# 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_Compound1
_database_code_depnum_ccdc_archive 'CCDC 1431698'
_audit_update_record             
;
2015-12-11 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{[tris(mu4-biphenyl-4,4'-dicarboxylato-kO:kO':kO'':kO''')diaquatricadmium(II)]dimethylformamide}
_chemical_formula_moiety         'C42 H28 Cd3 O14, (C3 H7 N O)'
_chemical_formula_structural     'C42 H28 Cd3 O14, (C3 H7 N O)'
_chemical_formula_sum            'C45 H35 Cd3 N O15'
_chemical_formula_weight         1166.99
_chemical_compound_source        'synthesis as described'


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_Int_Tables_number      148

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

_cell_length_a                   14.070(6)
_cell_length_b                   14.070(6)
_cell_length_c                   19.864(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3406(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15524
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      28.81

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.486 248.2 40.1
2 0.333 0.667 0.152 248.6 40.0
3 0.667 0.333 0.819 249.8 40.3
_platon_squeeze_details          
;
;

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1728
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_T_max  0.944


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3834
_diffrn_reflns_av_unetI/netI     0.1192
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.646
_diffrn_reflns_theta_max         28.808
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1963
_reflns_number_gt                1057
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0749P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1963
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1548
_refine_ls_wR_factor_gt          0.1396
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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
Cd1 Cd 0.6667 0.3333 -0.83449(4) 0.0303(3) Uani 1 3 d S T P . .
Cd2 Cd 0.6667 0.3333 -0.6667 0.0278(3) Uani 1 6 d S T P . .
O1A O 0.4959(3) 0.1854(3) -0.8285(2) 0.0337(10) Uani 1 1 d . . . . .
O2A O 0.5919(3) 0.1905(3) -0.7395(2) 0.0335(10) Uani 1 1 d . . . . .
C1A C 0.5035(5) 0.1497(5) -0.7708(3) 0.0313(15) Uani 1 1 d . . . . .
C2A C 0.4032(5) 0.0555(5) -0.7411(3) 0.0341(15) Uani 1 1 d . . . . .
C3A C 0.4078(6) 0.0178(7) -0.6795(5) 0.069(3) Uani 1 1 d . . . . .
H3A H 0.4742 0.0506 -0.6563 0.083 Uiso 1 1 calc R U . . .
C4A C 0.3158(6) -0.0688(7) -0.6498(5) 0.072(3) Uani 1 1 d . . . . .
H4A H 0.3217 -0.0920 -0.6069 0.086 Uiso 1 1 calc R U . . .
C5A C 0.2160(6) -0.1211(6) -0.6825(4) 0.046(2) Uani 1 1 d . . . . .
C6A C 0.2137(6) -0.0799(8) -0.7446(4) 0.074(3) Uani 1 1 d . . . . .
H6A H 0.1478 -0.1128 -0.7683 0.089 Uiso 1 1 calc R U . . .
C7A C 0.3036(6) 0.0075(6) -0.7740(4) 0.050(2) Uani 1 1 d . . . . .
H7A H 0.2972 0.0340 -0.8157 0.060 Uiso 1 1 calc R U . . .
O1W O 0.6667 0.3333 -0.9467(4) 0.056(3) Uani 1 3 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1W 2.229(9) . ?
Cd1 O1A 2.263(4) 2_655 ?
Cd1 O1A 2.263(4) . ?
Cd1 O1A 2.263(4) 3_665 ?
Cd1 O2A 2.568(5) . ?
Cd1 O2A 2.568(5) 2_655 ?
Cd1 O2A 2.568(5) 3_665 ?
Cd1 C1A 2.760(7) 2_655 ?
Cd1 C1A 2.760(7) 3_665 ?
Cd1 C1A 2.760(7) . ?
Cd1 Cd2 3.3337(16) . ?
Cd2 O2A 2.264(4) 16_653 ?
Cd2 O2A 2.264(4) 17_553 ?
Cd2 O2A 2.264(4) 2_655 ?
Cd2 O2A 2.264(4) . ?
Cd2 O2A 2.264(4) 3_665 ?
Cd2 O2A 2.264(4) 18_543 ?
Cd2 Cd1 3.3337(16) 16_653 ?
O1A C1A 1.277(8) . ?
O2A C1A 1.246(8) . ?
C1A C2A 1.492(9) . ?
C2A C3A 1.348(10) . ?
C2A C7A 1.379(9) . ?
C3A C4A 1.390(11) . ?
C4A C5A 1.380(9) . ?
C5A C6A 1.370(10) . ?
C5A C5A 1.478(14) 16_543 ?
C6A C7A 1.378(10) . ?

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
O1W Cd1 O1A 93.01(12) . 2_655 ?
O1W Cd1 O1A 93.01(12) . . ?
O1A Cd1 O1A 119.73(2) 2_655 . ?
O1W Cd1 O1A 93.01(12) . 3_665 ?
O1A Cd1 O1A 119.73(2) 2_655 3_665 ?
O1A Cd1 O1A 119.73(2) . 3_665 ?
O1W Cd1 O2A 137.31(10) . . ?
O1A Cd1 O2A 84.03(15) 2_655 . ?
O1A Cd1 O2A 53.88(15) . . ?
O1A Cd1 O2A 125.30(16) 3_665 . ?
O1W Cd1 O2A 137.31(10) . 2_655 ?
O1A Cd1 O2A 53.88(15) 2_655 2_655 ?
O1A Cd1 O2A 125.30(16) . 2_655 ?
O1A Cd1 O2A 84.03(15) 3_665 2_655 ?
O2A Cd1 O2A 71.92(15) . 2_655 ?
O1W Cd1 O2A 137.31(10) . 3_665 ?
O1A Cd1 O2A 125.30(16) 2_655 3_665 ?
O1A Cd1 O2A 84.03(15) . 3_665 ?
O1A Cd1 O2A 53.88(15) 3_665 3_665 ?
O2A Cd1 O2A 71.92(15) . 3_665 ?
O2A Cd1 O2A 71.92(15) 2_655 3_665 ?
O1W Cd1 C1A 117.27(14) . 2_655 ?
O1A Cd1 C1A 27.23(17) 2_655 2_655 ?
O1A Cd1 C1A 125.47(17) . 2_655 ?
O1A Cd1 C1A 103.70(17) 3_665 2_655 ?
O2A Cd1 C1A 74.96(16) . 2_655 ?
O2A Cd1 C1A 26.74(16) 2_655 2_655 ?
O2A Cd1 C1A 98.18(18) 3_665 2_655 ?
O1W Cd1 C1A 117.27(14) . 3_665 ?
O1A Cd1 C1A 125.47(18) 2_655 3_665 ?
O1A Cd1 C1A 103.70(17) . 3_665 ?
O1A Cd1 C1A 27.23(17) 3_665 3_665 ?
O2A Cd1 C1A 98.18(18) . 3_665 ?
O2A Cd1 C1A 74.96(16) 2_655 3_665 ?
O2A Cd1 C1A 26.74(16) 3_665 3_665 ?
C1A Cd1 C1A 100.66(17) 2_655 3_665 ?
O1W Cd1 C1A 117.27(14) . . ?
O1A Cd1 C1A 103.70(17) 2_655 . ?
O1A Cd1 C1A 27.23(17) . . ?
O1A Cd1 C1A 125.47(17) 3_665 . ?
O2A Cd1 C1A 26.74(16) . . ?
O2A Cd1 C1A 98.17(18) 2_655 . ?
O2A Cd1 C1A 74.96(16) 3_665 . ?
C1A Cd1 C1A 100.66(17) 2_655 . ?
C1A Cd1 C1A 100.66(17) 3_665 . ?
O1W Cd1 Cd2 180.0 . . ?
O1A Cd1 Cd2 86.99(12) 2_655 . ?
O1A Cd1 Cd2 86.99(12) . . ?
O1A Cd1 Cd2 86.99(12) 3_665 . ?
O2A Cd1 Cd2 42.69(10) . . ?
O2A Cd1 Cd2 42.69(10) 2_655 . ?
O2A Cd1 Cd2 42.69(10) 3_665 . ?
C1A Cd1 Cd2 62.73(14) 2_655 . ?
C1A Cd1 Cd2 62.73(14) 3_665 . ?
C1A Cd1 Cd2 62.73(14) . . ?
O2A Cd2 O2A 83.56(17) 16_653 17_553 ?
O2A Cd2 O2A 96.44(17) 16_653 2_655 ?
O2A Cd2 O2A 180.0 17_553 2_655 ?
O2A Cd2 O2A 180.0 16_653 . ?
O2A Cd2 O2A 96.44(17) 17_553 . ?
O2A Cd2 O2A 83.56(17) 2_655 . ?
O2A Cd2 O2A 96.44(17) 16_653 3_665 ?
O2A Cd2 O2A 96.44(17) 17_553 3_665 ?
O2A Cd2 O2A 83.56(17) 2_655 3_665 ?
O2A Cd2 O2A 83.56(17) . 3_665 ?
O2A Cd2 O2A 83.56(17) 16_653 18_543 ?
O2A Cd2 O2A 83.56(17) 17_553 18_543 ?
O2A Cd2 O2A 96.44(17) 2_655 18_543 ?
O2A Cd2 O2A 96.44(17) . 18_543 ?
O2A Cd2 O2A 180.0 3_665 18_543 ?
O2A Cd2 Cd1 50.30(12) 16_653 16_653 ?
O2A Cd2 Cd1 50.30(12) 17_553 16_653 ?
O2A Cd2 Cd1 129.70(12) 2_655 16_653 ?
O2A Cd2 Cd1 129.70(12) . 16_653 ?
O2A Cd2 Cd1 129.71(12) 3_665 16_653 ?
O2A Cd2 Cd1 50.30(12) 18_543 16_653 ?
O2A Cd2 Cd1 129.70(12) 16_653 . ?
O2A Cd2 Cd1 129.70(12) 17_553 . ?
O2A Cd2 Cd1 50.30(12) 2_655 . ?
O2A Cd2 Cd1 50.30(12) . . ?
O2A Cd2 Cd1 50.30(12) 3_665 . ?
O2A Cd2 Cd1 129.70(12) 18_543 . ?
Cd1 Cd2 Cd1 180.0 16_653 . ?
C1A O1A Cd1 98.6(4) . . ?
C1A O2A Cd2 129.9(4) . . ?
C1A O2A Cd1 85.2(4) . . ?
Cd2 O2A Cd1 87.01(14) . . ?
O2A C1A O1A 121.9(6) . . ?
O2A C1A C2A 119.6(6) . . ?
O1A C1A C2A 118.5(6) . . ?
O2A C1A Cd1 68.0(4) . . ?
O1A C1A Cd1 54.2(3) . . ?
C2A C1A Cd1 171.1(5) . . ?
C3A C2A C7A 118.4(7) . . ?
C3A C2A C1A 119.9(6) . . ?
C7A C2A C1A 121.6(6) . . ?
C2A C3A C4A 121.6(7) . . ?
C5A C4A C3A 121.4(7) . . ?
C6A C5A C4A 115.6(7) . . ?
C6A C5A C5A 122.7(8) . 16_543 ?
C4A C5A C5A 121.7(8) . 16_543 ?
C5A C6A C7A 123.7(7) . . ?
C6A C7A C2A 119.3(7) . . ?

_refine_diff_density_max         1.582
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.163

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_CHEMW03_Compound1           
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: Crystal structure contains voids in which solvent molecules could not
be located given that they are highly disordered. Therefore, there is a discrepancy 
between the crystallographic formula and the chemical formula determined by 
thermogravimetric and elemental analyses.
;
# end Validation Reply Form
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound2
_database_code_depnum_ccdc_archive 'CCDC 1431699'
_audit_update_record             
;
2015-12-11 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{[bis(mu4-biphenyl-4,4'-dicarboxylato-kO:kO':kO'':kO''')(mu4-biphenyl-4,4'-dicarboxylato-kO:kO,O':kO'':kO'',O''')(mu-1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene)trizinc(II)]pentakisdimethylformamide}
_chemical_formula_moiety         'C54 H34 N4 O12 Zn3, 5(C3 H7 N O)'
_chemical_formula_structural     'C54 H34 N4 O12 Zn3, 5(C3 H7 N O)'
_chemical_formula_sum            'C69 H69 N9 O17 Zn3'
_chemical_formula_weight         1492.51
_chemical_compound_source        'synthesis as described'


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   47.928(4)
_cell_length_b                   13.828(1)
_cell_length_c                   26.187(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.491(2)
_cell_angle_gamma                90.00
_cell_volume                     15794(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    56159
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      26.55

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.004 -0.001 -0.006 7667.5 134.1
_platon_squeeze_details          
;
;

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    none
_exptl_crystal_F_000             6176
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_T_max  0.964


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            56159
_diffrn_reflns_av_unetI/netI     0.0942
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.251
_diffrn_reflns_theta_max         26.553
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             16223
_reflns_number_gt                9446
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0678P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16223
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1443
_refine_ls_wR_factor_gt          0.1338
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_restrained_S_all      0.927
_refine_ls_shift/su_max          0.003
_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 0.64456(2) 0.24638(3) 0.54705(2) 0.01761(10) Uani 1 1 d . . . . .
Zn2 Zn 0.72092(2) 0.23642(3) 0.60915(2) 0.01886(10) Uani 1 1 d . . . . .
Zn3 Zn 0.56605(2) -0.73682(3) 0.48314(2) 0.02180(11) Uani 1 1 d . . . . .
O1A O 0.66663(5) 0.34479(18) 0.51860(10) 0.0313(6) Uani 1 1 d . . . . .
O2A O 0.71670(5) 0.31775(19) 0.54563(9) 0.0327(6) Uani 1 1 d . . . . .
C1A C 0.69110(8) 0.3541(2) 0.51315(13) 0.0249(8) Uani 1 1 d . . . . .
C2A C 0.69057(8) 0.4111(3) 0.46474(13) 0.0265(8) Uani 1 1 d . . . . .
C3A C 0.66320(9) 0.4428(3) 0.42319(14) 0.0369(9) Uani 1 1 d . . . . .
H3A H 0.6450 0.4324 0.4269 0.044 Uiso 1 1 calc R U . . .
C4A C 0.66267(9) 0.4897(3) 0.37637(16) 0.0400(10) Uani 1 1 d . . . . .
H4A H 0.6440 0.5110 0.3493 0.048 Uiso 1 1 calc R U . . .
C5A C 0.68913(8) 0.5060(3) 0.36848(14) 0.0302(8) Uani 1 1 d . . . . .
C6A C 0.71695(8) 0.4750(3) 0.41186(14) 0.0347(9) Uani 1 1 d . . . . .
H6A H 0.7353 0.4865 0.4087 0.042 Uiso 1 1 calc R U . . .
C7A C 0.71751(8) 0.4286(3) 0.45824(13) 0.0306(9) Uani 1 1 d . . . . .
H7A H 0.7362 0.4084 0.4859 0.037 Uiso 1 1 calc R U . . .
C8A C 0.68884(8) 0.5509(3) 0.31694(13) 0.0308(9) Uani 1 1 d . . . . .
C9A C 0.66212(12) 0.5649(4) 0.2704(2) 0.0714(15) Uani 1 1 d . . . . .
H9A H 0.6438 0.5418 0.2702 0.086 Uiso 1 1 calc R U . . .
C10A C 0.66169(11) 0.6133(5) 0.2231(2) 0.104(3) Uani 1 1 d . . . . .
H10A H 0.6430 0.6303 0.1944 0.125 Uiso 1 1 calc R U . . .
C11A C 0.68778(8) 0.6354(3) 0.21843(13) 0.0264(8) Uani 1 1 d . . . . .
C12A C 0.71426(10) 0.6125(5) 0.2625(2) 0.088(2) Uani 1 1 d . . . . .
H12A H 0.7328 0.6259 0.2605 0.105 Uiso 1 1 calc R U . . .
C13A C 0.71462(10) 0.5704(5) 0.3098(2) 0.082(2) Uani 1 1 d . . . . .
H13A H 0.7334 0.5543 0.3385 0.099 Uiso 1 1 calc R U . . .
C14A C 0.68776(8) 0.3188(2) 0.66696(13) 0.0256(8) Uani 1 1 d . . . . .
O3A O 0.66234(5) 0.2955(2) 0.62895(9) 0.0369(6) Uani 1 1 d . . . . .
O4A O 0.71347(5) 0.3074(2) 0.66551(10) 0.0381(7) Uani 1 1 d . . . . .
O1B O 0.68319(5) 0.14635(16) 0.56571(9) 0.0260(5) Uani 1 1 d . . . . .
O2B O 0.71912(6) 0.08524(19) 0.64124(13) 0.0527(8) Uani 1 1 d . . . . .
C1B C 0.69389(8) 0.0750(3) 0.59949(14) 0.0271(8) Uani 1 1 d . . . . .
C2B C 0.67768(8) -0.0182(2) 0.58906(14) 0.0261(8) Uani 1 1 d . . . . .
C3B C 0.65183(8) -0.0340(3) 0.53990(15) 0.0353(9) Uani 1 1 d . . . . .
H3B H 0.6439 0.0157 0.5140 0.042 Uiso 1 1 calc R U . . .
C4B C 0.63787(9) -0.1238(3) 0.52944(16) 0.0401(10) Uani 1 1 d . . . . .
H4B H 0.6212 -0.1342 0.4954 0.048 Uiso 1 1 calc R U . . .
C5B C 0.64801(8) -0.1993(3) 0.56826(16) 0.0373(9) Uani 1 1 d . . . . .
C6B C 0.67404(9) -0.1817(3) 0.61817(16) 0.0458(11) Uani 1 1 d . . . . .
H6B H 0.6817 -0.2304 0.6449 0.055 Uiso 1 1 calc R U . . .
C7B C 0.68844(9) -0.0927(3) 0.62807(16) 0.0431(11) Uani 1 1 d . . . . .
H7B H 0.7056 -0.0825 0.6614 0.052 Uiso 1 1 calc R U . . .
C8B C 0.63391(9) -0.2965(3) 0.55638(15) 0.0359(9) Uani 1 1 d . . . . .
C9B C 0.60275(9) -0.3069(3) 0.52080(18) 0.0492(12) Uani 1 1 d . . . . .
H9B H 0.5907 -0.2522 0.5063 0.059 Uiso 1 1 calc R U . . .
C10B C 0.58981(9) -0.3974(3) 0.50719(18) 0.0453(11) Uani 1 1 d . . . . .
H10B H 0.5692 -0.4031 0.4829 0.054 Uiso 1 1 calc R U . . .
C11B C 0.60692(8) -0.4801(3) 0.52895(15) 0.0313(8) Uani 1 1 d . . . . .
C12B C 0.63730(9) -0.4701(3) 0.56556(16) 0.0387(10) Uani 1 1 d . . . . .
H12B H 0.6489 -0.5247 0.5817 0.046 Uiso 1 1 calc R U . . .
C13B C 0.65063(9) -0.3793(3) 0.57845(16) 0.0398(10) Uani 1 1 d . . . . .
H13B H 0.6713 -0.3740 0.6025 0.048 Uiso 1 1 calc R U . . .
C14B C 0.59298(8) -0.5775(3) 0.51305(15) 0.0301(8) Uani 1 1 d . . . . .
O3B O 0.56443(6) -0.58485(19) 0.48266(12) 0.0484(8) Uani 1 1 d . . . . .
O4B O 0.60856(5) -0.65267(16) 0.53005(10) 0.0295(6) Uani 1 1 d . . . . .
O1C O 0.57105(6) -0.8183(2) 0.54607(10) 0.0426(7) Uani 1 1 d . . . . .
O2C O 0.62092(6) -0.85229(18) 0.57188(10) 0.0333(6) Uani 1 1 d . . . . .
C1C C 0.59645(8) -0.8577(3) 0.57782(13) 0.0304(9) Uani 1 1 d . . . . .
C2C C 0.59685(8) -0.9152(3) 0.62667(14) 0.0342(9) Uani 1 1 d . . . . .
C3C C 0.57082(9) -0.9233(4) 0.63671(17) 0.0582(14) Uani 1 1 d . . . . .
H3C H 0.5525 -0.8963 0.6113 0.070 Uiso 1 1 calc R U . . .
C4C C 0.57130(9) -0.9703(4) 0.68352(17) 0.0589(14) Uani 1 1 d . . . . .
H4C H 0.5534 -0.9748 0.6892 0.071 Uiso 1 1 calc R U . . .
C5C C 0.59827(9) -1.0111(3) 0.72235(15) 0.0423(11) Uani 1 1 d . . . . .
C6C C 0.62430(9) -1.0067(3) 0.71077(16) 0.0497(12) Uani 1 1 d . . . . .
H6C H 0.6423 -1.0368 0.7347 0.060 Uiso 1 1 calc R U . . .
C7C C 0.62336(9) -0.9579(3) 0.66399(16) 0.0484(12) Uani 1 1 d . . . . .
H7C H 0.6410 -0.9538 0.6577 0.058 Uiso 1 1 calc R U . . .
C8C C 0.59945(8) -1.0572(3) 0.77432(14) 0.0358(9) Uani 1 1 d . . . . .
C9C C 0.57407(9) -1.1049(3) 0.77439(15) 0.0410(10) Uani 1 1 d . . . . .
H9C H 0.5563 -1.1087 0.7414 0.049 Uiso 1 1 calc R U . . .
C10C C 0.57469(8) -1.1470(3) 0.82290(13) 0.0365(10) Uani 1 1 d . . . . .
H10C H 0.5575 -1.1796 0.8221 0.044 Uiso 1 1 calc R U . . .
C11C C 0.60110(8) -1.1404(3) 0.87299(13) 0.0286(8) Uani 1 1 d . . . . .
C12C C 0.62625(8) -1.0928(3) 0.87289(14) 0.0330(9) Uani 1 1 d . . . . .
H12C H 0.6440 -1.0889 0.9059 0.040 Uiso 1 1 calc R U . . .
C13C C 0.62550(8) -1.0508(3) 0.82441(14) 0.0382(10) Uani 1 1 d . . . . .
H13C H 0.6426 -1.0178 0.8254 0.046 Uiso 1 1 calc R U . . .
C14C C 0.60165(8) -1.1848(3) 0.92589(13) 0.0297(8) Uani 1 1 d . . . . .
O3C O 0.57602(6) -1.2148(2) 0.92307(9) 0.0343(6) Uani 1 1 d . . . . .
O4C O 0.62679(5) -1.18845(19) 0.96728(9) 0.0317(6) Uani 1 1 d . . . . .
N1D N 0.76762(6) 0.2309(2) 0.64543(11) 0.0254(6) Uani 1 1 d . . . . .
C2D C 0.78122(8) 0.1990(3) 0.69872(14) 0.0316(9) Uani 1 1 d . . . . .
H2D H 0.7691 0.1781 0.7166 0.038 Uiso 1 1 calc R U . . .
C3D C 0.81238(8) 0.1967(3) 0.72712(15) 0.0375(9) Uani 1 1 d . . . . .
H3D H 0.8214 0.1754 0.7641 0.045 Uiso 1 1 calc R U . . .
C4D C 0.83046(8) 0.2262(3) 0.70041(16) 0.0348(9) Uani 1 1 d . . . . .
C5D C 0.81627(8) 0.2570(3) 0.64586(16) 0.0357(9) Uani 1 1 d . . . . .
H5D H 0.8280 0.2763 0.6268 0.043 Uiso 1 1 calc R U . . .
C6D C 0.78481(8) 0.2596(3) 0.61927(15) 0.0301(8) Uani 1 1 d . . . . .
H6D H 0.7754 0.2816 0.5825 0.036 Uiso 1 1 calc R U . . .
C7D C 0.86437(8) 0.2263(3) 0.72981(17) 0.0440(10) Uani 1 1 d . . . . .
H7D H 0.8763 0.2352 0.7097 0.053 Uiso 1 1 calc R U . . .
N8D N 0.87701(7) 0.2143(3) 0.78247(16) 0.0596(11) Uani 1 1 d . . . . .
N9D N 0.90939(8) 0.2162(3) 0.80306(15) 0.0619(12) Uani 1 1 d . . . . .
C10D C 0.92167(9) 0.2363(4) 0.85401(19) 0.0574(14) Uani 1 1 d . . . . .
H10D H 0.9096 0.2475 0.8736 0.069 Uiso 1 1 calc R U . . .
C11D C 0.95558(9) 0.2424(4) 0.88342(17) 0.0518(12) Uani 1 1 d . . . . .
C13D C 1.00118(9) 0.2555(3) 0.96809(17) 0.0489(12) Uani 1 1 d . . . . .
H13D H 1.0102 0.2627 1.0069 0.059 Uiso 1 1 calc R U . . .
C12D C 0.96948(9) 0.2545(4) 0.94035(18) 0.0603(15) Uani 1 1 d . . . . .
H12D H 0.9576 0.2620 0.9605 0.072 Uiso 1 1 calc R U . . .
N14D N 1.01870(6) 0.2468(2) 0.94138(11) 0.0307(7) Uani 1 1 d . . . . .
C15D C 1.00565(9) 0.2337(3) 0.88597(16) 0.0433(11) Uani 1 1 d . . . . .
H15D H 1.0181 0.2261 0.8669 0.052 Uiso 1 1 calc R U . . .
C16D C 0.97454(9) 0.2309(4) 0.85632(17) 0.0519(12) Uani 1 1 d . . . . .
H16D H 0.9662 0.2213 0.8177 0.062 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1A 2.044(2) . ?
Zn1 O2C 2.044(2) 1_565 ?
Zn1 O4C 2.063(2) 6_545 ?
Zn1 O3A 2.067(2) . ?
Zn1 O4B 2.118(2) 1_565 ?
Zn1 O1B 2.198(2) . ?
Zn2 O4A 1.926(2) . ?
Zn2 O2A 1.948(2) . ?
Zn2 N1D 2.039(3) . ?
Zn2 O1B 2.100(2) . ?
Zn2 O2B 2.268(3) . ?
Zn2 C1B 2.541(4) . ?
Zn3 O1C 1.928(2) . ?
Zn3 O3C 1.943(2) 6_535 ?
Zn3 N14D 2.076(3) 8_445 ?
Zn3 O3B 2.103(3) . ?
Zn3 O4B 2.223(2) . ?
Zn3 C14B 2.508(4) . ?
O1A C1A 1.245(4) . ?
O2A C1A 1.271(4) . ?
C1A C2A 1.484(5) . ?
C2A C3A 1.383(5) . ?
C2A C7A 1.392(5) . ?
C3A C4A 1.378(5) . ?
C4A C5A 1.385(5) . ?
C5A C6A 1.413(5) . ?
C5A C8A 1.481(4) . ?
C6A C7A 1.364(5) . ?
C8A C13A 1.350(5) . ?
C8A C9A 1.367(6) . ?
C9A C10A 1.401(6) . ?
C10A C11A 1.341(5) . ?
C11A C12A 1.353(5) . ?
C11A C14A 1.489(4) 6_565 ?
C12A C13A 1.363(5) . ?
C14A O3A 1.255(4) . ?
C14A O4A 1.258(4) . ?
C14A C11A 1.489(4) 6_566 ?
O1B C1B 1.282(4) . ?
O2B C1B 1.258(4) . ?
C1B C2B 1.470(5) . ?
C2B C3B 1.385(4) . ?
C2B C7B 1.391(5) . ?
C3B C4B 1.383(5) . ?
C4B C5B 1.397(5) . ?
C5B C6B 1.404(5) . ?
C5B C8B 1.478(5) . ?
C6B C7B 1.381(5) . ?
C8B C13B 1.379(5) . ?
C8B C9B 1.402(5) . ?
C9B C10B 1.376(5) . ?
C10B C11B 1.385(5) . ?
C11B C12B 1.379(5) . ?
C11B C14B 1.485(5) . ?
C12B C13B 1.386(5) . ?
C14B O4B 1.249(4) . ?
C14B O3B 1.270(4) . ?
O4B Zn1 2.118(2) 1_545 ?
O1C C1C 1.277(4) . ?
O2C C1C 1.247(4) . ?
O2C Zn1 2.044(2) 1_545 ?
C1C C2C 1.500(5) . ?
C2C C7C 1.374(5) . ?
C2C C3C 1.382(5) . ?
C3C C4C 1.380(5) . ?
C4C C5C 1.390(5) . ?
C5C C6C 1.402(5) . ?
C5C C8C 1.483(5) . ?
C6C C7C 1.383(5) . ?
C8C C9C 1.384(5) . ?
C8C C13C 1.389(5) . ?
C9C C10C 1.386(5) . ?
C10C C11C 1.398(4) . ?
C11C C12C 1.374(5) . ?
C11C C14C 1.506(4) . ?
C12C C13C 1.383(5) . ?
C14C O4C 1.243(4) . ?
C14C O3C 1.269(4) . ?
O3C Zn3 1.943(2) 6_536 ?
O4C Zn1 2.063(2) 6_546 ?
N1D C6D 1.332(4) . ?
N1D C2D 1.346(4) . ?
C2D C3D 1.365(5) . ?
C3D C4D 1.382(5) . ?
C4D C5D 1.371(5) . ?
C4D C7D 1.482(5) . ?
C5D C6D 1.374(5) . ?
C7D N8D 1.266(5) . ?
N8D N9D 1.416(5) . ?
N9D C10D 1.246(5) . ?
C10D C11D 1.484(6) . ?
C11D C12D 1.368(6) . ?
C11D C16D 1.375(6) . ?
C13D N14D 1.302(5) . ?
C13D C12D 1.386(5) . ?
N14D C15D 1.333(4) . ?
N14D Zn3 2.076(3) 8_546 ?
C15D C16D 1.367(5) . ?

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
O1A Zn1 O2C 177.38(10) . 1_565 ?
O1A Zn1 O4C 87.04(10) . 6_545 ?
O2C Zn1 O4C 90.70(10) 1_565 6_545 ?
O1A Zn1 O3A 96.11(10) . . ?
O2C Zn1 O3A 86.19(10) 1_565 . ?
O4C Zn1 O3A 176.27(11) 6_545 . ?
O1A Zn1 O4B 89.10(9) . 1_565 ?
O2C Zn1 O4B 89.77(10) 1_565 1_565 ?
O4C Zn1 O4B 94.85(9) 6_545 1_565 ?
O3A Zn1 O4B 87.20(10) . 1_565 ?
O1A Zn1 O1B 89.12(9) . . ?
O2C Zn1 O1B 92.06(9) 1_565 . ?
O4C Zn1 O1B 86.39(9) 6_545 . ?
O3A Zn1 O1B 91.66(9) . . ?
O4B Zn1 O1B 177.77(9) 1_565 . ?
O4A Zn2 O2A 111.94(12) . . ?
O4A Zn2 N1D 100.29(10) . . ?
O2A Zn2 N1D 97.18(10) . . ?
O4A Zn2 O1B 109.02(10) . . ?
O2A Zn2 O1B 96.82(9) . . ?
N1D Zn2 O1B 139.71(10) . . ?
O4A Zn2 O2B 97.96(12) . . ?
O2A Zn2 O2B 147.38(11) . . ?
N1D Zn2 O2B 89.76(11) . . ?
O1B Zn2 O2B 59.83(9) . . ?
O4A Zn2 C1B 106.00(11) . . ?
O2A Zn2 C1B 123.66(11) . . ?
N1D Zn2 C1B 115.43(11) . . ?
O1B Zn2 C1B 30.21(10) . . ?
O2B Zn2 C1B 29.63(10) . . ?
O1C Zn3 O3C 120.38(12) . 6_535 ?
O1C Zn3 N14D 97.63(11) . 8_445 ?
O3C Zn3 N14D 97.62(11) 6_535 8_445 ?
O1C Zn3 O3B 125.49(12) . . ?
O3C Zn3 O3B 111.12(12) 6_535 . ?
N14D Zn3 O3B 91.95(11) 8_445 . ?
O1C Zn3 O4B 94.19(10) . . ?
O3C Zn3 O4B 98.68(10) 6_535 . ?
N14D Zn3 O4B 151.39(11) 8_445 . ?
O3B Zn3 O4B 60.21(9) . . ?
O1C Zn3 C14B 112.39(12) . . ?
O3C Zn3 C14B 106.73(12) 6_535 . ?
N14D Zn3 C14B 122.13(12) 8_445 . ?
O3B Zn3 C14B 30.38(10) . . ?
O4B Zn3 C14B 29.84(10) . . ?
C1A O1A Zn1 139.9(2) . . ?
C1A O2A Zn2 121.9(2) . . ?
O1A C1A O2A 125.2(3) . . ?
O1A C1A C2A 118.0(3) . . ?
O2A C1A C2A 116.8(3) . . ?
C3A C2A C7A 118.3(3) . . ?
C3A C2A C1A 121.0(3) . . ?
C7A C2A C1A 120.6(3) . . ?
C4A C3A C2A 120.7(4) . . ?
C3A C4A C5A 121.9(3) . . ?
C4A C5A C6A 116.6(3) . . ?
C4A C5A C8A 122.7(3) . . ?
C6A C5A C8A 120.6(3) . . ?
C7A C6A C5A 121.5(3) . . ?
C6A C7A C2A 121.0(3) . . ?
C13A C8A C9A 114.9(4) . . ?
C13A C8A C5A 123.1(3) . . ?
C9A C8A C5A 121.6(4) . . ?
C8A C9A C10A 121.4(5) . . ?
C11A C10A C9A 121.1(4) . . ?
C10A C11A C12A 116.7(4) . . ?
C10A C11A C14A 121.9(3) . 6_565 ?
C12A C11A C14A 121.4(3) . 6_565 ?
C11A C12A C13A 122.0(4) . . ?
C8A C13A C12A 122.9(4) . . ?
O3A C14A O4A 125.8(3) . . ?
O3A C14A C11A 117.6(3) . 6_566 ?
O4A C14A C11A 116.6(3) . 6_566 ?
C14A O3A Zn1 139.0(2) . . ?
C14A O4A Zn2 125.6(2) . . ?
C1B O1B Zn2 94.3(2) . . ?
C1B O1B Zn1 134.2(2) . . ?
Zn2 O1B Zn1 101.78(9) . . ?
C1B O2B Zn2 87.3(2) . . ?
O2B C1B O1B 118.6(3) . . ?
O2B C1B C2B 120.3(3) . . ?
O1B C1B C2B 121.1(3) . . ?
O2B C1B Zn2 63.09(19) . . ?
O1B C1B Zn2 55.52(17) . . ?
C2B C1B Zn2 175.4(2) . . ?
C3B C2B C7B 118.8(3) . . ?
C3B C2B C1B 120.7(3) . . ?
C7B C2B C1B 120.4(3) . . ?
C4B C3B C2B 119.9(3) . . ?
C3B C4B C5B 122.3(3) . . ?
C4B C5B C6B 117.0(3) . . ?
C4B C5B C8B 122.4(3) . . ?
C6B C5B C8B 120.4(3) . . ?
C7B C6B C5B 120.8(4) . . ?
C6B C7B C2B 121.2(3) . . ?
C13B C8B C9B 117.8(3) . . ?
C13B C8B C5B 122.1(3) . . ?
C9B C8B C5B 120.1(3) . . ?
C10B C9B C8B 120.5(4) . . ?
C9B C10B C11B 121.2(4) . . ?
C12B C11B C10B 118.6(3) . . ?
C12B C11B C14B 120.6(3) . . ?
C10B C11B C14B 120.9(3) . . ?
C11B C12B C13B 120.5(3) . . ?
C8B C13B C12B 121.4(4) . . ?
O4B C14B O3B 119.1(3) . . ?
O4B C14B C11B 121.5(3) . . ?
O3B C14B C11B 119.4(3) . . ?
O4B C14B Zn3 62.30(18) . . ?
O3B C14B Zn3 56.85(18) . . ?
C11B C14B Zn3 176.2(3) . . ?
C14B O3B Zn3 92.8(2) . . ?
C14B O4B Zn1 159.7(2) . 1_545 ?
C14B O4B Zn3 87.9(2) . . ?
Zn1 O4B Zn3 104.56(10) 1_545 . ?
C1C O1C Zn3 123.6(2) . . ?
C1C O2C Zn1 138.9(2) . 1_545 ?
O2C C1C O1C 125.8(3) . . ?
O2C C1C C2C 117.2(3) . . ?
O1C C1C C2C 116.9(3) . . ?
C7C C2C C3C 118.2(3) . . ?
C7C C2C C1C 121.0(3) . . ?
C3C C2C C1C 120.8(3) . . ?
C4C C3C C2C 121.5(4) . . ?
C3C C4C C5C 120.6(4) . . ?
C4C C5C C6C 117.7(3) . . ?
C4C C5C C8C 121.1(4) . . ?
C6C C5C C8C 121.2(3) . . ?
C7C C6C C5C 120.5(4) . . ?
C2C C7C C6C 121.4(4) . . ?
C9C C8C C13C 118.4(3) . . ?
C9C C8C C5C 120.4(3) . . ?
C13C C8C C5C 121.1(3) . . ?
C8C C9C C10C 121.1(3) . . ?
C9C C10C C11C 120.0(4) . . ?
C12C C11C C10C 118.9(3) . . ?
C12C C11C C14C 121.1(3) . . ?
C10C C11C C14C 120.0(3) . . ?
C11C C12C C13C 120.9(3) . . ?
C12C C13C C8C 120.7(4) . . ?
O4C C14C O3C 127.0(3) . . ?
O4C C14C C11C 117.4(3) . . ?
O3C C14C C11C 115.6(3) . . ?
C14C O3C Zn3 128.5(2) . 6_536 ?
C14C O4C Zn1 138.0(2) . 6_546 ?
C6D N1D C2D 119.6(3) . . ?
C6D N1D Zn2 122.9(2) . . ?
C2D N1D Zn2 117.5(2) . . ?
N1D C2D C3D 121.5(3) . . ?
C2D C3D C4D 119.4(3) . . ?
C5D C4D C3D 118.4(3) . . ?
C5D C4D C7D 120.3(4) . . ?
C3D C4D C7D 121.3(4) . . ?
C4D C5D C6D 120.1(3) . . ?
N1D C6D C5D 121.0(3) . . ?
N8D C7D C4D 119.5(4) . . ?
C7D N8D N9D 111.5(4) . . ?
C10D N9D N8D 111.6(4) . . ?
N9D C10D C11D 119.9(4) . . ?
C12D C11D C16D 116.7(4) . . ?
C12D C11D C10D 120.4(4) . . ?
C16D C11D C10D 122.8(4) . . ?
N14D C13D C12D 121.9(4) . . ?
C11D C12D C13D 120.4(4) . . ?
C13D N14D C15D 118.8(3) . . ?
C13D N14D Zn3 122.1(2) . 8_546 ?
C15D N14D Zn3 118.8(3) . 8_546 ?
N14D C15D C16D 122.1(4) . . ?
C15D C16D C11D 120.2(4) . . ?

_refine_diff_density_max         1.276
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.084

_shelxl_version_number           2014-3



# start Validation Reply Form
_vrf_CHEMW03_Compound2           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Crystal structure contains voids in which solvent molecules could not
be located given the absence of electron density found in the Fourier difference
map. Therefore, there is a discrepancy between the crystallographic formula and
the chemical formula.
;
_vrf_PLAT213_Compound2           
;
PROBLEM: Atom C10A            has ADP max/min Ratio .....        4.5 prolat
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
_vrf_PLAT230_Compound2           
;
PROBLEM: Hirshfeld Test Diff for    C8A    --  C9A     ..       15.7 s.u.  
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
_vrf_PLAT241_Compound2           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C10A Check 
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
_vrf_PLAT242_Compound2           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       C11A Check 
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
# end Validation Reply Form
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1431700'
_audit_update_record             
;
2015-12-11 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{[bis(mu4-biphenyl-4,4'-dicarboxylato-kO:kO':kO'':kO''')(mu-1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene)dizinc(II)]heptakisdimethylformamide}
_chemical_formula_moiety         'C40 H26 N4 O8 Zn2, 7 (C3 H7 N O)'
_chemical_formula_structural     'C40 H26 N4 O8 Zn2, 7 (C3 H7 N O)'
_chemical_formula_sum            'C61 H75 N11 O15 Zn2'
_chemical_formula_weight         1333.09
_chemical_compound_source        'synthesis as described'


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.174(2)
_cell_length_b                   15.185(2)
_cell_length_c                   18.174(2)
_cell_angle_alpha                81.094(3)
_cell_angle_beta                 84.734(3)
_cell_angle_gamma                78.952(3)
_cell_volume                     4052.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    45908
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      23.37

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.004 -0.003 0.003 2644.1 25.5
_platon_squeeze_details          
;
;

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1396
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_T_max  0.974


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            45908
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.243
_diffrn_reflns_theta_max         23.374
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.798
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.798
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.798
_reflns_number_total             11698
_reflns_number_gt                8035
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0962P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11698
_refine_ls_number_parameters     487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1605
_refine_ls_wR_factor_gt          0.1542
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_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 0.62471(3) 0.37942(3) 0.70083(2) 0.01858(16) Uani 1 1 d . . . . .
Zn2 Zn 0.61105(3) 0.35260(3) 0.86323(2) 0.01742(15) Uani 1 1 d . . . . .
O1A O 0.6060(2) 0.22575(17) 0.84378(15) 0.0257(7) Uani 1 1 d . . . . .
O2A O 0.6518(2) 0.24118(16) 0.72202(14) 0.0285(7) Uani 1 1 d . . . . .
C1A C 0.6278(3) 0.1959(3) 0.7823(2) 0.0332(12) Uani 1 1 d . . . . .
C2A C 0.6309(4) 0.0965(3) 0.7812(2) 0.0410(14) Uani 1 1 d . . . . .
C3A C 0.6635(5) 0.0556(3) 0.7194(3) 0.0611(19) Uani 1 1 d . . . . .
H3A H 0.6879 0.0889 0.6779 0.073 Uiso 1 1 calc R U . . .
C4A C 0.6604(5) -0.0343(3) 0.7182(3) 0.066(2) Uani 1 1 d . . . . .
H4A H 0.6818 -0.0606 0.6756 0.079 Uiso 1 1 calc R U . . .
C5A C 0.6262(5) -0.0850(3) 0.7787(3) 0.065(2) Uani 1 1 d . . . . .
C6A C 0.5967(5) -0.0439(3) 0.8407(3) 0.077(2) Uani 1 1 d . . . . .
H6A H 0.5738 -0.0777 0.8827 0.092 Uiso 1 1 calc R U . . .
C7A C 0.5997(4) 0.0442(3) 0.8428(3) 0.0580(18) Uani 1 1 d . . . . .
H7A H 0.5804 0.0693 0.8863 0.070 Uiso 1 1 calc R U . . .
C8A C 0.6229(5) -0.1816(3) 0.7767(3) 0.0611(19) Uani 1 1 d . . . . .
C9A C 0.6336(4) -0.2460(3) 0.8434(3) 0.0560(17) Uani 1 1 d . . . . .
H9A H 0.6451 -0.2278 0.8876 0.067 Uiso 1 1 calc R U . . .
C10A C 0.6270(4) -0.3350(3) 0.8416(3) 0.0509(16) Uani 1 1 d . . . . .
H10A H 0.6326 -0.3756 0.8856 0.061 Uiso 1 1 calc R U . . .
C11A C 0.6122(4) -0.3663(3) 0.7770(2) 0.0391(13) Uani 1 1 d . . . . .
C12A C 0.6001(5) -0.3016(3) 0.7117(3) 0.0602(19) Uani 1 1 d . . . . .
H12A H 0.5896 -0.3202 0.6674 0.072 Uiso 1 1 calc R U . . .
C13A C 0.6035(5) -0.2131(3) 0.7128(3) 0.072(2) Uani 1 1 d . . . . .
H13A H 0.5926 -0.1722 0.6696 0.086 Uiso 1 1 calc R U . . .
C14A C 0.6085(3) -0.4617(3) 0.7767(2) 0.0270(11) Uani 1 1 d . . . . .
O3A O 0.6195(2) -0.51339(17) 0.83687(15) 0.0252(7) Uani 1 1 d . . . . .
O4A O 0.5988(2) -0.48689(17) 0.71537(15) 0.0299(8) Uani 1 1 d . . . . .
O1B O 0.74881(18) 0.32526(19) 0.84271(16) 0.0291(7) Uani 1 1 d . . . . .
O2B O 0.7534(2) 0.3801(2) 0.72081(16) 0.0319(7) Uani 1 1 d . . . . .
C1B C 0.7897(3) 0.3509(3) 0.7824(2) 0.0289(11) Uani 1 1 d . . . . .
C2B C 0.8864(3) 0.3526(3) 0.7842(2) 0.0331(11) Uani 1 1 d . . . . .
C3B C 0.9351(3) 0.3885(4) 0.7191(3) 0.0495(14) Uani 1 1 d . . . . .
H3B H 0.9057 0.4096 0.6753 0.059 Uiso 1 1 calc R U . . .
C4B C 1.0229(3) 0.3922(4) 0.7201(3) 0.0506(15) Uani 1 1 d . . . . .
H4B H 1.0527 0.4156 0.6765 0.061 Uiso 1 1 calc R U . . .
C5B C 1.0708(3) 0.3623(4) 0.7840(3) 0.0432(13) Uani 1 1 d . . . . .
C6B C 1.0227(3) 0.3270(4) 0.8481(3) 0.0513(15) Uani 1 1 d . . . . .
H6B H 1.0520 0.3070 0.8920 0.062 Uiso 1 1 calc R U . . .
C7B C 0.9332(3) 0.3214(4) 0.8474(3) 0.0406(13) Uani 1 1 d . . . . .
H7B H 0.9038 0.2960 0.8903 0.049 Uiso 1 1 calc R U . . .
C8B C 1.1668(3) 0.3695(4) 0.7853(3) 0.0398(13) Uani 1 1 d . . . . .
C9B C 1.2016(3) 0.3854(3) 0.8495(3) 0.0391(13) Uani 1 1 d . . . . .
H9B H 1.1643 0.3938 0.8923 0.047 Uiso 1 1 calc R U . . .
C10B C 1.2897(3) 0.3886(3) 0.8488(3) 0.0379(12) Uani 1 1 d . . . . .
H10B H 1.3121 0.3979 0.8924 0.046 Uiso 1 1 calc R U . . .
C11B C 1.3487(3) 0.3788(3) 0.7869(2) 0.0288(11) Uani 1 1 d . . . . .
C12B C 1.3129(3) 0.3626(3) 0.7222(2) 0.0320(11) Uani 1 1 d . . . . .
H12B H 1.3505 0.3551 0.6794 0.038 Uiso 1 1 calc R U . . .
C13B C 1.2258(3) 0.3581(3) 0.7215(3) 0.0412(13) Uani 1 1 d . . . . .
H13B H 1.2038 0.3472 0.6783 0.049 Uiso 1 1 calc R U . . .
C14B C 0.4473(3) 0.3784(3) 0.7879(2) 0.0205(9) Uani 1 1 d . . . . .
O3B O 0.47626(18) 0.38609(17) 0.84873(15) 0.0219(6) Uani 1 1 d . . . . .
O4B O 0.49244(19) 0.37275(18) 0.72579(15) 0.0255(7) Uani 1 1 d . . . . .
N1C N 0.6260(2) 0.3917(2) 0.58804(17) 0.0219(8) Uani 1 1 d . . . . .
C2C C 0.6193(6) 0.4686(4) 0.5461(3) 0.093(3) Uani 1 1 d . . . . .
H2C H 0.6163 0.5203 0.5686 0.112 Uiso 1 1 calc R U . . .
C3C C 0.6164(7) 0.4787(4) 0.4711(3) 0.120(4) Uani 1 1 d . . . . .
H3C H 0.6115 0.5363 0.4436 0.143 Uiso 1 1 calc R U . . .
C4C C 0.6206(4) 0.4047(3) 0.4353(2) 0.0437(14) Uani 1 1 d . . . . .
C5C C 0.6190(7) 0.3307(4) 0.4802(3) 0.115(4) Uani 1 1 d . . . . .
H5C H 0.6131 0.2789 0.4610 0.138 Uiso 1 1 calc R U . . .
C6C C 0.6255(6) 0.3257(4) 0.5544(3) 0.102(3) Uani 1 1 d . . . . .
H6C H 0.6299 0.2688 0.5828 0.122 Uiso 1 1 calc R U . . .
C7C C 0.6145(4) 0.4152(4) 0.3538(3) 0.0591(17) Uani 1 1 d . . . . .
H7C H 0.6049 0.4730 0.3268 0.071 Uiso 1 1 calc R U . . .
N8C N 0.6219(4) 0.3477(3) 0.3202(2) 0.0558(14) Uani 1 1 d . . . . .
N9C N 0.6195(3) 0.3725(3) 0.2428(2) 0.0497(13) Uani 1 1 d . . . . .
C10C C 0.6145(4) 0.3065(3) 1.2109(2) 0.0493(15) Uani 1 1 d . . . . .
H10C H 0.6126 0.2502 1.2391 0.059 Uiso 1 1 calc R U . . .
C11C C 0.6115(4) 0.3171(3) 1.1299(3) 0.0443(14) Uani 1 1 d . . . . .
C12C C 0.5997(4) 0.4027(3) 1.0885(2) 0.0384(10) Uani 1 1 d . . . . .
H12C H 0.5938 0.4544 1.1114 0.046 Uiso 1 1 calc R U . . .
C13C C 0.5969(4) 0.4086(3) 1.0126(2) 0.0382(10) Uani 1 1 d . . . . .
H13C H 0.5884 0.4660 0.9848 0.046 Uiso 1 1 calc R U . . .
N14C N 0.6054(2) 0.3378(2) 0.97655(17) 0.0218(8) Uani 1 1 d . . . . .
C15C C 0.6128(4) 0.2540(3) 1.0169(2) 0.0436(14) Uani 1 1 d . . . . .
H15C H 0.6144 0.2038 0.9929 0.052 Uiso 1 1 calc R U . . .
C16C C 0.6180(4) 0.2427(3) 1.0939(2) 0.0513(16) Uani 1 1 d . . . . .
H16C H 0.6259 0.1848 1.1210 0.062 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O2B 2.021(3) . ?
Zn1 N1C 2.028(3) . ?
Zn1 O4B 2.035(3) . ?
Zn1 O2A 2.043(2) . ?
Zn1 O4A 2.046(3) 1_565 ?
Zn1 Zn2 2.9098(6) . ?
Zn2 O1A 2.028(2) . ?
Zn2 N14C 2.033(3) . ?
Zn2 O3B 2.042(3) . ?
Zn2 O3A 2.043(3) 1_565 ?
Zn2 O1B 2.062(3) . ?
O1A C1A 1.264(5) . ?
O2A C1A 1.262(5) . ?
C1A C2A 1.504(6) . ?
C2A C7A 1.371(6) . ?
C2A C3A 1.374(6) . ?
C3A C4A 1.378(6) . ?
C4A C5A 1.363(7) . ?
C5A C6A 1.369(7) . ?
C5A C8A 1.483(6) . ?
C6A C7A 1.353(6) . ?
C8A C13A 1.397(7) . ?
C8A C9A 1.435(7) . ?
C9A C10A 1.380(6) . ?
C10A C11A 1.385(6) . ?
C11A C12A 1.421(6) . ?
C11A C14A 1.461(6) . ?
C12A C13A 1.357(6) . ?
C14A O3A 1.248(5) . ?
C14A O4A 1.262(5) . ?
O3A Zn2 2.043(3) 1_545 ?
O4A Zn1 2.046(3) 1_545 ?
O1B C1B 1.254(5) . ?
O2B C1B 1.272(5) . ?
C1B C2B 1.476(6) . ?
C2B C7B 1.377(6) . ?
C2B C3B 1.428(7) . ?
C3B C4B 1.346(7) . ?
C4B C5B 1.396(7) . ?
C5B C6B 1.406(7) . ?
C5B C8B 1.484(6) . ?
C6B C7B 1.379(6) . ?
C8B C9B 1.394(6) . ?
C8B C13B 1.410(6) . ?
C9B C10B 1.347(6) . ?
C10B C11B 1.380(6) . ?
C11B C12B 1.412(6) . ?
C11B C14B 1.496(6) 1_655 ?
C12B C13B 1.339(6) . ?
C14B O3B 1.257(5) . ?
C14B O4B 1.271(5) . ?
C14B C11B 1.496(6) 1_455 ?
N1C C6C 1.253(6) . ?
N1C C2C 1.284(6) . ?
C2C C3C 1.352(7) . ?
C3C C4C 1.373(7) . ?
C4C C5C 1.285(7) . ?
C4C C7C 1.473(6) . ?
C5C C6C 1.351(8) . ?
C7C N8C 1.254(6) . ?
N8C N9C 1.400(5) . ?
N9C C10C 1.250(6) 1_554 ?
C10C N9C 1.250(6) 1_556 ?
C10C C11C 1.460(6) . ?
C11C C16C 1.375(6) . ?
C11C C12C 1.385(6) . ?
C12C C13C 1.372(6) . ?
C13C N14C 1.323(5) . ?
N14C C15C 1.357(5) . ?
C15C C16C 1.392(6) . ?

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
O2B Zn1 N1C 104.04(13) . . ?
O2B Zn1 O4B 157.09(12) . . ?
N1C Zn1 O4B 98.87(13) . . ?
O2B Zn1 O2A 88.59(12) . . ?
N1C Zn1 O2A 97.85(12) . . ?
O4B Zn1 O2A 87.86(12) . . ?
O2B Zn1 O4A 86.46(12) . 1_565 ?
N1C Zn1 O4A 100.25(12) . 1_565 ?
O4B Zn1 O4A 89.94(12) . 1_565 ?
O2A Zn1 O4A 161.88(11) . 1_565 ?
O2B Zn1 Zn2 80.07(8) . . ?
N1C Zn1 Zn2 175.15(9) . . ?
O4B Zn1 Zn2 77.02(8) . . ?
O2A Zn1 Zn2 79.55(7) . . ?
O4A Zn1 Zn2 82.44(8) 1_565 . ?
O1A Zn2 N14C 102.16(12) . . ?
O1A Zn2 O3B 88.12(11) . . ?
N14C Zn2 O3B 98.53(12) . . ?
O1A Zn2 O3A 156.74(11) . 1_565 ?
N14C Zn2 O3A 101.09(12) . 1_565 ?
O3B Zn2 O3A 88.89(11) . 1_565 ?
O1A Zn2 O1B 88.97(12) . . ?
N14C Zn2 O1B 99.03(13) . . ?
O3B Zn2 O1B 162.43(11) . . ?
O3A Zn2 O1B 86.96(11) 1_565 . ?
O1A Zn2 Zn1 79.93(8) . . ?
N14C Zn2 Zn1 177.40(9) . . ?
O3B Zn2 Zn1 83.03(8) . . ?
O3A Zn2 Zn1 76.81(8) 1_565 . ?
O1B Zn2 Zn1 79.40(8) . . ?
C1A O1A Zn2 125.4(3) . . ?
C1A O2A Zn1 124.0(3) . . ?
O2A C1A O1A 125.7(4) . . ?
O2A C1A C2A 116.6(4) . . ?
O1A C1A C2A 117.6(4) . . ?
C7A C2A C3A 118.1(4) . . ?
C7A C2A C1A 120.0(4) . . ?
C3A C2A C1A 121.9(4) . . ?
C2A C3A C4A 120.7(4) . . ?
C5A C4A C3A 120.8(4) . . ?
C4A C5A C6A 117.7(4) . . ?
C4A C5A C8A 120.3(4) . . ?
C6A C5A C8A 122.0(4) . . ?
C7A C6A C5A 122.2(5) . . ?
C6A C7A C2A 120.4(4) . . ?
C13A C8A C9A 117.0(4) . . ?
C13A C8A C5A 122.7(5) . . ?
C9A C8A C5A 120.2(4) . . ?
C10A C9A C8A 119.8(4) . . ?
C9A C10A C11A 122.6(4) . . ?
C10A C11A C12A 117.0(4) . . ?
C10A C11A C14A 121.1(4) . . ?
C12A C11A C14A 121.9(4) . . ?
C13A C12A C11A 121.3(4) . . ?
C12A C13A C8A 122.2(5) . . ?
O3A C14A O4A 124.6(3) . . ?
O3A C14A C11A 117.2(4) . . ?
O4A C14A C11A 118.1(4) . . ?
C14A O3A Zn2 130.2(3) . 1_545 ?
C14A O4A Zn1 122.0(3) . 1_545 ?
C1B O1B Zn2 124.5(3) . . ?
C1B O2B Zn1 125.9(3) . . ?
O1B C1B O2B 125.2(4) . . ?
O1B C1B C2B 117.2(4) . . ?
O2B C1B C2B 117.5(4) . . ?
C7B C2B C3B 117.2(4) . . ?
C7B C2B C1B 122.7(4) . . ?
C3B C2B C1B 120.1(4) . . ?
C4B C3B C2B 121.0(5) . . ?
C3B C4B C5B 122.4(5) . . ?
C4B C5B C6B 116.5(5) . . ?
C4B C5B C8B 122.1(4) . . ?
C6B C5B C8B 121.4(4) . . ?
C7B C6B C5B 121.6(5) . . ?
C2B C7B C6B 121.3(4) . . ?
C9B C8B C13B 118.3(4) . . ?
C9B C8B C5B 121.5(4) . . ?
C13B C8B C5B 120.2(4) . . ?
C10B C9B C8B 119.4(4) . . ?
C9B C10B C11B 123.5(4) . . ?
C10B C11B C12B 116.7(4) . . ?
C10B C11B C14B 122.9(4) . 1_655 ?
C12B C11B C14B 120.2(4) . 1_655 ?
C13B C12B C11B 121.0(4) . . ?
C12B C13B C8B 121.0(4) . . ?
O3B C14B O4B 126.9(4) . . ?
O3B C14B C11B 117.3(3) . 1_455 ?
O4B C14B C11B 115.8(3) . 1_455 ?
C14B O3B Zn2 119.7(3) . . ?
C14B O4B Zn1 128.5(2) . . ?
C6C N1C C2C 114.7(4) . . ?
C6C N1C Zn1 122.4(3) . . ?
C2C N1C Zn1 122.6(3) . . ?
N1C C2C C3C 123.6(5) . . ?
C2C C3C C4C 120.5(5) . . ?
C5C C4C C3C 113.3(5) . . ?
C5C C4C C7C 125.2(5) . . ?
C3C C4C C7C 120.9(5) . . ?
C4C C5C C6C 122.1(5) . . ?
N1C C6C C5C 125.3(6) . . ?
N8C C7C C4C 121.4(5) . . ?
C7C N8C N9C 112.1(4) . . ?
C10C N9C N8C 111.4(4) 1_554 . ?
N9C C10C C11C 120.6(5) 1_556 . ?
C16C C11C C12C 119.1(4) . . ?
C16C C11C C10C 120.6(4) . . ?
C12C C11C C10C 120.3(4) . . ?
C13C C12C C11C 117.8(4) . . ?
N14C C13C C12C 124.2(4) . . ?
C13C N14C C15C 118.5(4) . . ?
C13C N14C Zn2 121.4(3) . . ?
C15C N14C Zn2 120.1(3) . . ?
N14C C15C C16C 120.4(4) . . ?
C11C C16C C15C 119.9(4) . . ?

_refine_diff_density_max         0.916
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.082

_shelxl_version_number           2014-3



# start Validation Reply Form
_vrf_CHEMW03_Compound3           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Crystal structure contains voids in which solvent molecules could not
be located given the absence of electron density found in the Fourier difference
map. Therefore, there is a discrepancy between the crystallographic formula and
the chemical formula.
;
_vrf_THETM01_Compound3           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Given the presence of voids in the structure, the crystal does not
diffract at high 2theta angles.
;
_vrf_PLAT213_Compound3           
;
PROBLEM: Atom C3C             has ADP max/min Ratio .....        4.1 prolat
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
_vrf_PLAT241_Compound3           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C3C Check 
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
_vrf_PLAT242_Compound3           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C4C Check 
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
# end Validation Reply Form_exptl_crystal_preparation       Luminescent
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound4
_database_code_depnum_ccdc_archive 'CCDC 1431701'
_audit_update_record             
;
2015-12-11 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{[diaquatris(mu4-biphenyl-4,4'-dicarboxylato-kO:kO':kO'':kO''')dimethylformamide(mu4-oxo)tetrazinc(II)]heptakisdimethylformamidetrihydrate}
_chemical_formula_moiety         'C31 H33 N O15 Zn4, 7(C3 H7 N O), 3(H2O)'
_chemical_formula_structural     'C31 H33 N O15 Zn4, 7(C3 H7 N O), 3(H2O)'
_chemical_formula_sum            'C66 H88 N8 O25 Zn4'
_chemical_formula_weight         1655.00
_chemical_compound_source        'synthesis as described'


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P nnm'
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_Int_Tables_number      58

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

_cell_length_a                   17.256(4)
_cell_length_b                   23.227(6)
_cell_length_c                   25.426(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10191(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16811
_cell_measurement_theta_min      1.19
_cell_measurement_theta_max      18.89

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.023 0.004 -0.003 6052.7 1926.1
_platon_squeeze_details          
;
;

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    none
_exptl_crystal_F_000             3440
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_T_max  0.955


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16811
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.187
_diffrn_reflns_theta_max         18.886
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.436
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.436
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.436
_reflns_number_total             4128
_reflns_number_gt                3788
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1209P)²+29.2136P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4128
_refine_ls_number_parameters     347
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.2018
_refine_ls_wR_factor_gt          0.1975
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.079
_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 0.29128(6) -0.58348(4) 0.0000 0.0321(5) Uani 1 2 d S T P . .
Zn2 Zn 0.29801(6) -0.72083(5) 0.0000 0.0392(5) Uani 1 2 d S T P . .
Zn3 Zn 0.16391(5) -0.65747(3) -0.06221(3) 0.0394(4) Uani 1 1 d . . . . .
O1C O 0.2300(3) -0.65296(19) 0.0000 0.0222(14) Uani 1 2 d S T P D .
O1A O 0.2742(3) -0.53456(19) 0.06099(17) 0.0501(14) Uani 1 1 d . . . . .
O2A O 0.1850(3) -0.58559(19) 0.10325(18) 0.0455(13) Uani 1 1 d . . . . .
C1A C 0.2307(4) -0.5425(3) 0.0991(3) 0.0341(17) Uani 1 1 d . . . . .
C2A C 0.2302(4) -0.4999(3) 0.1415(3) 0.0360(17) Uani 1 1 d . . . . .
C5A C 0.2323(5) -0.4198(3) 0.2255(3) 0.055(2) Uani 1 1 d . . . . .
C3A C 0.2590(10) -0.4440(8) 0.1333(7) 0.034(5) Uiso 0.422(14) 1 d . . P A 1
H3A H 0.2812 -0.4358 0.1009 0.041 Uiso 0.422(14) 1 calc R U P A 1
C4A C 0.2566(8) -0.4004(7) 0.1705(6) 0.019(4) Uiso 0.422(14) 1 d . . P A 1
H4A H 0.2688 -0.3623 0.1626 0.022 Uiso 0.422(14) 1 calc R U P A 1
C6A C 0.2141(9) -0.4748(7) 0.2299(6) 0.025(5) Uiso 0.422(14) 1 d . . P A 1
H6A H 0.2011 -0.4877 0.2634 0.030 Uiso 0.422(14) 1 calc R U P A 1
C7A C 0.2125(10) -0.5151(6) 0.1901(6) 0.021(4) Uiso 0.422(14) 1 d . . P A 1
H7A H 0.1990 -0.5530 0.1974 0.025 Uiso 0.422(14) 1 calc R U P A 1
C3A1 C 0.2871(11) -0.4606(7) 0.1467(7) 0.062(5) Uiso 0.578(14) 1 d . . P A 2
H3A1 H 0.3291 -0.4614 0.1238 0.075 Uiso 0.578(14) 1 calc R U P A 2
C4A1 C 0.2836(9) -0.4183(6) 0.1865(6) 0.048(4) Uiso 0.578(14) 1 d . . P A 2
H4A1 H 0.3188 -0.3880 0.1854 0.058 Uiso 0.578(14) 1 calc R U P A 2
C6A1 C 0.1726(11) -0.4596(6) 0.2234(6) 0.061(5) Uiso 0.578(14) 1 d . . P A 2
H6A1 H 0.1323 -0.4575 0.2476 0.073 Uiso 0.578(14) 1 calc R U P A 2
C7A1 C 0.1725(11) -0.5043(7) 0.1838(6) 0.067(5) Uiso 0.578(14) 1 d . . P A 2
H7A1 H 0.1373 -0.5346 0.1851 0.081 Uiso 0.578(14) 1 calc R U P A 2
C8A C 0.2639(6) -0.8795(3) -0.2315(3) 0.070(3) Uani 1 1 d . . . . .
C9A C 0.2119(7) -0.8344(5) -0.2346(5) 0.112(4) Uani 1 1 d . . . . .
H9A H 0.1803 -0.8311 -0.2640 0.135 Uiso 1 1 calc R U . . .
C10A C 0.2054(7) -0.7911(5) -0.1922(5) 0.116(4) Uani 1 1 d . . . . .
H10A H 0.1699 -0.7610 -0.1937 0.139 Uiso 1 1 calc R U . . .
C11A C 0.2582(5) -0.7983(4) -0.1477(3) 0.066(2) Uani 1 1 d . . . . .
C12A C 0.3061(5) -0.8458(4) -0.1458(4) 0.093(4) Uani 1 1 d . . . . .
H12A H 0.3364 -0.8527 -0.1163 0.112 Uiso 1 1 calc R U . . .
C13A C 0.3088(6) -0.8840(5) -0.1890(4) 0.096(3) Uani 1 1 d . . . . .
H13A H 0.3441 -0.9141 -0.1877 0.115 Uiso 1 1 calc R U . . .
C14A C 0.2535(6) -0.7564(5) -0.1042(4) 0.084(3) Uani 1 1 d . . . . .
O3A O 0.2944(3) -0.7686(3) -0.0622(2) 0.0770(18) Uani 1 1 d . . . . .
O4A O 0.2081(7) -0.7136(3) -0.1103(2) 0.159(4) Uani 1 1 d . . . . .
O1B O 0.4035(3) -0.5944(3) 0.0000 0.0423(17) Uani 1 2 d S T P . .
O2B O 0.4049(4) -0.6927(3) 0.0000 0.0532(19) Uani 1 2 d S T P . .
C1B C 0.4384(6) -0.6445(5) 0.0000 0.034(3) Uani 1 2 d S T P . .
C2B C 0.5225(5) -0.6416(4) 0.0000 0.036(3) Uani 1 2 d S T P . .
C3B C 0.5664(6) -0.6933(6) 0.0000 0.115(6) Uani 1 2 d S T P . .
H3B H 0.5407 -0.7285 0.0000 0.138 Uiso 1 2 calc R U P . .
C4B C 0.6443(9) -0.6926(7) 0.0000 0.104(5) Uani 1 2 d S T P . .
H4B H 0.6708 -0.7274 0.0000 0.125 Uiso 1 2 calc R U P . .
C5B C 0.6872(5) -0.6410(4) 0.0000 0.031(2) Uani 1 2 d S T P B .
C6B C 0.6474(5) -0.5938(5) 0.0000 0.053(3) Uani 1 2 d S T P . .
H6B H 0.6741 -0.5590 0.0000 0.064 Uiso 1 2 calc R U P . .
C7B C 0.5661(6) -0.5920(5) 0.0000 0.051(3) Uani 1 2 d S T P . .
H7B H 0.5411 -0.5566 0.0000 0.061 Uiso 1 2 calc R U P . .
C8B C 0.7746(6) -0.6430(4) 0.0000 0.038(3) Uani 1 2 d S T P . .
C11B C 0.9363(5) -0.6465(4) 0.0000 0.043(3) Uani 1 2 d S T P . .
C14B C 1.0239(8) -0.6441(5) 0.0000 0.057(3) Uani 1 2 d S T P . .
O3B O 1.0567(3) -0.6462(4) 0.0421(4) 0.173(5) Uani 1 1 d . . . . .
C9B C 0.8176(8) -0.6121(6) 0.0318(6) 0.046(4) Uani 0.5 1 d . . P B -3
H9B H 0.7942 -0.5874 0.0557 0.055 Uiso 0.5 1 calc R U P B -3
C10B C 0.8958(10) -0.6160(7) 0.0301(7) 0.067(5) Uani 0.5 1 d . . P B -3
H10B H 0.9227 -0.5933 0.0541 0.080 Uiso 0.5 1 calc R U P B -3
C12B C 0.8956(7) -0.6754(5) -0.0447(5) 0.035(3) Uani 0.5 1 d . . P B -3
H12B H 0.9220 -0.6934 -0.0720 0.043 Uiso 0.5 1 calc R U P B -3
C13B C 0.8133(8) -0.6731(6) -0.0421(6) 0.047(4) Uani 0.5 1 d . . P B -3
H13B H 0.7840 -0.6912 -0.0680 0.057 Uiso 0.5 1 calc R U P B -3
O1E O 0.0218(12) -0.5460(9) -0.2036(6) 0.160(7) Uiso 0.5 1 d D . P C -3
C2E C 0.0286(18) -0.5356(7) -0.1564(7) 0.149(10) Uiso 0.5 1 d D . P C -3
N3E N 0.0319(8) -0.4883(6) -0.1284(5) 0.086(5) Uiso 0.5 1 d D . P C -3
C4E C 0.016(2) -0.4355(8) -0.1554(11) 0.192(14) Uiso 0.5 1 d D . P C -3
C5E C 0.0368(11) -0.4927(9) -0.0724(5) 0.099(6) Uiso 0.5 1 d D . P C -3
O1D O 0.1331(7) -0.7455(5) -0.0250(4) 0.061(5) Uiso 0.400(10) 1 d D . P D -3
C2D C 0.080(2) -0.7648(9) 0.0022(16) 0.60(8) Uiso 0.400(10) 1 d D . P D -3
O1W O 0.0794(9) -0.6776(7) -0.1253(6) 0.237(6) Uiso 1 1 d . . . . .
N3D N 0.0506(9) -0.8167(6) 0.0000 0.122(7) Uiso 0.80(2) 2 d DS . P . .
C4D C -0.0271(11) -0.838(2) 0.0000 0.42(5) Uiso 0.80(2) 2 d DS . P D .
C5D C 0.1162(15) -0.8543(15) 0.0000 0.37(4) Uiso 0.80(2) 2 d DS . P D .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1C 1.930(5) . ?
Zn1 O1A 1.945(4) 6 ?
Zn1 O1A 1.945(4) . ?
Zn1 O1B 1.954(6) . ?
Zn2 O3A 1.934(5) . ?
Zn2 O3A 1.934(5) 6 ?
Zn2 O2B 1.957(7) . ?
Zn2 O1C 1.965(5) . ?
Zn3 O3B 1.937(6) 6_455 ?
Zn3 O4A 1.943(7) . ?
Zn3 O1C 1.952(3) . ?
Zn3 O2A 2.002(5) 6 ?
Zn3 O1W 2.218(15) . ?
Zn3 O1D 2.314(12) . ?
O1C Zn3 1.952(3) 6 ?
O1A C1A 1.239(8) . ?
O2A C1A 1.279(7) . ?
O2A Zn3 2.002(5) 6 ?
C1A C2A 1.462(9) . ?
C2A C7A 1.320(15) . ?
C2A C3A1 1.347(16) . ?
C2A C3A 1.406(18) . ?
C2A C7A1 1.470(18) . ?
C5A C6A 1.320(16) . ?
C5A C4A1 1.331(15) . ?
C5A C6A1 1.384(16) . ?
C5A C8A 1.440(11) 7_666 ?
C5A C4A 1.529(17) . ?
C3A C4A 1.39(2) . ?
C6A C7A 1.38(2) . ?
C3A1 C4A1 1.413(19) . ?
C6A1 C7A1 1.45(2) . ?
C8A C13A 1.334(12) . ?
C8A C9A 1.382(14) . ?
C8A C5A 1.440(11) 7_655 ?
C9A C10A 1.479(16) . ?
C10A C11A 1.461(14) . ?
C11A C12A 1.379(12) . ?
C11A C14A 1.476(13) . ?
C12A C13A 1.411(13) . ?
C14A O4A 1.276(12) . ?
C14A O3A 1.310(11) . ?
O1B C1B 1.309(11) . ?
O2B C1B 1.260(11) . ?
C1B C2B 1.453(14) . ?
C2B C7B 1.375(14) . ?
C2B C3B 1.420(16) . ?
C3B C4B 1.344(18) . ?
C4B C5B 1.408(18) . ?
C5B C6B 1.295(13) . ?
C5B C8B 1.508(14) . ?
C6B C7B 1.403(14) . ?
C8B C9B 1.311(15) . ?
C8B C13B 1.442(16) . ?
C11B C10B 1.255(18) . ?
C11B C12B 1.495(14) . ?
C11B C14B 1.512(17) . ?
C14B O3B 1.212(9) . ?
C14B O3B 1.213(9) 6 ?
O3B Zn3 1.937(6) 6_655 ?
C9B C10B 1.35(2) . ?
C12B C13B 1.423(19) . ?
O1E C2E 1.2301(11) . ?
C2E N3E 1.3099(11) . ?
N3E C5E 1.4299(11) . ?
N3E C4E 1.4300(11) . ?
O1D C2D 1.2300(11) . ?
C2D N3D 1.3100(11) . ?
N3D C4D 1.4300(11) . ?
N3D C5D 1.4300(11) . ?

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
O1C Zn1 O1A 113.91(16) . 6 ?
O1C Zn1 O1A 113.91(16) . . ?
O1A Zn1 O1A 105.7(3) 6 . ?
O1C Zn1 O1B 115.8(3) . . ?
O1A Zn1 O1B 103.09(19) 6 . ?
O1A Zn1 O1B 103.08(19) . . ?
O3A Zn2 O3A 109.8(4) . 6 ?
O3A Zn2 O2B 102.83(19) . . ?
O3A Zn2 O2B 102.83(19) 6 . ?
O3A Zn2 O1C 116.2(2) . . ?
O3A Zn2 O1C 116.2(2) 6 . ?
O2B Zn2 O1C 107.2(3) . . ?
O3B Zn3 O4A 129.1(5) 6_455 . ?
O3B Zn3 O1C 109.7(3) 6_455 . ?
O4A Zn3 O1C 108.5(3) . . ?
O3B Zn3 O2A 101.5(2) 6_455 6 ?
O4A Zn3 O2A 99.2(3) . 6 ?
O1C Zn3 O2A 105.75(19) . 6 ?
O3B Zn3 O1W 65.9(5) 6_455 . ?
O4A Zn3 O1W 70.2(5) . . ?
O1C Zn3 O1W 168.9(4) . . ?
O2A Zn3 O1W 85.3(4) 6 . ?
O3B Zn3 O1D 78.0(4) 6_455 . ?
O4A Zn3 O1D 75.9(4) . . ?
O1C Zn3 O1D 81.4(3) . . ?
O2A Zn3 O1D 172.5(3) 6 . ?
O1W Zn3 O1D 87.7(5) . . ?
Zn1 O1C Zn3 111.40(15) . . ?
Zn1 O1C Zn3 111.40(15) . 6 ?
Zn3 O1C Zn3 108.2(3) . 6 ?
Zn1 O1C Zn2 110.1(3) . . ?
Zn3 O1C Zn2 107.81(16) . . ?
Zn3 O1C Zn2 107.80(16) 6 . ?
C1A O1A Zn1 128.9(4) . . ?
C1A O2A Zn3 136.2(4) . 6 ?
O1A C1A O2A 123.6(6) . . ?
O1A C1A C2A 118.7(6) . . ?
O2A C1A C2A 117.7(6) . . ?
C7A C2A C3A 117.8(10) . . ?
C7A C2A C1A 120.7(8) . . ?
C3A1 C2A C1A 121.7(8) . . ?
C3A C2A C1A 120.9(8) . . ?
C3A1 C2A C7A1 117.9(10) . . ?
C1A C2A C7A1 119.8(8) . . ?
C4A1 C5A C6A1 119.0(10) . . ?
C6A C5A C8A 125.2(9) . 7_666 ?
C4A1 C5A C8A 121.1(9) . 7_666 ?
C6A1 C5A C8A 119.8(9) . 7_666 ?
C6A C5A C4A 115.4(9) . . ?
C8A C5A C4A 119.3(8) 7_666 . ?
C4A C3A C2A 124.3(14) . . ?
C3A C4A C5A 114.6(12) . . ?
C5A C6A C7A 126.8(13) . . ?
C2A C7A C6A 120.1(12) . . ?
C2A C3A1 C4A1 120.7(13) . . ?
C5A C4A1 C3A1 122.9(12) . . ?
C5A C6A1 C7A1 120.5(13) . . ?
C6A1 C7A1 C2A 117.3(13) . . ?
C13A C8A C9A 118.8(9) . . ?
C13A C8A C5A 122.5(7) . 7_655 ?
C9A C8A C5A 118.7(10) . 7_655 ?
C8A C9A C10A 121.6(11) . . ?
C11A C10A C9A 116.0(10) . . ?
C12A C11A C10A 119.5(9) . . ?
C12A C11A C14A 122.3(8) . . ?
C10A C11A C14A 118.0(9) . . ?
C11A C12A C13A 119.7(9) . . ?
C8A C13A C12A 124.2(9) . . ?
O4A C14A O3A 126.8(10) . . ?
O4A C14A C11A 117.1(9) . . ?
O3A C14A C11A 116.0(9) . . ?
C14A O3A Zn2 124.0(6) . . ?
C14A O4A Zn3 133.3(7) . . ?
C1B O1B Zn1 124.8(6) . . ?
C1B O2B Zn2 136.8(6) . . ?
O2B C1B O1B 125.4(8) . . ?
O2B C1B C2B 119.9(10) . . ?
O1B C1B C2B 114.7(9) . . ?
C7B C2B C3B 114.6(9) . . ?
C7B C2B C1B 125.8(9) . . ?
C3B C2B C1B 119.6(9) . . ?
C4B C3B C2B 121.5(13) . . ?
C3B C4B C5B 122.4(14) . . ?
C6B C5B C4B 116.2(11) . . ?
C6B C5B C8B 123.8(8) . . ?
C4B C5B C8B 120.0(10) . . ?
C5B C6B C7B 123.7(10) . . ?
C2B C7B C6B 121.5(10) . . ?
C9B C8B C13B 117.4(11) . . ?
C9B C8B C5B 123.3(9) . . ?
C13B C8B C5B 118.5(8) . . ?
C10B C11B C12B 117.0(11) . . ?
C10B C11B C14B 122.4(10) . . ?
C12B C11B C14B 119.1(7) . . ?
O3B C14B O3B 124.1(13) . 6 ?
O3B C14B C11B 117.7(7) . . ?
O3B C14B C11B 117.7(7) 6 . ?
C14B O3B Zn3 133.2(8) . 6_655 ?
C8B C9B C10B 120.6(14) . . ?
C11B C10B C9B 127.8(16) . . ?
C13B C12B C11B 114.6(11) . . ?
C12B C13B C8B 121.0(12) . . ?
O1E C2E N3E 134(2) . . ?
C2E N3E C5E 118.8(15) . . ?
C2E N3E C4E 116.7(18) . . ?
C5E N3E C4E 123.4(17) . . ?
C2D O1D Zn3 136.3(17) . . ?
O1D C2D N3D 127.0(19) . . ?
C2D N3D C4D 133(3) . . ?
C2D N3D C5D 105(3) . . ?
C4D N3D C5D 122(2) . . ?

_refine_diff_density_max         0.801
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.092

_shelxl_version_number           2014-3



# start Validation Reply Form
_vrf_CHEMW03_Compound4           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The different molecular weight is due to the disorder present
in the compound that prevents the location of solvent molecules placed in 
the large voids of the structure. The disorder also affects the ligands,
in such a way that the coordinated dimethylformamide molecule had to be 
refined with a lower occupation factor.
;
_vrf_THETM01_Compound4           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The presence of highly disordered solvent molecules present in the
voids of the structure makes single crystals of the compound, despite their
good quality, to diffract up to a low theta angle, which could not be improved
with longer measure times.
;
_vrf_PLAT043_Compound4           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      70.75 Check 
RESPONSE: The difference in the molecular weight is due to the disorder.
;
_vrf_PLAT602_Compound4           
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: Given the high disorder present in the solvent molecules occupying 
the voids, the remaining residual density has been removed by the SQUEEZE
routine.
;
_vrf_PLAT201_Compound4           
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          5 Report
RESPONSE: The atoms refined isotropically are severely disordered, which 
precludes their anisotropic refinement.
;
_vrf_PLAT213_Compound4           
;
PROBLEM: Atom O3B             has ADP max/min Ratio .....        4.1 prolat
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
_vrf_PLAT220_Compound4           
;
PROBLEM: Large Non-Solvent  C     Ueq(max)/Ueq(min) Range       10.0 Ratio 
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
_vrf_PLAT230_Compound4           
;
PROBLEM: Hirshfeld Test Diff for    O3B    --  C14B    ..       11.6 s.u.  
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
_vrf_PLAT241_Compound4           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        O4A Check 
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
_vrf_PLAT242_Compound4           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Zn3 Check 
RESPONSE: The presence of voids in the structure filled with disordered
solvent molecules that could not be placed affects thermal ellipsoids of 
some atoms belonging to the organic ligands.
;
# end Validation Reply Form
_exptl_crystal_preparation       Luminescent
