C2 1.476(6) . ?
C2 C3 1.363(5) . ?
C2 C3 1.363(5) 30 ?
C3 C3 1.371(8) 102_655 ?
C3 N1 1.44(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Zn1 Zn1 Zn1 60.0 75 122 ?
Zn1 Zn1 Zn1 60.0 148 122 ?
Zn1 Zn1 Zn1 60.0 148 75 ?
O1 Zn1 Zn1 35.3 . 75 ?
O1 Zn1 Zn1 35.3 . 148 ?
O1 Zn1 Zn1 35.3 . 122 ?
O2 Zn1 Zn1 124.42(6) 88 148 ?
O2 Zn1 Zn1 76.01(8) 63 75 ?
O2 Zn1 Zn1 124.42(6) 63 122 ?
O2 Zn1 Zn1 124.42(6) 63 148 ?
O2 Zn1 Zn1 124.42(6) . 75 ?
O2 Zn1 Zn1 76.01(8) . 148 ?
O2 Zn1 Zn1 124.42(6) . 122 ?
O2 Zn1 Zn1 124.42(6) 88 75 ?
O2 Zn1 Zn1 76.01(8) 88 122 ?
O2 Zn1 O1 111.27(8) 88 . ?
O2 Zn1 O1 111.27(8) 63 . ?
O2 Zn1 O1 111.27(8) . . ?
O2 Zn1 O2 107.61(8) 88 63 ?
O2 Zn1 O2 107.61(8) 63 . ?
O2 Zn1 O2 107.61(8) 88 . ?
Zn1 O1 Zn1 109.5 75 . ?
Zn1 O1 Zn1 109.5 148 . ?
Zn1 O1 Zn1 109.5 122 . ?
Zn1 O1 Zn1 109.5 75 122 ?
Zn1 O1 Zn1 109.5 148 122 ?
Zn1 O1 Zn1 109.5 148 75 ?
C1 O2 Zn1 131.9(2) . . ?
O2 C1 O2 124.2(4) . 30 ?
O2 C1 C2 117.92(19) 30 . ?
O2 C1 C2 117.92(19) . . ?
C3 C2 C1 120.9(2) 30 . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 C3 118.2(5) 30 . ?
C2 C3 C3 120.9(2) . 102_655 ?
C2 C3 N1 124.7(8) . . ?
C3 C3 N1 114.4(8) 102_655 . ?

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
Zn1 O2 C1 O2 0.000(0) . . . 30 ?
Zn1 O2 C1 C2 180.000(0) . . . . ?
O2 C1 C2 C3 0.000(0) 30 . . . ?
O2 C1 C2 C3 180.000(0) 30 . . 30 ?
O2 C1 C2 C3 0.000(0) . . . 30 ?
O2 C1 C2 C3 180.000(0) . . . . ?
C1 C2 C3 C3 180.000(0) . . . 102_655 ?
C1 C2 C3 N1 0.000(1) . . . . ?
C3 C2 C3 C3 0.000(0) 30 . . 102_655 ?
C3 C2 C3 N1 180.000(1) 30 . . . ?

_iucr_refine_instructions_details 
;
TITL dlk29 in Fm-3m
REM dlk29 in Fm-3m
REM yellow block
CELL 0.6889 25.762711 25.762711 25.762711 90 90 90
ZERR 8 0.000247 0.000247 0.000247 0 0 0
LATT 4
SYMM -Y,+X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X,+Z
SYMM +X,-Z,+Y
SYMM +X,-Y,-Z
SYMM +X,+Z,-Y
SYMM +Z,+Y,-X
SYMM -X,+Y,-Z
SYMM -Z,+Y,+X
SYMM +Z,+X,+Y
SYMM +Y,+Z,+X
SYMM -Y,-Z,+X
SYMM +Z,-X,-Y
SYMM -Y,+Z,-X
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,-Z,-X
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM -X,+Z,+Y
SYMM -X,-Z,-Y
SYMM +Z,-Y,+X
SYMM -Z,-Y,-X
SFAC C H N O Zn
DISP C 0.003 0.001 10.848
DISP H -0 0 0.623
DISP N 0.006 0.003 18.337
DISP O 0.011 0.006 30.192
DISP Zn 0.326 1.388 5404.793
UNIT 632 664 24 104 32
ISOR 0.01 0.02 N1
 
L.S. 5 0 4
PLAN  -4
SIZE 0.1 0.1 0.05
TEMP -23
GRID
BOND $H
CONF
MORE -1
ABIN
fmap 2
acta
MERG 2
SHEL 20 0.84
REM <olex2.extras>
REM <HklSrc "%.\\dlk29.hkl">
REM </olex2.extras>
 
WGHT    0.065500   29.848400
FVAR       1.72979
ZN1   5    0.293323    0.206677    0.206677    10.16667    0.03945    0.03945 =
         0.03945   -0.00144    0.00144    0.00144
O1    4    0.250000    0.250000    0.250000    10.04167    0.03982    0.03982 =
         0.03982    0.00000    0.00000    0.00000
O2    4    0.366094    0.219499    0.219499    10.50000    0.03679    0.08906 =
         0.08906   -0.02304    0.00099    0.00099
C1    1    0.388954    0.250000    0.250000    10.25000    0.03756    0.06996 =
         0.06996   -0.00069    0.00000    0.00000
C2    1    0.446243    0.250000    0.250000    10.25000    0.04237    0.07925 =
         0.07925   -0.00743    0.00000    0.00000
C3    1    0.473391    0.282095    0.282095    10.50000    0.04367    0.14119 =
         0.14119   -0.06869    0.00254    0.00254
N1    3    0.450319    0.317994    0.317994    10.12500    0.08191    0.19845 =
         0.19845   -0.10314    0.00364    0.00364
HKLF 4
 
REM  dlk29 in Fm-3m
REM R1 =  0.0365 for     713 Fo > 4sig(Fo)  and  0.0416 for all     803 data
REM     31 parameters refined using      6 restraints
 
END  
     
WGHT      0.0655     29.8609 

REM Highest difference peak  0.434,  deepest hole -0.337,  1-sigma level  0.040
Q1    1   0.2908  0.2092  0.1686  10.50000  0.05    0.43
Q2    1   0.4782  0.3478  0.3574  11.00000  0.05    0.24
Q3    1   0.2948  0.2052  0.2441  10.50000  0.05    0.23
Q4    1   0.4495  0.2837  0.3423  11.00000  0.05    0.21

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0365 for 713 Fo > 4sig(Fo) and 0.0416 for all 52267 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.43, deepest hole -0.34
  REM Mean Shift 0, Max Shift -0.001.
  
  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0416
  REM R1_gt = 0.0365
  REM wR_ref = 0.1175
  REM GOOF = 1.155
  REM Shift_max = -0.001
  REM Shift_mean = 0
  REM Reflections_all = 52267
  REM Reflections_gt = 713
  REM Parameters = n/a
  REM Hole = -0.34
  REM Peak = 0.43
  REM Flack = n/a
  
  
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 1 1.327
0 0 2 1.532
0 2 2 2.167
2 2 2 2.655
0 0 4 3.066
0 2 4 3.428
0 4 4 4.338
1 3 5 4.537
3 3 5 5.030
1 5 5 5.479
3 5 5 5.895
5 5 5 6.649
0 0 6 4.601
3 3 7 6.283
3 5 7 6.996
5 5 7 7.645
0 0 10 7.684
0 0 12 9.233
0 2 12 9.361
2 2 12 9.488

# SQUEEZE RESULTS (Version = 110516)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.031 -0.013 -0.010 12003 680 ' '

_platon_squeeze_void_probe_radius 1.20
_diffrn_radiation_source         synchrotron
####################################################################### 
# 
# 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_dlk30_sq
_database_code_depnum_ccdc_archive 'CCDC 1482582'
_audit_update_record             
;
2016-05-29 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;
_audit_creation_date             2016-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C108 N12 O52 Zn16)'
_chemical_formula_sum            'C77.10 H83.40 N3 O13 Zn4'
_chemical_formula_weight         1521.54
_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 0.0030 0.0010 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3260 1.3880 '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           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, -y+1/2, -z+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-x, y+1/2, -z+1/2'
'-z, y+1/2, x+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -z, y+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -z+1/2, y'
'x+1/2, -y+1/2, -z'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-x+1/2, y+1/2, -z'
'-z+1/2, y+1/2, x'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-x, z+1/2, -y+1/2'
'-x, y+1/2, z+1/2'
'-x, -z+1/2, y+1/2'
'-z, -y+1/2, x+1/2'
'x, -y+1/2, z+1/2'
'z, -y+1/2, -x+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y, z+1/2, -x+1/2'
'-z, x+1/2, y+1/2'
'y, -z+1/2, x+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, z+1/2, x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-z, y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'y+1/2, -x, -z+1/2'
'x+1/2, y, -z+1/2'
'-y+1/2, x, -z+1/2'
'-x+1/2, z, -y+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -z, y+1/2'
'-z+1/2, -y, x+1/2'
'x+1/2, -y, z+1/2'
'z+1/2, -y, -x+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x, y+1/2'
'y+1/2, -z, x+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, z, x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'y+1/2, -x+1/2, -z'
'x+1/2, y+1/2, -z'
'-y+1/2, x+1/2, -z'
'-x+1/2, z+1/2, -y'
'-x+1/2, y+1/2, z'
'-x+1/2, -z+1/2, y'
'-z+1/2, -y+1/2, x'
'x+1/2, -y+1/2, z'
'z+1/2, -y+1/2, -x'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/2, z+1/2, -x'
'-z+1/2, x+1/2, y'
'y+1/2, -z+1/2, x'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, z+1/2, x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-z+1/2, y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   25.77025(14)
_cell_length_b                   25.77025(14)
_cell_length_c                   25.77025(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17114.2(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8958
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      28.7600
_cell_measurement_theta_min      2.5240
_shelx_estimated_absorpt_T_max   0.929
_shelx_estimated_absorpt_T_min   0.882
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6328
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26286
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.719
_diffrn_reflns_theta_min         2.541
_diffrn_ambient_temperature      250.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  
;
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
;
_diffrn_measurement_method       ?
# Solvent Accessible Volume = 10774
# Note: Atoms in Void as Cxxx and Qxxx all others
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1004
_reflns_number_total             1163
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         1163
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0382
_refine_ls_restrained_S_all      1.199
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0901P)²+5.2817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1370
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The optimal data collection strategy with crystals from this family is 
to use large samples, a lot of attenuation (3.75mm of aluminium in this 
instance) and a speedy data collection. This minimises the influence 
of the (extensive) diffuse scattering during integration of the 
intensities and, more importantly, provides the best means of 
ensuring that the data collection completes without catastrophic 
degradation of the sample by the X-ray beam. Thus were the data for 
this sample obtained, and integration gave a pre-squeeze R(int) of 
4.5%.

Very high crystallographic symmetry coupled with disorder precluded 
finding the pendant group on the ligand with any certainty. However, 
atom (N1) was readily located and noted as being present at 12.5% 
occupancy, which means that the pendant group is subject to dynamic 
disorder around all four carbons of the dicarboxylate ligand. A 
slightly less confident assignment has been made for C4, which 
credibly refined without distance restraints as the aliphatic carbon 
adjacent to N1.  Electron density at C4 is somewhat diffuse. N1 and 
C4 were both treated with ADP restraints. Overall, this disorder 
precluded the addition of any hydrogen atoms to the model.

The residual electron density in the crystal structure was treated 
using Platon SQUEEZE, which indicated a void volume of approximately 
10761 Å3 per unit cell. This equates to a void space of 1345 Å3 
per 4 zinc centres. There are 3 ligands present per 4 zincs, and 2 
atoms per ligand that could not be reliably located and included 
in the model. This equates to 6 atoms per 4 zincs and, allowing a 
crude atomic volume of 24Å3, the ?missing? atoms account for 
144 Å3 approximately. Based on TGA measurements, 6.3  toluene 
molecules have also been added to the formula per 4 zinc atoms, 
although the electron count via SQUEEZE falls somewhat short. 
The pre-SQUEEZE Fo-Fc showed that the residual electron density 
is very diffuse -- but given the nature of the samples and the 
well documented deficiencies in measuring diffraction data 
associated with MOFs of this type, the composition must be 
weighted in favour of chemical analysis. 

1H NMR analysis of the digested product indicated a 7% presence 
of bdc-NH2 versus bdc-NHEt. This percentage has not been accounted 
for in this model.
;
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
2. Others
 Fixed Sof: N1(0.125) C4(0.125)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_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 0.29332(2) 0.20668(2) 0.20668(2) 0.0347(2) Uani 1 6 d S T P . .
O1 O 0.2500 0.2500 0.2500 0.0318(8) Uani 1 24 d S T P . .
O2 O 0.36598(7) 0.21938(6) 0.21938(6) 0.0636(5) Uani 1 2 d S T P . .
N1 N 0.4497(5) 0.3192(4) 0.3192(4) 0.149(7) Uani 0.25 2 d S TU P . .
C1 C 0.38859(11) 0.2500 0.2500 0.0524(8) Uani 1 4 d S T P . .
C2 C 0.44609(12) 0.2500 0.2500 0.0606(9) Uani 1 4 d S T P . .
C3 C 0.47326(12) 0.28236(10) 0.28236(10) 0.0922(13) Uani 1 2 d S T P . .
C4 C 0.4764(9) 0.3540(6) 0.3540(6) 0.196(11) Uani 0.25 2 d S TU P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0347(2) 0.0347(2) 0.0347(2) -0.00154(7) 0.00154(7) 0.00154(7)
O1 0.0318(8) 0.0318(8) 0.0318(8) 0.000 0.000 0.000
O2 0.0336(8) 0.0786(8) 0.0786(8) -0.0211(10) 0.0008(5) 0.0008(5)
N1 0.048(6) 0.199(12) 0.199(12) -0.123(14) 0.003(4) 0.003(4)
C1 0.0322(13) 0.0626(12) 0.0626(12) 0.0026(16) 0.000 0.000
C2 0.0304(13) 0.0758(15) 0.0758(15) -0.0022(18) 0.000 0.000
C3 0.0351(15) 0.121(2) 0.121(2) -0.049(2) 0.0021(9) 0.0021(9)
C4 0.114(14) 0.236(15) 0.236(15) -0.142(19) 0.008(7) 0.008(7)

_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 3.1578(6) 122 ?
Zn1 Zn1 3.1578(6) 75 ?
Zn1 Zn1 3.1578(6) 148 ?
Zn1 O1 1.9337(4) . ?
Zn1 O2 1.9290(17) 63 ?
Zn1 O2 1.9290(17) 88 ?
Zn1 O2 1.9289(17) . ?
O1 Zn1 1.9337(4) 148 ?
O1 Zn1 1.9337(4) 75 ?
O1 Zn1 1.9337(4) 122 ?
O2 C1 1.259(2) . ?
N1 C3 1.474(13) . ?
N1 C4 1.44(3) . ?
C1 O2 1.259(2) 30 ?
C1 C2 1.482(4) . ?
C2 C3 1.372(4) . ?
C2 C3 1.372(4) 30 ?
C3 C3 1.378(6) 102_655 ?
C4 C4 1.22(5) 102_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
Zn1 Zn1 Zn1 60.0 148 75 ?
Zn1 Zn1 Zn1 60.0 122 75 ?
Zn1 Zn1 Zn1 60.0 148 122 ?
O1 Zn1 Zn1 35.3 . 148 ?
O1 Zn1 Zn1 35.3 . 75 ?
O1 Zn1 Zn1 35.3 . 122 ?
O2 Zn1 Zn1 76.11(6) . 148 ?
O2 Zn1 Zn1 124.50(5) 63 122 ?
O2 Zn1 Zn1 124.50(5) . 75 ?
O2 Zn1 Zn1 124.50(5) 63 148 ?
O2 Zn1 Zn1 76.11(6) 88 122 ?
O2 Zn1 Zn1 124.50(5) 88 148 ?
O2 Zn1 Zn1 124.50(5) 88 75 ?
O2 Zn1 Zn1 124.50(5) . 122 ?
O2 Zn1 Zn1 76.11(6) 63 75 ?
O2 Zn1 O1 111.37(6) . . ?
O2 Zn1 O1 111.37(6) 63 . ?
O2 Zn1 O1 111.37(6) 88 . ?
O2 Zn1 O2 107.50(7) . 63 ?
O2 Zn1 O2 107.51(7) 63 88 ?
O2 Zn1 O2 107.50(7) . 88 ?
Zn1 O1 Zn1 109.5 148 122 ?
Zn1 O1 Zn1 109.5 122 . ?
Zn1 O1 Zn1 109.5 75 . ?
Zn1 O1 Zn1 109.5 75 122 ?
Zn1 O1 Zn1 109.5 148 . ?
Zn1 O1 Zn1 109.5 148 75 ?
C1 O2 Zn1 131.45(17) . . ?
C4 N1 C3 127.2(12) . . ?
O2 C1 O2 124.9(3) 30 . ?
O2 C1 C2 117.56(14) . . ?
O2 C1 C2 117.57(14) 30 . ?
C3 C2 C1 120.69(17) 30 . ?
C3 C2 C1 120.69(17) . . ?
C3 C2 C3 118.6(3) . 30 ?
C2 C3 N1 125.0(6) . . ?
C2 C3 C3 120.70(17) . 102_655 ?
C3 C3 N1 114.3(5) 102_655 . ?
C4 C4 N1 118.5(10) 102_655 . ?

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
Zn1 O2 C1 O2 0.000(0) . . . 30 ?
Zn1 O2 C1 C2 180.000(0) . . . . ?
O2 C1 C2 C3 0.000(0) . . . 30 ?
O2 C1 C2 C3 180.000(0) 30 . . 30 ?
O2 C1 C2 C3 0.000(0) 30 . . . ?
O2 C1 C2 C3 180.000(0) . . . . ?
C1 C2 C3 N1 0.000(1) . . . . ?
C1 C2 C3 C3 180.000(0) . . . 102_655 ?
C3 N1 C4 C4 0.000(4) . . . 102_655 ?
C3 C2 C3 N1 180.000(1) 30 . . . ?
C3 C2 C3 C3 0.000(0) 30 . . 102_655 ?
C4 N1 C3 C2 180.000(1) . . . . ?
C4 N1 C3 C3 0.000(1) . . . 102_655 ?

_iucr_refine_instructions_details 
;
TITL dlk30 in Fm-3m
REM Fm-3m (#225 in standard setting)
CELL 0.6889 25.770248 25.770248 25.770248 90 90 90
ZERR 8 0.00014 0.00014 0.00014 0 0 0
LATT 4
SYMM -Y,+X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X,+Z
SYMM +X,-Z,+Y
SYMM +X,-Y,-Z
SYMM +X,+Z,-Y
SYMM +Z,+Y,-X
SYMM -X,+Y,-Z
SYMM -Z,+Y,+X
SYMM +Z,+X,+Y
SYMM +Y,+Z,+X
SYMM -Y,-Z,+X
SYMM +Z,-X,-Y
SYMM -Y,+Z,-X
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,-Z,-X
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM -X,+Z,+Y
SYMM -X,-Z,-Y
SYMM +Z,-Y,+X
SYMM -Z,-Y,-X
SFAC C H N O Zn
DISP C 0.003 0.001 10.848
DISP H -0 0 0.623
DISP N 0.006 0.003 18.337
DISP O 0.011 0.006 30.192
DISP Zn 0.326 1.388 5404.793
UNIT 616.8 667.2 24 104 32
ISOR 0.03 0.06 N1 C4
 
L.S. 14 0 3
PLAN  4
SIZE 0.1 0.12 0.07
TEMP -23
GRID
BOND $H
CONF
MORE -1
ABIN
fmap 2
acta
MERG 2
SHEL 20 0.74
OMIT 2 2 2
OMIT 4 6 6
REM <olex2.extras>
REM <HklSrc "%.\\dlk30.hkl">
REM </olex2.extras>
 
WGHT    0.090100    5.281700
FVAR       1.06177
ZN1   5    0.293323    0.206677    0.206677    10.16667    0.03468    0.03468 =
         0.03468   -0.00154    0.00154    0.00154
O1    4    0.250000    0.250000    0.250000    10.04167    0.03183    0.03183 =
         0.03183    0.00000    0.00000    0.00000
O2    4    0.365984    0.219382    0.219382    10.50000    0.03363    0.07857 =
         0.07857   -0.02109    0.00077    0.00077
N1    3    0.449686    0.319205    0.319205    10.12500    0.04828    0.19914 =
         0.19914   -0.12311    0.00280    0.00280
C1    1    0.388588    0.250000    0.250000    10.25000    0.03216    0.06257 =
         0.06257    0.00263    0.00000    0.00000
C2    1    0.446094    0.250000    0.250000    10.25000    0.03037    0.07576 =
         0.07576   -0.00220    0.00000    0.00000
C3    1    0.473263    0.282364    0.282364    10.50000    0.03511    0.12070 =
         0.12070   -0.04919    0.00214    0.00214
C4    1    0.476379    0.354002    0.354002    10.12500    0.11450    0.23606 =
         0.23606   -0.14221    0.00785    0.00785
HKLF 4
 
REM  dlk30 in Fm-3m
REM R1 =  0.0382 for    1004 Fo > 4sig(Fo)  and  0.0421 for all    1163 data
REM     37 parameters refined using     12 restraints
 
END  
     
WGHT      0.0901      5.2817 

REM Highest difference peak  0.704,  deepest hole -0.329,  1-sigma level  0.076
Q1    1   0.3894  0.3894  0.3894  10.16667  0.05    0.70
Q2    1   0.4246  0.3797  0.3903  11.00000  0.05    0.45
Q3    1   0.4179  0.2500  0.2500  10.25000  0.05    0.30
Q4    1   0.4627  0.2937  0.2937  10.50000  0.05    0.27

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0382 for 1004 Fo > 4sig(Fo) and 0.0421 for all 29526 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.70, deepest hole -0.33
  REM Mean Shift 0, Max Shift 0.000.
  
  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0421
  REM R1_gt = 0.0382
  REM wR_ref = 0.1370
  REM GOOF = 1.172
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 29526
  REM Reflections_gt = 1004
  REM Parameters = n/a
  REM Hole = -0.33
  REM Peak = 0.70
  REM Flack = n/a
  
  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_dlk12_sq
_database_code_depnum_ccdc_archive 'CCDC 1482583'
_audit_update_record             
;
2016-05-29 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C73.98 H77.40 N3 O13 Zn4'
_chemical_formula_weight         1478.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3260 1.3880 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'

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

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

_cell_length_a                   25.7752(2)
_cell_length_b                   25.7752(2)
_cell_length_c                   25.7752(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17124.0(4)
_cell_formula_units_Z            8


_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    17186
_cell_measurement_theta_min      2.5403
_cell_measurement_theta_max      26.5663

_exptl_crystal_description       block
_exptl_crystal_colour            golden
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_F_000             6130
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.071
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.76121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_type           Synchrotron
_diffrn_source                   Synchrotron
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42796
_diffrn_reflns_av_unetI/netI     0.0054
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.754
_diffrn_reflns_theta_max         26.566
_diffrn_reflns_theta_full        24.415
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             1028
_reflns_number_gt                972
_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       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The optimal data collection strategy with crystals from this family 
is to use large samples, a lot of attenuation (3.75mm of aluminium 
in this instance) and a speedy data collection. This minimises the 
influence of the (extensive) diffuse scattering during integration 
of the intensities and, more importantly, provides the best means 
of ensuring that the data collection completes without catastrophic 
degradation of the sample by the X-ray beam. 
Very high crystallographic symmetry coupled with disorder meant 
that only the amine nitrogen and carbon from the pendant group on 
the ligand could be located with any certainty. These atoms (N1 & C4) 
are present at 12.5% occupancy, which means that the remainder of  
the functionalised group is subject to dynamic disorder around all 
four carbons of the dicarboxylate ligand. This disorder precluded 
the addition of any hydrogen atoms to the model.
The residual electron density in the crystal structure was treated 
using Platon SQUEEZE which indicated a void volume of approximately 
10846 Å3 per unit cell. This equates to a void space of 1356 Å3 
per 4 zinc centres. There are 3 ligands present per 4 zincs, and 6 atoms 
per ligand that could not be reliably located and included in the 
model. This corresponds to 18 atoms per 4 zincs and, allowing a 
crude atomic volume of 24 Å3, the ?missing? atoms account for 
432 Å3 approximately. Based on TGA measurements, 4.5 toluene 
molecules have also been added to the formula per 4 zinc atoms, 
although the electron count via SQUEEZE falls somewhat short. 
The pre-SQUEEZE Fo-Fc map below shows that the residual electron 
density is very diffuse -- but given the nature of the samples 
and the well documented deficiencies in measuring diffraction 
data associated with MOFs of this type, the composition must be 
weighted in favour of chemical analysis. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1301P)²+37.3688P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1028
_refine_ls_number_parameters     37
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1973
_refine_ls_wR_factor_gt          0.1958
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.115
_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
Zn1 Zn 0.29320(2) 0.20680(2) 0.20680(2) 0.0393(4) Uani 1 6 d S T P . .
O1 O 0.2500 0.2500 0.2500 0.0347(13) Uani 1 24 d S T P . .
O2 O 0.36588(11) 0.21921(9) 0.21921(9) 0.0701(9) Uani 1 2 d S T P . .
C1 C 0.38820(18) 0.2500 0.2500 0.0607(14) Uani 1 4 d S T P . .
C2 C 0.4463(2) 0.2500 0.2500 0.0709(17) Uani 1 4 d S T P . .
C3 C 0.47328(19) 0.28259(16) 0.28259(16) 0.095(2) Uani 1 2 d S T P . .
N1 N 0.4501(9) 0.3180(7) 0.3180(7) 0.124(8) Uani 0.25 2 d S TU P . .
C4 C 0.4775(13) 0.3552(10) 0.3552(10) 0.155(13) Uani 0.25 2 d S TU P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0393(4) 0.0393(4) 0.0393(4) -0.00190(12) 0.00190(12) 0.00190(12)
O1 0.0347(13) 0.0347(13) 0.0347(13) 0.000 0.000 0.000
O2 0.0349(13) 0.0877(13) 0.0877(13) -0.0194(17) 0.0007(9) 0.0007(9)
C1 0.034(2) 0.074(2) 0.074(2) -0.001(3) 0.000 0.000
C2 0.034(2) 0.089(3) 0.089(3) -0.009(3) 0.000 0.000
C3 0.044(3) 0.120(3) 0.120(3) -0.048(4) 0.0000(14) 0.0000(14)
N1 0.073(10) 0.149(11) 0.149(11) -0.037(13) -0.010(7) -0.010(7)
C4 0.134(19) 0.166(14) 0.166(14) -0.053(16) 0.009(10) 0.009(10)

_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 O2 1.927(3) . ?
Zn1 O2 1.927(3) 63 ?
Zn1 O2 1.927(3) 88 ?
Zn1 O1 1.9285(6) . ?
Zn1 Zn1 3.1491(10) 148 ?
Zn1 Zn1 3.1491(10) 122 ?
Zn1 Zn1 3.1491(10) 75 ?
O1 Zn1 1.9284(6) 148 ?
O1 Zn1 1.9284(6) 75 ?
O1 Zn1 1.9284(6) 122 ?
O2 C1 1.261(4) . ?
C1 O2 1.261(4) 30 ?
C1 C2 1.497(7) . ?
C2 C3 1.377(6) . ?
C2 C3 1.377(6) 30 ?
C3 C3 1.377(10) 102_655 ?
C3 N1 1.42(3) . ?
N1 C4 1.53(4) . ?
C4 C4 1.16(7) 102_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
O2 Zn1 O2 107.16(11) . 63 ?
O2 Zn1 O2 107.16(11) . 88 ?
O2 Zn1 O2 107.16(11) 63 88 ?
O2 Zn1 O1 111.69(10) . . ?
O2 Zn1 O1 111.69(10) 63 . ?
O2 Zn1 O1 111.69(10) 88 . ?
O2 Zn1 Zn1 76.43(10) . 148 ?
O2 Zn1 Zn1 124.75(8) 63 148 ?
O2 Zn1 Zn1 124.75(8) 88 148 ?
O1 Zn1 Zn1 35.3 . 148 ?
O2 Zn1 Zn1 124.75(8) . 122 ?
O2 Zn1 Zn1 124.75(8) 63 122 ?
O2 Zn1 Zn1 76.43(10) 88 122 ?
O1 Zn1 Zn1 35.3 . 122 ?
Zn1 Zn1 Zn1 60.0 148 122 ?
O2 Zn1 Zn1 124.75(8) . 75 ?
O2 Zn1 Zn1 76.43(10) 63 75 ?
O2 Zn1 Zn1 124.75(8) 88 75 ?
O1 Zn1 Zn1 35.3 . 75 ?
Zn1 Zn1 Zn1 60.0 148 75 ?
Zn1 Zn1 Zn1 60.0 122 75 ?
Zn1 O1 Zn1 109.5 148 75 ?
Zn1 O1 Zn1 109.5 148 122 ?
Zn1 O1 Zn1 109.5 75 122 ?
Zn1 O1 Zn1 109.5 148 . ?
Zn1 O1 Zn1 109.5 75 . ?
Zn1 O1 Zn1 109.5 122 . ?
C1 O2 Zn1 130.7(3) . . ?
O2 C1 O2 125.7(5) . 30 ?
O2 C1 C2 117.1(2) . . ?
O2 C1 C2 117.1(2) 30 . ?
C3 C2 C3 119.3(6) . 30 ?
C3 C2 C1 120.4(3) . . ?
C3 C2 C1 120.4(3) 30 . ?
C2 C3 C3 120.4(3) . 102_655 ?
C2 C3 N1 124.8(10) . . ?
C3 C3 N1 114.8(9) 102_655 . ?
C3 N1 C4 128(2) . . ?
C4 C4 N1 117.6(16) 102_655 . ?

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
Zn1 O2 C1 O2 0.000(0) . . . 30 ?
Zn1 O2 C1 C2 180.000(0) . . . . ?
O2 C1 C2 C3 180.000(0) . . . . ?
O2 C1 C2 C3 0.000(0) 30 . . . ?
O2 C1 C2 C3 0.000(0) . . . 30 ?
O2 C1 C2 C3 180.000(0) 30 . . 30 ?
C3 C2 C3 C3 0.000(1) 30 . . 102_655 ?
C1 C2 C3 C3 180.000(0) . . . 102_655 ?
C3 C2 C3 N1 180.000(2) 30 . . . ?
C1 C2 C3 N1 0.000(2) . . . . ?
C2 C3 N1 C4 180.000(2) . . . . ?
C3 C3 N1 C4 0.000(3) 102_655 . . . ?
C3 N1 C4 C4 0.000(6) . . . 102_655 ?

_refine_diff_density_max         0.554
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.078

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 1stabs in Fm-3m
REM Fm-3m (#225 in standard setting)
CELL 0.6889 25.7752 25.7752 25.7752 90 90 90
ZERR 8 0.0002 0.0002 0.0002 0 0 0
LATT 4
SYMM -Y,+X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X,+Z
SYMM +X,-Z,+Y
SYMM +X,-Y,-Z
SYMM +X,+Z,-Y
SYMM +Z,+Y,-X
SYMM -X,+Y,-Z
SYMM -Z,+Y,+X
SYMM +Z,+X,+Y
SYMM +Y,+Z,+X
SYMM -Y,-Z,+X
SYMM +Z,-X,-Y
SYMM -Y,+Z,-X
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,-Z,-X
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM -X,+Z,+Y
SYMM -X,-Z,-Y
SYMM +Z,-Y,+X
SYMM -Z,-Y,-X
SFAC C H N O Zn
DISP C 0.003 0.001 10.848
DISP H -0 0 0.623
DISP N 0.006 0.003 18.337
DISP O 0.011 0.006 30.192
DISP Zn 0.326 1.388 5404.793
UNIT 591.84 619.2 24 104 32
ISOR 0.02 0.01 N1 C4

L.S. 15 0 2
PLAN  8
SIZE 0.12 0.12 0.1
TEMP -23
GRID
BOND $H
CONF
DAMP 3
MORE -1
ABIN
fmap 2
acta
MERG 2
SHEL 20 0.77
OMIT 2 6 6
OMIT 1 3 3
OMIT 1 1 3
REM <olex2.extras>
REM <HklSrc "%.\\dlk12_sq.hkl">
REM </olex2.extras>

WGHT    0.130100   37.368801
FVAR      13.14132
ZN1   5    0.293197    0.206803    0.206803    10.16667    0.03931    0.03931 =
         0.03931   -0.00190    0.00190    0.00190
O1    4    0.250000    0.250000    0.250000    10.04167    0.03467    0.03467 =
         0.03467    0.00000    0.00000    0.00000
O2    4    0.365882    0.219213    0.219213    10.50000    0.03493    0.08772 =
         0.08772   -0.01938    0.00067    0.00067
C1    1    0.388200    0.250000    0.250000    10.25000    0.03384    0.07409 =
         0.07409   -0.00111    0.00000    0.00000
C2    1    0.446296    0.250000    0.250000    10.25000    0.03438    0.08920 =
         0.08920   -0.00855    0.00000    0.00000
C3    1    0.473284    0.282590    0.282590    10.50000    0.04383    0.12038 =
         0.12038   -0.04771    0.00003    0.00003
N1    3    0.450098    0.318016    0.318016    10.12500    0.07252    0.14928 =
         0.14928   -0.03717   -0.00997   -0.00997
C4    1    0.477521    0.355182    0.355182    10.12500    0.13427    0.16608 =
         0.16608   -0.05328    0.00914    0.00914
HKLF 4

REM  1stabs in Fm-3m
REM R1 =  0.0534 for     972 Fo > 4sig(Fo)  and  0.0545 for all    1028 data
REM     37 parameters refined using     12 restraints

END

WGHT      0.1301     37.3856

REM Highest difference peak  0.554,  deepest hole -0.542,  1-sigma level  0.078
Q1    1   0.4158  0.4158  0.3536  10.50000  0.05    0.44
Q2    1   0.5000  0.3800  0.3967  10.50000  0.05    0.37
Q3    1   0.5000  0.5000  0.5000  10.02083  0.05    0.33
Q4    1   0.2905  0.2095  0.1765  10.50000  0.05    0.30
Q5    1   0.4486  0.2930  0.3401  11.00000  0.05    0.26
Q6    1   0.3609  0.2466  0.2107  11.00000  0.05    0.25
Q7    1   0.3317  0.2166  0.2166  10.50000  0.05    0.24
Q8    1   0.3138  0.1862  0.2832  10.50000  0.05    0.22
;
_shelx_res_checksum              92303

_shelx_fab_file                  
;
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    2    4    4     19.38      0.00
    4    4    4    -53.31      0.00
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    9   13   27      1.13      0.00
   11   13   27     -0.43      0.00
   13   13   27     -0.65      0.00
    1   15   27      0.82      0.00
    3   15   27     -0.46      0.00
    5   15   27     -0.22      0.00
    7   15   27      0.63      0.00
    9   15   27     -1.07      0.00
   11   15   27     -0.11      0.00
    1   17   27     -0.43      0.00
    3   17   27     -0.23      0.00
    5   17   27      0.62      0.00
    7   17   27     -0.43      0.00
    9   17   27      0.12      0.00
    1   19   27     -1.69      0.00
    3   19   27      1.60      0.00
    5   19   27      0.20      0.00
    0    0   28      2.99      0.00
    0    2   28      0.42      0.00
    2    2   28     -0.96      0.00
    0    4   28     -0.58      0.00
    2    4   28     -0.68      0.00
    4    4   28      3.41      0.00
    0    6   28     -0.09      0.00
    2    6   28     -1.68      0.00
    4    6   28      0.65      0.00
    6    6   28     -0.16      0.00
    0    8   28      0.83      0.00
    2    8   28      0.09      0.00
    4    8   28     -0.02      0.00
    6    8   28      1.22      0.00
    8    8   28      2.16      0.00
    0   10   28     -0.94      0.00
    2   10   28     -0.25      0.00
    4   10   28      0.05      0.00
    6   10   28      1.07      0.00
    8   10   28     -0.08      0.00
   10   10   28     -0.78      0.00
    0   12   28     -1.92      0.00
    2   12   28      0.29      0.00
    4   12   28      0.52      0.00
    6   12   28     -0.27      0.00
    8   12   28      0.34      0.00
   10   12   28     -0.23      0.00
   12   12   28     -1.40      0.00
    0   14   28     -0.15      0.00
    2   14   28     -0.41      0.00
    4   14   28     -0.27      0.00
    6   14   28     -0.36      0.00
    8   14   28     -0.27      0.00
   10   14   28     -0.73      0.00
    0   16   28      2.60      0.00
    2   16   28     -0.99      0.00
    4   16   28      0.63      0.00
    6   16   28      1.26      0.00
    8   16   28      0.28      0.00
    0   18   28      0.60      0.00
    2   18   28     -1.48      0.00
    1    1   29      0.06      0.00
    1    3   29      0.10      0.00
    3    3   29     -0.10      0.00
    1    5   29      0.75      0.00
    3    5   29     -0.15      0.00
    5    5   29     -1.51      0.00
    1    7   29      0.19      0.00
    3    7   29     -0.81      0.00
    5    7   29     -1.05      0.00
    7    7   29      0.17      0.00
    1    9   29      0.43      0.00
    3    9   29      0.22      0.00
    5    9   29      0.80      0.00
    7    9   29      0.63      0.00
    9    9   29     -1.43      0.00
    1   11   29     -0.04      0.00
    3   11   29      0.58      0.00
    5   11   29     -0.56      0.00
    7   11   29      0.98      0.00
    9   11   29      0.11      0.00
   11   11   29      0.32      0.00
    1   13   29     -0.91      0.00
    3   13   29     -0.50      0.00
    5   13   29     -1.71      0.00
    7   13   29     -0.09      0.00
    9   13   29      0.12      0.00
    1   15   29     -0.31      0.00
    3   15   29     -0.14      0.00
    5   15   29      0.42      0.00
    7   15   29     -0.12      0.00
    0    0   30      1.21      0.00
    0    2   30      1.13      0.00
    2    2   30     -0.38      0.00
    0    4   30      1.28      0.00
    2    4   30     -0.37      0.00
    4    4   30      1.39      0.00
    0    6   30     -0.14      0.00
    2    6   30     -1.86      0.00
    4    6   30     -0.38      0.00
    6    6   30     -0.86      0.00
    0    8   30      0.32      0.00
    2    8   30     -0.60      0.00
    4    8   30     -0.16      0.00
    6    8   30      0.40      0.00
    8    8   30      1.08      0.00
    0   10   30     -0.88      0.00
    2   10   30      0.89      0.00
    4   10   30     -0.38      0.00
    6   10   30     -0.05      0.00
    8   10   30      0.91      0.00
   10   10   30     -1.68      0.00
    0   12   30     -1.05      0.00
    2   12   30      1.37      0.00
    4   12   30     -0.12      0.00
    6   12   30     -0.47      0.00
    8   12   30      0.56      0.00
    0   14   30      0.13      0.00
    2   14   30      0.17      0.00
    4   14   30     -0.17      0.00
    1    1   31     -0.55      0.00
    1    3   31     -0.37      0.00
    3    3   31     -0.91      0.00
    1    5   31     -0.47      0.00
    3    5   31     -0.33      0.00
    5    5   31      0.29      0.00
    1    7   31      0.92      0.00
    3    7   31      0.26      0.00
    5    7   31     -0.52      0.00
    7    7   31     -0.34      0.00
    1    9   31      0.02      0.00
    3    9   31      0.35      0.00
    5    9   31     -1.06      0.00
    7    9   31      0.63      0.00
    1   11   31     -0.94      0.00
    3   11   31      0.12      0.00
    5   11   31     -1.44      0.00
    0    0   32     -1.20      0.00
    0    2   32      0.39      0.00
    2    2   32      0.15      0.00
    0    4   32      1.54      0.00
    2    4   32     -0.27      0.00
    4    4   32     -0.52      0.00
    0    6   32     -0.81      0.00
    2    6   32     -1.82      0.00
    4    6   32     -1.26      0.00
    6    6   32     -1.13      0.00
    0    8   32     -0.68      0.00
    2    8   32     -0.34      0.00
    4    8   32     -1.16      0.00
    1    1   33      0.35      0.00
    1    3   33     -0.73      0.00
    3    3   33     -0.99      0.00
    1    5   33     -2.22      0.00
    1    1    1    124.95      0.00
    0    0    2    110.95      0.00
    0    2    2      4.25      0.00
    2    2    2    -61.94      0.00
    1    1    3    -60.18      0.00
    1    3    3     68.98      0.00
    0    0    4    -46.48      0.00
    0    2    4     66.34      0.00
    0    4    4    126.98      0.00
    3    3    5     13.54      0.00
    1    5    5     11.25      0.00
    5    5    5     18.04      0.00
    0    0    6     94.76      0.00
    2    6    6     18.19      0.00
    0    0   12     49.21      0.00
   18   20   20     -0.64      0.00
   18   18   22     -0.14      0.00
    8   22   24      0.98      0.00
   14   16   26      0.11      0.00
   13   15   27      1.02      0.00
   12   14   28     -0.41      0.00
    4   18   28     -0.71      0.00
   11   13   29      0.17      0.00
    1   17   29     -0.27      0.00
    6   14   30     -1.14      0.00
    9    9   31      0.25      0.00
    7   11   31      1.33      0.00
    1   13   31     -1.32      0.00
    6    8   32     -0.93      0.00
    0   10   32     -1.84      0.00
    2   10   32      0.02      0.00
    3    5   33     -0.80      0.00
    0    0    0      0.00      0.00
# SQUEEZE RESULTS (Version = 110516)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.092 -0.035 -0.024     10846       375 ' '
   2  0.129  0.129  0.371         5         0 ' '
   3  0.129  0.129  0.629         5         0 ' '
   4  0.129  0.371  0.129         5         0 ' '
   5  0.129  0.371  0.871         5         0 ' '
   6  0.129  0.629  0.129         5         0 ' '
   7  0.129  0.629  0.871         5         0 ' '
   8  0.129  0.871  0.371         5         0 ' '
   9  0.129  0.871  0.629         5         0 ' '
  10  0.371  0.129  0.129         5         0 ' '
  11  0.371  0.129  0.871         5         0 ' '
  12  0.371  0.371  0.371         5         0 ' '
  13  0.371  0.371  0.629         5         0 ' '
  14  0.371  0.629  0.371         5         0 ' '
  15  0.371  0.629  0.629         5         0 ' '
  16  0.371  0.871  0.129         5         0 ' '
  17  0.371  0.871  0.871         5         0 ' '
  18  0.629  0.129  0.129         5         0 ' '
  19  0.629  0.129  0.871         5         0 ' '
  20  0.629  0.371  0.371         5         0 ' '
  21  0.629  0.371  0.629         5         0 ' '
  22  0.629  0.629  0.371         5         0 ' '
  23  0.629  0.629  0.629         5         0 ' '
  24  0.629  0.871  0.129         5         0 ' '
  25  0.629  0.871  0.871         5         0 ' '
  26  0.871  0.129  0.371         5         0 ' '
  27  0.871  0.129  0.629         5         0 ' '
  28  0.871  0.371  0.129         5         0 ' '
  29  0.871  0.371  0.871         5         0 ' '
  30  0.871  0.629  0.129         5         0 ' '
  31  0.871  0.629  0.871         5         0 ' '
  32  0.871  0.871  0.371         5         0 ' '
  33  0.871  0.871  0.629         5         0 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
  _platon_missing_refln_index_h
  _platon_missing_refln_index_k
  _platon_missing_refln_index_l
  _platon_missing_refln_theta
    1    1    1     1.326
    0    0    2     1.532
    0    2    2     2.166
    2    2    2     2.653
    1    1    3     2.540
    1    3    3     3.339
    0    0    4     3.064
    0    2    4     3.426
    0    4    4     4.335
    3    3    5     5.027
    1    5    5     5.476
    5    5    5     6.646
    0    0    6     4.599
    2    6    6     6.690
    0    0   12     9.228
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details
;
# Solvent Accessible Volume =     11083
# Note: Atoms in Void as Cxxx and Qxxx all others
_shelx_fab_checksum              43780
_diffrn_radiation_monochromator  Synchrotron
_diffrn_measurement_device       
;
CrystalLogic Kappa (3 circle)
;
####################################################################### 
# 
# 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_dlk11_sq
_database_code_depnum_ccdc_archive 'CCDC 1482584'
_audit_update_record             
;
2016-05-29 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78.10 H74.60 N3 O13 S1.95 Zn4'
_chemical_formula_weight         1587.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1180 0.1170 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3260 1.3880 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'

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

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

_cell_length_a                   25.8577(2)
_cell_length_b                   25.8577(2)
_cell_length_c                   25.8577(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17289.0(4)
_cell_formula_units_Z            8

_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    13993
_cell_measurement_theta_min      2.5322
_cell_measurement_theta_max      24.2141

_exptl_crystal_description       blocks
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_F_000             6555
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.107
_shelx_estimated_absorpt_T_min   0.879
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_type           Synchrotron
_diffrn_source                   Synchrotron
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34574
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.527
_diffrn_reflns_theta_max         24.201
_diffrn_reflns_theta_full        24.415
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             824
_reflns_number_gt                816
_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       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The optimal data collection strategy with crystals from this 
family is to use large samples, a lot of attenuation (3.75mm of 
aluminium in this instance) and a speedy data collection. This 
minimises the influence of the (extensive) diffuse scattering 
during integration of the intensities and, more importantly, 
provides the best means of ensuring that the data collection 
completes without catastrophic degradation of the sample by 
the X-ray beam. Thus were the data for this sample obtained, 
and integration gave a pre-squeeze R(int) of 9%.
Very high crystallographic symmetry coupled with disorder meant 
that only the nitrogen from the pendant group on the ligand could 
be located with any certainty. This atom (N1) is present at 12.5% 
occupancy, which means that the pendant group is subject to dynamic 
disorder around all four carbons of the dicarboxylate ligand. This 
disorder precluded the addition of any hydrogen atoms to the model.
The residual electron density in the crystal structure was treated 
using Platon SQUEEZE which indicated a void volume of 
approximately 12094 Å3 per unit cell. 
This equates to a void space of 1512 Å3 per 4 zinc 
centres. There are 3 ligands present per 4 zincs, and 9 atoms per 
ligand that could not be reliably located and included in the model. 
This equates to 27 atoms per 4 zincs and, allowing a crude atomic 
volume of 24 Å3, the ?missing? atoms account for 650 Å3 approximately. 
Based on TGA measurements, 6 toluene molecules have also been added 
to the formula per 4 zinc atoms, although the electron count via SQUEEZE 
falls somewhat short. The pre-SQUEEZE Fo-Fc map below shows that the 
residual electron density is very diffuse -- but given the nature of the 
samples and the well documented deficiencies in measuring diffraction 
data associated with MOFs of this type, the composition must be weighted 
in favour of chemical analysis. 

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1173P)²+36.0469P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         824
_refine_ls_number_parameters     31
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.2064
_refine_ls_wR_factor_gt          0.1951
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_restrained_S_all      1.227
_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
Zn1 Zn 0.29319(2) 0.20681(2) 0.20681(2) 0.0608(5) Uani 1 6 d S T P . .
O1 O 0.2500 0.2500 0.2500 0.0479(19) Uani 1 24 d S T P . .
O2 O 0.36614(16) 0.21843(14) 0.21843(14) 0.1030(15) Uani 1 2 d S T P . .
C1 C 0.3881(3) 0.2500 0.2500 0.091(2) Uani 1 4 d S T P . .
C2 C 0.4467(3) 0.2500 0.2500 0.092(2) Uani 1 4 d S T P . .
C3 C 0.4736(3) 0.2826(2) 0.2826(2) 0.127(3) Uani 1 2 d S T P . .
N1 N 0.4509(9) 0.3204(9) 0.3204(9) 0.175(15) Uani 0.25 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0608(5) 0.0608(5) 0.0608(5) -0.00301(19) 0.00301(19) 0.00301(19)
O1 0.0479(19) 0.0479(19) 0.0479(19) 0.000 0.000 0.000
O2 0.053(2) 0.128(2) 0.128(2) -0.013(3) -0.0047(15) -0.0047(15)
C1 0.052(4) 0.111(4) 0.111(4) -0.004(5) 0.000 0.000
C2 0.058(4) 0.109(4) 0.109(4) -0.005(5) 0.000 0.000
C3 0.057(4) 0.162(5) 0.162(5) -0.031(6) -0.010(3) -0.010(3)
N1 0.060(13) 0.23(2) 0.23(2) -0.09(3) -0.001(10) -0.001(10)

_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 O2 1.934(4) . ?
Zn1 O2 1.934(4) 88 ?
Zn1 O2 1.934(4) 63 ?
Zn1 O1 1.9341(9) . ?
Zn1 Zn1 3.1585(15) 148 ?
Zn1 Zn1 3.1585(15) 75 ?
Zn1 Zn1 3.1585(15) 122 ?
O1 Zn1 1.9342(9) 148 ?
O1 Zn1 1.9342(9) 122 ?
O1 Zn1 1.9342(9) 75 ?
O2 C1 1.287(5) . ?
C1 O2 1.287(5) 30 ?
C1 C2 1.514(10) . ?
C2 C3 1.381(9) . ?
C2 C3 1.381(9) 30 ?
C3 C3 1.363(14) 102_655 ?
C3 N1 1.50(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O2 106.19(17) . 88 ?
O2 Zn1 O2 106.19(17) . 63 ?
O2 Zn1 O2 106.19(17) 88 63 ?
O2 Zn1 O1 112.58(16) . . ?
O2 Zn1 O1 112.58(16) 88 . ?
O2 Zn1 O1 112.58(16) 63 . ?
O2 Zn1 Zn1 77.31(16) . 148 ?
O2 Zn1 Zn1 125.45(12) 88 148 ?
O2 Zn1 Zn1 125.45(12) 63 148 ?
O1 Zn1 Zn1 35.3 . 148 ?
O2 Zn1 Zn1 125.45(12) . 75 ?
O2 Zn1 Zn1 125.45(12) 88 75 ?
O2 Zn1 Zn1 77.31(16) 63 75 ?
O1 Zn1 Zn1 35.3 . 75 ?
Zn1 Zn1 Zn1 60.0 148 75 ?
O2 Zn1 Zn1 125.45(12) . 122 ?
O2 Zn1 Zn1 77.31(16) 88 122 ?
O2 Zn1 Zn1 125.45(12) 63 122 ?
O1 Zn1 Zn1 35.3 . 122 ?
Zn1 Zn1 Zn1 60.0 148 122 ?
Zn1 Zn1 Zn1 60.0 75 122 ?
Zn1 O1 Zn1 109.5 . 148 ?
Zn1 O1 Zn1 109.5 . 122 ?
Zn1 O1 Zn1 109.5 148 122 ?
Zn1 O1 Zn1 109.5 . 75 ?
Zn1 O1 Zn1 109.5 148 75 ?
Zn1 O1 Zn1 109.5 122 75 ?
C1 O2 Zn1 128.9(4) . . ?
O2 C1 O2 127.6(7) 30 . ?
O2 C1 C2 116.2(3) 30 . ?
O2 C1 C2 116.2(3) . . ?
C3 C2 C3 119.3(9) . 30 ?
C3 C2 C1 120.3(4) . . ?
C3 C2 C1 120.3(4) 30 . ?
C3 C3 C2 120.3(4) 102_655 . ?
C3 C3 N1 113.1(10) 102_655 . ?
C2 C3 N1 126.6(11) . . ?

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
Zn1 O2 C1 O2 0.000(1) . . . 30 ?
Zn1 O2 C1 C2 180.000(0) . . . . ?
O2 C1 C2 C3 0.000(1) 30 . . . ?
O2 C1 C2 C3 180.000(1) . . . . ?
O2 C1 C2 C3 180.000(0) 30 . . 30 ?
O2 C1 C2 C3 0.000(1) . . . 30 ?
C3 C2 C3 C3 0.000(1) 30 . . 102_655 ?
C1 C2 C3 C3 180.000(1) . . . 102_655 ?
C3 C2 C3 N1 180.000(2) 30 . . . ?
C1 C2 C3 N1 0.000(2) . . . . ?

_refine_diff_density_max         0.414
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.067

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL dlk11 in Fm-3m
REM dlk11 in Fm-3m
REM 31 parameters refined using 0 restraints
REM Highest difference peak 0.373, deepest hole -0.436, 1-sigma level 0.058
CELL 0.6889 25.8577 25.8577 25.8577 90 90 90
ZERR 8 0.0002 0.0002 0.0002 0 0 0
LATT 4
SYMM -Y,+X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X,+Z
SYMM +X,-Z,+Y
SYMM +X,-Y,-Z
SYMM +X,+Z,-Y
SYMM +Z,+Y,-X
SYMM -X,+Y,-Z
SYMM -Z,+Y,+X
SYMM +Z,+X,+Y
SYMM +Y,+Z,+X
SYMM -Y,-Z,+X
SYMM +Z,-X,-Y
SYMM -Y,+Z,-X
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,-Z,-X
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM -X,+Z,+Y
SYMM -X,-Z,-Y
SYMM +Z,-Y,+X
SYMM -Z,-Y,-X
SFAC C H N O S Zn
DISP C 0.003 0.001 10.848
DISP H -0 0 0.623
DISP N 0.006 0.003 18.337
DISP O 0.011 0.006 30.192
DISP S 0.118 0.117 489.407
DISP Zn 0.326 1.388 5404.793
UNIT 624.8 596.8 24 104 15.6 32

L.S. 14 0 22
PLAN  -4
SIZE 0.12 0.1 0.05
TEMP -23
GRID
BOND $H
CONF
MORE -1
ABIN
fmap 2
ACTA
MERG 2
SHEL 20 0.84
REM <olex2.extras>
REM <HklSrc "%.\\dlk11_sq.hkl">
REM </olex2.extras>

WGHT    0.117300   36.046902
FVAR       0.14838
ZN1   6    0.293185    0.206815    0.206815    10.16667    0.06083    0.06083 =
         0.06083   -0.00301    0.00301    0.00301
O1    4    0.250000    0.250000    0.250000    10.04167    0.04792    0.04792 =
         0.04792    0.00000    0.00000    0.00000
O2    4    0.366139    0.218427    0.218427    10.50000    0.05279    0.12816 =
         0.12816   -0.01318   -0.00467   -0.00467
C1    1    0.388123    0.250000    0.250000    10.25000    0.05197    0.11052 =
         0.11052   -0.00411    0.00000    0.00000
C2    1    0.446676    0.250000    0.250000    10.25000    0.05778    0.10920 =
         0.10920   -0.00537    0.00000    0.00000
C3    1    0.473645    0.282600    0.282600    10.50000    0.05714    0.16222 =
         0.16222   -0.03051   -0.00994   -0.00994
N1    3    0.450852    0.320430    0.320430    10.12500    0.05967    0.23274 =
         0.23274   -0.08795   -0.00123   -0.00123
HKLF 4

REM  dlk11 in Fm-3m
REM R1 =  0.0640 for     816 Fo > 4sig(Fo)  and  0.0660 for all     824 data
REM     31 parameters refined using      0 restraints

END

WGHT      0.1173     36.0470

REM Highest difference peak  0.414,  deepest hole -0.494,  1-sigma level  0.067
Q1    1   0.3191  0.1809  0.2812  10.50000  0.05    0.41
Q2    1   0.3474  0.1526  0.1526  10.16667  0.05    0.36
Q3    1   0.4698  0.3527  0.3527  10.50000  0.05    0.34
Q4    1   0.2419  0.1404  0.2103  11.00000  0.05    0.30
;
_shelx_res_checksum              24326

_shelx_fab_file                  
;
    0    0    2   1732.22      0.00
    1    1    3    -64.68      0.00
    1    3    3    119.67      0.00
    3    3    3    -73.34      0.00
    0    2    4    178.85      0.00
    2    2    4     37.13      0.00
    0    4    4    110.27      0.00
    2    4    4     23.52      0.00
    4    4    4      0.78      0.00
    1    1    5     61.12      0.00
    1    3    5      4.34      0.00
    3    3    5    -20.80      0.00
    1    5    5      0.96      0.00
    3    5    5    -18.12      0.00
    5    5    5    104.83      0.00
    0    0    6     25.65      0.00
    0    2    6    -12.77      0.00
    2    2    6     75.55      0.00
    0    4    6    -42.93      0.00
    2    4    6     20.81      0.00
    4    4    6     28.70      0.00
    0    6    6     62.68      0.00
    2    6    6      0.25      0.00
    4    6    6    -11.97      0.00
    6    6    6    -13.98      0.00
    1    1    7     26.39      0.00
    1    3    7    -17.43      0.00
    3    3    7    -27.36      0.00
    1    5    7     35.49      0.00
    3    5    7     12.59      0.00
    5    5    7     -2.15      0.00
    1    7    7     11.43      0.00
    3    7    7     -1.50      0.00
    5    7    7    -36.34      0.00
    7    7    7    -37.66      0.00
    0    0    8    -30.22      0.00
    0    2    8     42.25      0.00
    2    2    8     35.72      0.00
    0    4    8      9.18      0.00
    2    4    8     13.48      0.00
    4    4    8     -6.43      0.00
    0    6    8     21.10      0.00
    2    6    8     22.89      0.00
    4    6    8    -18.67      0.00
    6    6    8    -12.57      0.00
    0    8    8     35.98      0.00
    2    8    8    -28.82      0.00
    4    8    8     -6.98      0.00
    6    8    8     44.20      0.00
    8    8    8     -0.29      0.00
    1    1    9    -27.45      0.00
    1    3    9     29.11      0.00
    3    3    9    -15.20      0.00
    1    5    9     12.03      0.00
    3    5    9     11.15      0.00
    5    5    9    -26.30      0.00
    1    7    9    -26.20      0.00
    3    7    9    -11.65      0.00
    5    7    9      9.43      0.00
    7    7    9      1.00      0.00
    1    9    9     -2.96      0.00
    3    9    9     -1.58      0.00
    5    9    9      6.16      0.00
    7    9    9    -13.23      0.00
    9    9    9      8.97      0.00
    0    0   10     17.13      0.00
    0    2   10      4.20      0.00
    2    2   10      4.55      0.00
    0    4   10     13.28      0.00
    2    4   10      4.42      0.00
    4    4   10    -13.78      0.00
    0    6   10     -0.33      0.00
    2    6   10    -13.66      0.00
    4    6   10     -1.36      0.00
    6    6   10     20.33      0.00
    0    8   10     -2.84      0.00
    2    8   10     -1.34      0.00
    4    8   10      7.95      0.00
    6    8   10     -8.65      0.00
    8    8   10     -8.13      0.00
    0   10   10     15.84      0.00
    2   10   10     -1.95      0.00
    4   10   10    -13.41      0.00
    6   10   10     -1.25      0.00
    8   10   10      9.86      0.00
   10   10   10     10.35      0.00
    1    1   11      0.92      0.00
    1    3   11      5.90      0.00
    3    3   11     39.53      0.00
    1    5   11    -11.37      0.00
    3    5   11    -28.73      0.00
    5    5   11     16.96      0.00
    1    7   11      0.11      0.00
    3    7   11     -4.92      0.00
    5    7   11      2.96      0.00
    7    7   11      2.53      0.00
    1    9   11      8.65      0.00
    3    9   11      3.82      0.00
    5    9   11    -17.23      0.00
    7    9   11      7.75      0.00
    9    9   11      4.55      0.00
    1   11   11     -2.78      0.00
    3   11   11     -8.73      0.00
    5   11   11      8.47      0.00
    7   11   11     -4.10      0.00
    9   11   11    -11.33      0.00
   11   11   11      9.68      0.00
    0    2   12    -44.26      0.00
    2    2   12    -11.61      0.00
    0    4   12      8.12      0.00
    2    4   12     11.21      0.00
    4    4   12     -0.94      0.00
    0    6   12     -3.54      0.00
    2    6   12     -0.90      0.00
    4    6   12      2.14      0.00
    6    6   12    -10.66      0.00
    0    8   12    -11.88      0.00
    2    8   12     10.98      0.00
    4    8   12      5.59      0.00
    6    8   12     -6.84      0.00
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    9    9   23      0.35      0.00
    1   11   23      0.28      0.00
    3   11   23      3.13      0.00
    5   11   23     -0.80      0.00
    7   11   23      1.28      0.00
    9   11   23     -0.50      0.00
   11   11   23     -0.84      0.00
    1   13   23     -6.59      0.00
    3   13   23     -1.61      0.00
    5   13   23     -3.05      0.00
    7   13   23      1.29      0.00
    9   13   23      4.80      0.00
   11   13   23      1.60      0.00
   13   13   23      1.39      0.00
    1   15   23     -5.74      0.00
    3   15   23     -1.40      0.00
    5   15   23      1.74      0.00
    7   15   23      0.08      0.00
    9   15   23     -1.05      0.00
   11   15   23     -5.12      0.00
   13   15   23      2.08      0.00
    1   17   23      3.70      0.00
    3   17   23      1.09      0.00
    5   17   23      0.33      0.00
    7   17   23      0.41      0.00
    9   17   23      1.42      0.00
   11   17   23     -8.49      0.00
    1   19   23     -5.44      0.00
    3   19   23     -6.01      0.00
    5   19   23      4.63      0.00
    7   19   23     -3.25      0.00
    0    0   24      1.88      0.00
    0    2   24      0.15      0.00
    2    2   24      1.58      0.00
    0    4   24      3.45      0.00
    2    4   24     -0.78      0.00
    4    4   24     -1.38      0.00
    0    6   24      1.38      0.00
    2    6   24     -2.67      0.00
    4    6   24      2.40      0.00
    6    6   24      3.91      0.00
    0    8   24     -1.16      0.00
    2    8   24      0.42      0.00
    4    8   24      2.30      0.00
    6    8   24     -0.21      0.00
    8    8   24     -1.83      0.00
    0   10   24      0.77      0.00
    2   10   24     -2.55      0.00
    4   10   24     -2.61      0.00
    6   10   24     -1.21      0.00
    8   10   24      0.19      0.00
   10   10   24      0.30      0.00
    0   12   24      2.39      0.00
    2   12   24     -2.46      0.00
    4   12   24     -0.43      0.00
    6   12   24      1.67      0.00
    8   12   24      0.95      0.00
   10   12   24      0.12      0.00
   12   12   24     -0.15      0.00
    0   14   24      0.61      0.00
    2   14   24      0.05      0.00
    4   14   24      2.51      0.00
    6   14   24      0.85      0.00
    8   14   24     -3.45      0.00
   10   14   24      1.12      0.00
   12   14   24      1.48      0.00
    0   16   24     -3.38      0.00
    2   16   24     -0.02      0.00
    4   16   24     -2.74      0.00
    6   16   24     -3.68      0.00
    8   16   24      1.12      0.00
   10   16   24      2.33      0.00
    0   18   24      2.83      0.00
    2   18   24     -1.78      0.00
    4   18   24      0.08      0.00
    6   18   24      5.04      0.00
    1    1   25     -6.59      0.00
    1    3   25     -0.47      0.00
    3    3   25      6.25      0.00
    1    5   25     -2.37      0.00
    3    5   25      0.06      0.00
    5    5   25     -0.92      0.00
    1    7   25      0.40      0.00
    3    7   25     -1.38      0.00
    5    7   25     -1.79      0.00
    7    7   25      3.09      0.00
    1    9   25     -4.05      0.00
    3    9   25      1.09      0.00
    5    9   25     -0.18      0.00
    7    9   25      4.13      0.00
    9    9   25     -2.21      0.00
    1   11   25     -3.50      0.00
    3   11   25      1.00      0.00
    5   11   25     -4.47      0.00
    7   11   25      2.89      0.00
    9   11   25     -0.96      0.00
   11   11   25     -0.02      0.00
    1   13   25      1.52      0.00
    3   13   25     -0.23      0.00
    5   13   25     -1.40      0.00
    7   13   25      3.16      0.00
    9   13   25      1.76      0.00
   11   13   25     -1.54      0.00
    1   15   25     -0.36      0.00
    3   15   25     -0.86      0.00
    5   15   25      0.83      0.00
    7   15   25     -0.59      0.00
    9   15   25      0.12      0.00
    1   17   25      3.40      0.00
    3   17   25      0.49      0.00
    5   17   25     -2.24      0.00
    0    0   26     -6.77      0.00
    0    2   26     -1.35      0.00
    2    2   26     -6.13      0.00
    0    4   26      5.08      0.00
    2    4   26     -3.28      0.00
    4    4   26     -0.87      0.00
    0    6   26     -1.05      0.00
    2    6   26     -1.53      0.00
    4    6   26      3.44      0.00
    6    6   26      0.31      0.00
    0    8   26     -1.26      0.00
    2    8   26     -2.06      0.00
    4    8   26      1.93      0.00
    6    8   26     -1.37      0.00
    8    8   26     -4.63      0.00
    0   10   26     -0.91      0.00
    2   10   26     -0.77      0.00
    4   10   26     -0.30      0.00
    6   10   26      1.53      0.00
    8   10   26      3.00      0.00
   10   10   26      0.98      0.00
    0   12   26     -0.22      0.00
    2   12   26      2.41      0.00
    4   12   26      1.24      0.00
    6   12   26      2.92      0.00
    8   12   26      2.24      0.00
   10   12   26     -3.84      0.00
    0   14   26     -1.00      0.00
    2   14   26     -0.25      0.00
    4   14   26     -1.99      0.00
    6   14   26     -1.18      0.00
    8   14   26     -2.89      0.00
    0   16   26      0.39      0.00
    2   16   26     -1.10      0.00
    1    1   27     -1.00      0.00
    1    3   27      1.83      0.00
    3    3   27     -0.41      0.00
    1    5   27     -2.22      0.00
    3    5   27     -0.58      0.00
    5    5   27     -0.79      0.00
    1    7   27      1.77      0.00
    3    7   27     -0.74      0.00
    5    7   27     -0.41      0.00
    7    7   27      3.24      0.00
    1    9   27     -0.45      0.00
    3    9   27     -0.04      0.00
    5    9   27     -0.33      0.00
    7    9   27     -0.09      0.00
    9    9   27     -5.49      0.00
    1   11   27     -6.12      0.00
    3   11   27      0.24      0.00
    5   11   27     -1.92      0.00
    7   11   27      1.11      0.00
    9   11   27      1.89      0.00
    1   13   27     -2.54      0.00
    3   13   27      0.01      0.00
    5   13   27      1.04      0.00
    7   13   27      1.20      0.00
    0    0   28     -2.45      0.00
    0    2   28     -0.03      0.00
    2    2   28     -1.34      0.00
    0    4   28     -0.64      0.00
    2    4   28     -2.03      0.00
    4    4   28      8.48      0.00
    0    6   28     -6.14      0.00
    2    6   28     -6.64      0.00
    4    6   28      4.84      0.00
    6    6   28      4.13      0.00
    0    8   28     -1.56      0.00
    2    8   28     -1.06      0.00
    4    8   28     -1.72      0.00
    6    8   28     -1.38      0.00
    8    8   28      3.41      0.00
    0   10   28     -0.47      0.00
    2   10   28      2.98      0.00
    4   10   28      1.35      0.00
    6   10   28      1.80      0.00
    0   12   28     -1.06      0.00
    2   12   28     -0.54      0.00
    4   12   28     -3.22      0.00
    1    1   29     -0.51      0.00
    1    3   29      0.18      0.00
    3    3   29     -0.81      0.00
    1    5   29      1.80      0.00
    3    5   29     -1.72      0.00
    5    5   29      3.90      0.00
    1    7   29     -0.32      0.00
    3    7   29     -0.45      0.00
    5    7   29     -0.24      0.00
    7    7   29     -0.14      0.00
    1    9   29     -1.70      0.00
    3    9   29      0.03      0.00
    5    9   29     -1.38      0.00
    0    0   30     -3.16      0.00
    0    2   30      0.73      0.00
    2    2   30      2.45      0.00
    0    4   30      0.83      0.00
    2    4   30     -1.17      0.00
    4    4   30      3.04      0.00
    0    6   30      0.35      0.00
    2    6   30     -3.96      0.00
    1    1    1   -115.14      0.00
    0    2    2    726.97      0.00
    2    2    2    110.04      0.00
    0    0    4    267.92      0.00
    0    0   12    -33.71      0.00
   18   18   18      3.66      0.00
   17   19   19     18.33      0.00
   19   19   19      4.61      0.00
   16   18   20      6.43      0.00
   18   18   20      0.26      0.00
   14   20   20      2.90      0.00
   16   20   20      1.39      0.00
   18   20   20     -3.76      0.00
   15   17   21      1.17      0.00
   17   17   21      3.98      0.00
   13   19   21      3.49      0.00
   15   19   21      6.56      0.00
   17   19   21     -2.18      0.00
    9   21   21     -3.70      0.00
   11   21   21      8.70      0.00
   13   21   21      1.48      0.00
   15   21   21     -6.52      0.00
   16   16   22      3.80      0.00
   12   18   22      3.05      0.00
   14   18   22      2.49      0.00
   16   18   22     -3.79      0.00
   18   18   22     -6.06      0.00
    8   20   22     -9.31      0.00
   10   20   22     -4.39      0.00
   12   20   22      8.49      0.00
   14   20   22      0.62      0.00
   16   20   22     -4.70      0.00
    0   22   22      5.77      0.00
    2   22   22      0.71      0.00
    4   22   22      6.53      0.00
    6   22   22      5.53      0.00
    8   22   22      1.82      0.00
   10   22   22     -1.28      0.00
   12   22   22      0.48      0.00
   15   15   23     13.05      0.00
   13   17   23      3.41      0.00
   15   17   23      6.53      0.00
   17   17   23     -4.17      0.00
    9   19   23     -7.34      0.00
   11   19   23      1.52      0.00
   13   19   23      1.41      0.00
   15   19   23     -4.63      0.00
    1   21   23     -9.73      0.00
    3   21   23     -1.06      0.00
    5   21   23     -1.44      0.00
    7   21   23     -3.48      0.00
    9   21   23     -0.98      0.00
   11   21   23      3.66      0.00
   13   21   23     -7.21      0.00
    1   23   23     -7.70      0.00
    3   23   23     -0.05      0.00
    5   23   23     -8.79      0.00
    7   23   23      3.92      0.00
    9   23   23      4.84      0.00
   14   14   24      1.47      0.00
   12   16   24      3.92      0.00
   14   16   24      4.86      0.00
   16   16   24     -2.18      0.00
    8   18   24      0.42      0.00
   10   18   24      3.35      0.00
   12   18   24      6.19      0.00
   14   18   24     -2.35      0.00
    0   20   24      3.39      0.00
    2   20   24     -0.59      0.00
    4   20   24      6.61      0.00
    6   20   24      4.82      0.00
    8   20   24     -1.04      0.00
   10   20   24      2.79      0.00
   12   20   24      1.70      0.00
    0   22   24      1.36      0.00
    2   22   24      1.89      0.00
    4   22   24      3.84      0.00
    6   22   24     -1.06      0.00
    8   22   24      4.55      0.00
   13   13   25     -0.06      0.00
   11   15   25     -7.25      0.00
   13   15   25      7.72      0.00
   15   15   25      9.85      0.00
    7   17   25    -10.25      0.00
    9   17   25     -3.52      0.00
   11   17   25     -2.04      0.00
   13   17   25      3.07      0.00
   15   17   25     -4.56      0.00
    1   19   25     -8.81      0.00
    3   19   25     -2.12      0.00
    5   19   25     -2.70      0.00
    7   19   25     -7.03      0.00
    9   19   25      0.23      0.00
   11   19   25      2.29      0.00
    1   21   25     -3.13      0.00
    3   21   25     -0.16      0.00
    5   21   25     -4.46      0.00
    7   21   25      1.05      0.00
   12   12   26     -6.18      0.00
   10   14   26     -2.35      0.00
   12   14   26     -1.01      0.00
   14   14   26     -0.27      0.00
    4   16   26     -4.06      0.00
    6   16   26     -1.27      0.00
    8   16   26      0.42      0.00
   10   16   26      5.24      0.00
   12   16   26      4.73      0.00
   14   16   26     -1.91      0.00
    0   18   26      3.59      0.00
    2   18   26      5.58      0.00
    4   18   26      2.08      0.00
    6   18   26      1.95      0.00
    8   18   26      4.65      0.00
   10   18   26      4.20      0.00
    0   20   26      2.29      0.00
    2   20   26      4.18      0.00
    4   20   26      1.87      0.00
    6   20   26      0.47      0.00
    8   20   26      4.13      0.00
   11   11   27      9.81      0.00
    9   13   27     -1.41      0.00
   11   13   27      2.07      0.00
   13   13   27      5.08      0.00
    1   15   27     -4.83      0.00
    3   15   27      0.94      0.00
    5   15   27      7.10      0.00
    7   15   27     -1.80      0.00
    9   15   27     -1.58      0.00
   11   15   27     -0.31      0.00
   13   15   27      2.68      0.00
    1   17   27     -3.02      0.00
    3   17   27      5.16      0.00
    5   17   27      0.54      0.00
    7   17   27     -9.48      0.00
    9   17   27     -1.07      0.00
   11   17   27     -1.04      0.00
    1   19   27     -5.26      0.00
    3   19   27      1.39      0.00
    5   19   27     -3.06      0.00
    7   19   27     -1.38      0.00
    8   10   28      2.56      0.00
   10   10   28      0.61      0.00
    6   12   28     -1.23      0.00
    8   12   28     -2.29      0.00
   10   12   28     -1.72      0.00
   12   12   28     -0.49      0.00
    0   14   28      0.49      0.00
    2   14   28     -2.35      0.00
    4   14   28     -6.25      0.00
    6   14   28     -1.77      0.00
    8   14   28     -0.20      0.00
   10   14   28      0.85      0.00
   12   14   28     -0.07      0.00
    0   16   28      3.42      0.00
    2   16   28      2.69      0.00
    4   16   28     -1.34      0.00
    6   16   28      1.54      0.00
    8   16   28      3.80      0.00
   10   16   28      4.02      0.00
    0   18   28      1.95      0.00
    2   18   28      4.10      0.00
    4   18   28     -0.32      0.00
    7    9   29      2.51      0.00
    9    9   29      0.22      0.00
    1   11   29     -1.23      0.00
    3   11   29      0.08      0.00
    5   11   29      4.95      0.00
    7   11   29      3.28      0.00
    9   11   29      0.25      0.00
   11   11   29      9.40      0.00
    1   13   29     -0.24      0.00
    3   13   29      4.23      0.00
    5   13   29      2.32      0.00
    7   13   29     -5.41      0.00
    9   13   29     -2.77      0.00
   11   13   29      4.29      0.00
    1   15   29     -2.88      0.00
    3   15   29      4.83      0.00
    5   15   29      1.06      0.00
    7   15   29     -3.86      0.00
    1   17   29     -2.99      0.00
    3   17   29      0.08      0.00
    4    6   30      0.21      0.00
    6    6   30     -1.96      0.00
    0    8   30      5.88      0.00
    2    8   30      4.85      0.00
    4    8   30     -0.60      0.00
    6    8   30     -1.90      0.00
    8    8   30      4.69      0.00
    0   10   30      2.63      0.00
    2   10   30      2.78      0.00
    4   10   30      0.15      0.00
    6   10   30      3.09      0.00
    8   10   30      2.35      0.00
   10   10   30     -3.18      0.00
    0   12   30     -0.98      0.00
    2   12   30     -3.39      0.00
    4   12   30     -4.82      0.00
    6   12   30     -1.08      0.00
    8   12   30     -0.69      0.00
    0   14   30     -0.74      0.00
    2   14   30     -2.04      0.00
    4   14   30     -3.47      0.00
    6   14   30     -0.67      0.00
    0    0    0      0.00      0.00
;
# SQUEEZE RESULTS (Version = 110516)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.033 -0.013 -0.010 12094 3808 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 1 1.322
0 2 2 2.159
2 2 2 2.645
0 0 4 3.054
0 0 12 9.198
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL dlk11 in Fm-3m
CELL   25.8577   25.8577   25.8577     90.00     90.00     90.00
SPGR Fm-3m
# Solvent Accessible Volume =     12278
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 1.000 0.500 0.000 !       2.57 eA-3
C102 0.500 0.500 0.000 !       2.23 eA-3
C103 0.980 0.023-0.004 !       2.15 eA-3
C104 0.485 0.015 0.015 !       2.09 eA-3
C105 0.035 0.500 0.000 !       1.95 eA-3
C106 0.459 0.039 0.002 !       1.65 eA-3
Q107 0.817 0.314 0.314 !       1.16 eA-3
C108 0.117 0.500 0.000 !       1.14 eA-3
C109 0.032 0.101 0.486 !       1.07 eA-3
Q110 0.639 0.361 0.361 !       0.88 eA-3
C111 0.569 0.073 0.421 !       0.76 eA-3
Q112 1.000 0.119 0.389 !       0.75 eA-3
Q113 0.369 0.478 0.368 !       0.67 eA-3
C114 0.855 0.355 0.355 !       0.57 eA-3
C115 0.897 0.102 0.001 !       0.55 eA-3
C116 0.976 0.164 0.020 !       0.54 eA-3
C117 0.331 0.167 0.335 !       0.51 eA-3
C118 0.382 0.118 0.118 !       0.51 eA-3
C119 0.319 0.046 0.454 !       0.51 eA-3
C120 0.918 0.501 0.211 !       0.50 eA-3

;
_shelx_fab_checksum              99754
_diffrn_radiation_source         Synchrotron'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_measurement_device       
;
CrystalLogic Kappa (3 circle)
;

#===end
