# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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 1415511'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{dimethylamonnium[(mu-4,4'-azobenzenedicarboxylate-k2O,O':k2O'',O''')(mu-acetato-kO:kO)cadmate(II)]}
_chemical_formula_moiety         'C16 H11 Cd N2 O6, C2 H8 N'
_chemical_formula_structural     'C16 H11 Cd N2 O6, C2 H8 N'
_chemical_formula_sum            'C18 H19 Cd N3 O6'
_chemical_formula_weight         480.73
_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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m c a'
_symmetry_space_group_name_Hall  '-C 2bc 2'
_symmetry_Int_Tables_number      64

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

_cell_length_a                   30.09(3)
_cell_length_b                   17.23(2)
_cell_length_c                   8.658(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4488(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1646
_cell_measurement_theta_min      1.35
_cell_measurement_theta_max      23.19

_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    1.438
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    1.008
_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  0.864
_exptl_absorpt_correction_T_max  0.939

# 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 0.250 0.033 0.250 36.0 7.1
2 0.250 0.533 0.250 36.0 7.1
3 0.750 0.533 0.250 36.0 7.1
4 0.750 0.033 0.250 36.0 7.1
5 0.250 0.467 0.750 36.0 6.5
6 0.250 0.967 0.750 36.0 6.5
7 0.750 0.967 0.750 36.0 6.5
8 0.750 0.467 0.750 36.0 6.5
_platon_squeeze_details          
;
;

_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  Xcalibur
_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            9596
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         23.19
_reflns_number_total             1646
_reflns_number_gt                1423
_reflns_threshold_expression     >2sigma(I)

_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     
'calc w=1/[σ²(Fo²)+(0.0791P)²+514.1306P] 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         1646
_refine_ls_number_parameters     122
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.1524
_refine_ls_wR_factor_ref         0.3321
_refine_ls_wR_factor_gt          0.3267
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd -0.5000 -0.06850(11) -0.1539(2) 0.0572(9) Uani 1 2 d S . .
O1A O -0.5571(5) -0.1627(8) -0.1690(18) 0.058(4) Uani 1 1 d . . .
O2A O -0.5580(6) -0.0638(9) -0.3232(16) 0.075(5) Uani 1 1 d . . .
C1A C -0.5738(8) -0.1246(11) -0.270(3) 0.056(6) Uani 1 1 d . . .
C2A C -0.6197(7) -0.1500(10) -0.333(2) 0.051(5) Uani 1 1 d . . .
C3A C -0.6406(6) -0.2168(12) -0.274(2) 0.053(5) Uani 1 1 d . . .
H3A H -0.6272 -0.2457 -0.1967 0.063 Uiso 1 1 calc R . .
C4A C -0.6808(6) -0.2385(14) -0.333(3) 0.058(6) Uani 1 1 d . . .
H4A H -0.6948 -0.2824 -0.2940 0.070 Uiso 1 1 calc R . .
C5A C -0.7009(6) -0.1971(11) -0.449(2) 0.046(5) Uani 1 1 d . . .
C6A C -0.6801(6) -0.1311(12) -0.508(2) 0.050(5) Uani 1 1 d . . .
H6A H -0.6937 -0.1026 -0.5860 0.060 Uiso 1 1 calc R . .
C7A C -0.6403(8) -0.1086(11) -0.452(2) 0.056(6) Uani 1 1 d . . .
H7A H -0.6263 -0.0651 -0.4937 0.067 Uiso 1 1 calc R . .
N8A N -0.7424(6) -0.2164(10) -0.516(2) 0.060(5) Uani 1 1 d . . .
O1B O -0.5000 -0.0590(9) 0.1009(18) 0.034(4) Uani 1 2 d S . .
C2B C -0.5000 -0.1199(10) 0.2097(19) 0.008(4) Uani 1 2 d S . .
O3B O -0.5000 -0.096(3) 0.362(6) 0.148(17) Uiso 0.50 2 d SP A 1
C4B C -0.5000 -0.188(5) 0.142(10) 0.28(4) Uiso 0.50 2 d SP A 1
O4B O -0.5000 -0.188(5) 0.142(10) 0.28(4) Uiso 0.50 2 d SP A 2
C3B C -0.5000 -0.096(3) 0.362(6) 0.148(17) Uiso 0.50 2 d SP A 2
N1C N -0.6794(13) 0.0000 0.0000 0.141(16) Uiso 1 2 d SD . .
C2C C -0.6537(14) 0.062(2) -0.073(8) 0.38(5) Uiso 1 1 d D . .
H2C1 H -0.6510 0.1048 -0.0027 0.563 Uiso 1 1 calc R . .
H2C2 H -0.6686 0.0787 -0.1651 0.563 Uiso 1 1 calc R . .
H2C3 H -0.6247 0.0428 -0.0989 0.563 Uiso 1 1 calc R . .


_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 O1B 2.212(15) . ?
Cd1 O2A 2.281(17) . ?
Cd1 O2A 2.281(17) 11_455 ?
Cd1 O1B 2.243(15) 9_455 ?
Cd1 O1A 2.365(13) . ?
Cd1 O1A 2.365(13) 11_455 ?
Cd1 C1A 2.62(2) . ?
Cd1 C1A 2.62(2) 11_455 ?
O1A C1A 1.21(2) . ?
O2A C1A 1.24(2) . ?
C1A C2A 1.55(3) . ?
C2A C3A 1.41(3) . ?
C2A C7A 1.40(3) . ?
C3A C4A 1.36(3) . ?
C4A C5A 1.37(3) . ?
C5A C6A 1.40(3) . ?
C5A N8A 1.42(3) . ?
C6A C7A 1.35(3) . ?
N8A N8A 1.28(3) 13_344 ?
O1B C2B 1.41(2) . ?
O1B Cd1 2.243(15) 9_455 ?
C2B C4B 1.32(8) . ?
C2B O3B 1.37(5) . ?
N1C C2C 1.460(10) . ?
N1C C2C 1.460(10) 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
O1B Cd1 O2A 129.7(4) . . ?
O1B Cd1 O2A 129.7(4) . 11_455 ?
O2A Cd1 O2A 99.8(8) . 11_455 ?
O1B Cd1 O1B 73.9(6) . 9_455 ?
O2A Cd1 O1B 95.6(5) . 9_455 ?
O2A Cd1 O1B 95.6(5) 11_455 9_455 ?
O1B Cd1 O1A 96.1(5) . . ?
O2A Cd1 O1A 55.5(5) . . ?
O2A Cd1 O1A 122.9(6) 11_455 . ?
O1B Cd1 O1A 133.0(4) 9_455 . ?
O1B Cd1 O1A 96.1(5) . 11_455 ?
O2A Cd1 O1A 122.9(6) . 11_455 ?
O2A Cd1 O1A 55.5(5) 11_455 11_455 ?
O1B Cd1 O1A 133.0(4) 9_455 11_455 ?
O1A Cd1 O1A 93.1(7) . 11_455 ?
O1B Cd1 C1A 114.3(5) . . ?
O2A Cd1 C1A 28.1(6) . . ?
O2A Cd1 C1A 114.4(6) 11_455 . ?
O1B Cd1 C1A 116.1(5) 9_455 . ?
O1A Cd1 C1A 27.4(5) . . ?
O1A Cd1 C1A 109.9(6) 11_455 . ?
O1B Cd1 C1A 114.3(5) . 11_455 ?
O2A Cd1 C1A 114.4(6) . 11_455 ?
O2A Cd1 C1A 28.1(6) 11_455 11_455 ?
O1B Cd1 C1A 116.0(5) 9_455 11_455 ?
O1A Cd1 C1A 109.9(6) . 11_455 ?
O1A Cd1 C1A 27.4(5) 11_455 11_455 ?
C1A Cd1 C1A 115.6(9) . 11_455 ?
C1A O1A Cd1 88.3(12) . . ?
C1A O2A Cd1 91.5(15) . . ?
O1A C1A O2A 125(2) . . ?
O1A C1A C2A 118.4(18) . . ?
O2A C1A C2A 117(2) . . ?
O1A C1A Cd1 64.3(12) . . ?
O2A C1A Cd1 60.3(12) . . ?
C2A C1A Cd1 174.1(14) . . ?
C3A C2A C7A 119(2) . . ?
C3A C2A C1A 120.1(19) . . ?
C7A C2A C1A 120.8(18) . . ?
C4A C3A C2A 119(2) . . ?
C3A C4A C5A 121(2) . . ?
C4A C5A C6A 119.7(19) . . ?
C4A C5A N8A 124.6(19) . . ?
C6A C5A N8A 115.6(17) . . ?
C7A C6A C5A 120.0(19) . . ?
C6A C7A C2A 120.8(19) . . ?
N8A N8A C5A 116(2) 13_344 . ?
C2B O1B Cd1 127.7(11) . . ?
C2B O1B Cd1 126.3(11) . 9_455 ?
Cd1 O1B Cd1 106.1(6) . 9_455 ?
C4B C2B O3B 133(5) . . ?
C4B C2B O1B 112(4) . . ?
O3B C2B O1B 115(2) . . ?
C2C N1C C2C 116.1(15) . 3 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        23.19
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.861
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.220


# start Validation Reply Form
_vrf_PLAT242_Compound1           
;
PROBLEM: Low       Ueq as Compared to Neighbors for .....        C2B Check 
RESPONSE: The crystal structure presents a disordered acetate molecule that
has been disordered in two equivalent dispositions with regard to the 
coordinated C-O moiety, which makes the disordered C3B and O4B atoms to 
present a higher Ueq compared to the non-disordered C2B atom.
;
_vrf_PLAT041_Compound1           
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The difference in the calculated and reported sum formula is due 
to the lack of hydrogen atoms refined for the disordered acetato anion.
;
_vrf_PLAT046_Compound1           
;
PROBLEM: Reported Z, MW and D(calc) are Inconsistent ....      1.423       
RESPONSE: This problem comes from the lack of refined hydrogen atoms in
the acetato anion that makes the reported formula not fit the calculated
one.
;
_vrf_PLAT068_Compound1           
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check
RESPONSE: This problem comes from the lack of refined hydrogen atoms in
the acetato anion that makes the reported formula not fit the calculated
one.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dimethylformamide'
_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 1415512'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{[(mu4-4,4'-azobenzenedicarboxylate-kO:k2O,O':kO'':k2O'',O''')(mu-4,4'-azobenzenedicarboxylate-k2O,O':k2O'',O''')tetrakis(dimethylsulfoxide)dicadmium(II)]dimethylsulfoxide}
_chemical_formula_moiety         'C48 H38 Cd3 N8 O14'
_chemical_formula_structural     'C48 H38 Cd3 N8 O14'
_chemical_formula_sum            'C38 H46 Cd2 N4 O13 S5'
_chemical_formula_weight         1151.94
_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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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

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                   31.831(6)
_cell_length_b                   7.884(2)
_cell_length_c                   19.449(4)
_cell_angle_alpha                90.000
_cell_angle_beta                 107.912(7)
_cell_angle_gamma                90.000
_cell_volume                     4644(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10985
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      23.30

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    none
_exptl_crystal_F_000             2328
_exptl_absorpt_coefficient_mu    1.205
_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  0.663
_exptl_absorpt_correction_T_max  0.840

_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  Xcalibur
_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            10985
_diffrn_reflns_av_R_equivalents  0.1320
_diffrn_reflns_av_unetI/netI     0.1584
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.67
_diffrn_reflns_theta_max         23.30
_reflns_number_total             3343
_reflns_number_gt                2058
_reflns_threshold_expression     >2sigma(I)

_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          
;
 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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0547P)²+8.7623P] 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         3343
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1353
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1281
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.029
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.71712(2) 0.21919(10) 0.89358(4) 0.0165(3) Uani 1 1 d . . .
O1A O 0.6847(2) 0.1075(10) 0.7740(3) 0.026(2) Uani 1 1 d . . .
O2A O 0.6419(2) 0.2564(10) 0.8209(3) 0.030(2) Uani 1 1 d . . .
C1A C 0.6476(3) 0.1654(13) 0.7704(5) 0.017(3) Uani 1 1 d . . .
C2A C 0.6092(3) 0.1265(14) 0.7069(5) 0.017(2) Uani 1 1 d . . .
C3A C 0.5672(3) 0.1836(14) 0.7027(5) 0.026(3) Uani 1 1 d . . .
H3A H 0.5632 0.2482 0.7401 0.031 Uiso 1 1 calc R . .
C4A C 0.5317(3) 0.1462(15) 0.6442(5) 0.027(3) Uani 1 1 d . . .
H4A H 0.5039 0.1842 0.6432 0.032 Uiso 1 1 calc R . .
C5A C 0.5360(3) 0.0543(15) 0.5870(5) 0.024(3) Uani 1 1 d . . .
C6A C 0.5783(3) -0.0086(14) 0.5900(5) 0.024(3) Uani 1 1 d . . .
H6A H 0.5818 -0.0726 0.5520 0.029 Uiso 1 1 calc R . .
C7A C 0.6143(3) 0.0256(14) 0.6498(5) 0.019(3) Uani 1 1 d . . .
H7A H 0.6419 -0.0180 0.6525 0.022 Uiso 1 1 calc R . .
N8A N 0.4958(3) 0.0280(13) 0.5279(5) 0.034(3) Uani 1 1 d . . .
O1B O 0.7085(2) 0.3264(10) 0.9999(4) 0.0284(19) Uani 1 1 d . . .
O2B O 0.7154(2) 0.3623(10) 1.1148(4) 0.033(2) Uani 1 1 d . . .
C1B C 0.6920(3) 0.3546(13) 1.0507(5) 0.014(2) Uani 1 1 d . . .
C2B C 0.6441(3) 0.3931(13) 1.0317(5) 0.014(2) Uani 1 1 d . . .
C3B C 0.6276(3) 0.4522(14) 1.0863(6) 0.023(3) Uani 1 1 d . . .
H3B H 0.6462 0.4667 1.1332 0.028 Uiso 1 1 calc R . .
C4B C 0.5824(3) 0.4891(15) 1.0690(6) 0.031(3) Uani 1 1 d . . .
H4B H 0.5709 0.5301 1.1044 0.037 Uiso 1 1 calc R . .
C5B C 0.5549(3) 0.4645(15) 0.9992(6) 0.025(3) Uani 1 1 d . . .
C6B C 0.5714(3) 0.4096(14) 0.9449(6) 0.023(3) Uani 1 1 d . . .
H6B H 0.5529 0.3985 0.8977 0.027 Uiso 1 1 calc R . .
C7B C 0.6163(3) 0.3711(15) 0.9625(5) 0.025(3) Uani 1 1 d . . .
H7B H 0.6275 0.3300 0.9269 0.030 Uiso 1 1 calc R . .
N8B N 0.5073(3) 0.4960(12) 0.9743(5) 0.032(3) Uani 1 1 d . . .
O1C O 0.7270(2) 0.4950(10) 0.8652(3) 0.030(2) Uani 1 1 d . . .
S2C S 0.70412(9) 0.5611(4) 0.78813(14) 0.0262(8) Uani 1 1 d . . .
C3C C 0.6553(3) 0.6631(16) 0.7914(6) 0.039(4) Uani 1 1 d . . .
H3C1 H 0.6359 0.5812 0.8022 0.058 Uiso 1 1 calc R . .
H3C2 H 0.6409 0.7150 0.7456 0.058 Uiso 1 1 calc R . .
H3C3 H 0.6626 0.7486 0.8284 0.058 Uiso 1 1 calc R . .
C4C C 0.7351(3) 0.7404(15) 0.7807(5) 0.033(3) Uani 1 1 d . . .
H4C1 H 0.7367 0.8167 0.8199 0.049 Uiso 1 1 calc R . .
H4C2 H 0.7211 0.7966 0.7356 0.049 Uiso 1 1 calc R . .
H4C3 H 0.7643 0.7061 0.7824 0.049 Uiso 1 1 calc R . .
O1D O 0.6925(2) -0.0320(10) 0.9264(4) 0.0283(19) Uani 1 1 d . . .
S2D S 0.67275(12) -0.0525(5) 0.98609(17) 0.0508(11) Uani 1 1 d . . .
C3D C 0.6186(4) -0.132(2) 0.9439(8) 0.086(6) Uani 1 1 d . . .
H3D1 H 0.6007 -0.0445 0.9150 0.129 Uiso 1 1 calc R . .
H3D2 H 0.6058 -0.1681 0.9802 0.129 Uiso 1 1 calc R . .
H3D3 H 0.6201 -0.2268 0.9137 0.129 Uiso 1 1 calc R . .
C4D C 0.6980(6) -0.2395(19) 1.0311(7) 0.101(7) Uani 1 1 d . . .
H4D1 H 0.6925 -0.3319 0.9973 0.152 Uiso 1 1 calc R . .
H4D2 H 0.6860 -0.2660 1.0693 0.152 Uiso 1 1 calc R . .
H4D3 H 0.7293 -0.2218 1.0509 0.152 Uiso 1 1 calc R . .
O1E O 0.5000 0.4457(19) 0.7500 0.078(5) Uani 1 2 d S . .
S2E S 0.5179(2) 0.6133(11) 0.7690(4) 0.058(2) Uani 0.50 1 d P . -1
C3E C 0.4860(8) 0.730(2) 0.8081(10) 0.134(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1C 2.288(8) . ?
Cd1 O1D 2.292(7) . ?
Cd1 O2B 2.294(7) 7_657 ?
Cd1 O1B 2.327(7) . ?
Cd1 O2A 2.396(6) . ?
Cd1 O1A 2.403(7) . ?
Cd1 O1B 2.647(7) 7_657 ?
Cd1 C1A 2.748(10) . ?
O1A C1A 1.249(11) . ?
O2A C1A 1.273(11) . ?
C1A C2A 1.479(13) . ?
C2A C3A 1.388(13) . ?
C2A C7A 1.415(13) . ?
C3A C4A 1.366(14) . ?
C4A C5A 1.369(14) . ?
C5A C6A 1.420(14) . ?
C5A N8A 1.447(13) . ?
C6A C7A 1.385(13) . ?
N8A N8A 1.273(16) 5_656 ?
O1B C1B 1.273(11) . ?
O1B Cd1 2.647(7) 7_657 ?
O2B C1B 1.242(11) . ?
O2B Cd1 2.294(7) 7_657 ?
C1B C2B 1.485(12) . ?
C2B C7B 1.375(13) . ?
C2B C3B 1.401(13) . ?
C3B C4B 1.402(13) . ?
C4B C5B 1.385(14) . ?
C5B C6B 1.384(13) . ?
C5B N8B 1.463(12) . ?
C6B C7B 1.398(13) . ?
N8B N8B 1.225(15) 5_667 ?
O1C S2C 1.543(7) . ?
S2C C4C 1.755(11) . ?
S2C C3C 1.768(10) . ?
O1D S2D 1.488(7) . ?
S2D C4D 1.776(15) . ?
S2D C3D 1.780(13) . ?
O1E S2E 1.442(14) . ?
O1E S2E 1.442(14) 2_656 ?
S2E C3E 1.712(18) . ?
S2E C3E 1.729(18) 2_656 ?
C3E S2E 1.729(18) 2_656 ?

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 Cd1 O1D 166.5(2) . . ?
O1C Cd1 O2B 92.7(3) . 7_657 ?
O1D Cd1 O2B 100.7(3) . 7_657 ?
O1C Cd1 O1B 86.1(3) . . ?
O1D Cd1 O1B 85.5(3) . . ?
O2B Cd1 O1B 122.3(3) 7_657 . ?
O1C Cd1 O2A 85.9(3) . . ?
O1D Cd1 O2A 84.5(3) . . ?
O2B Cd1 O2A 141.2(2) 7_657 . ?
O1B Cd1 O2A 96.3(2) . . ?
O1C Cd1 O1A 99.5(2) . . ?
O1D Cd1 O1A 82.6(3) . . ?
O2B Cd1 O1A 87.8(2) 7_657 . ?
O1B Cd1 O1A 149.4(2) . . ?
O2A Cd1 O1A 54.5(2) . . ?
O1C Cd1 O1B 99.3(2) . 7_657 ?
O1D Cd1 O1B 88.0(2) . 7_657 ?
O2B Cd1 O1B 52.2(2) 7_657 7_657 ?
O1B Cd1 O1B 71.1(3) . 7_657 ?
O2A Cd1 O1B 165.8(2) . 7_657 ?
O1A Cd1 O1B 136.2(2) . 7_657 ?
O1C Cd1 C1A 94.0(3) . . ?
O1D Cd1 C1A 81.8(3) . . ?
O2B Cd1 C1A 114.5(3) 7_657 . ?
O1B Cd1 C1A 123.2(3) . . ?
O2A Cd1 C1A 27.6(2) . . ?
O1A Cd1 C1A 27.0(2) . . ?
O1B Cd1 C1A 161.4(3) 7_657 . ?
C1A O1A Cd1 92.1(6) . . ?
C1A O2A Cd1 91.8(6) . . ?
O1A C1A O2A 121.4(9) . . ?
O1A C1A C2A 119.7(9) . . ?
O2A C1A C2A 118.9(9) . . ?
O1A C1A Cd1 60.9(5) . . ?
O2A C1A Cd1 60.6(5) . . ?
C2A C1A Cd1 176.0(7) . . ?
C3A C2A C7A 118.4(9) . . ?
C3A C2A C1A 121.0(9) . . ?
C7A C2A C1A 120.5(9) . . ?
C4A C3A C2A 120.9(10) . . ?
C3A C4A C5A 121.9(10) . . ?
C4A C5A C6A 118.7(9) . . ?
C4A C5A N8A 116.0(9) . . ?
C6A C5A N8A 125.3(10) . . ?
C7A C6A C5A 119.7(10) . . ?
C6A C7A C2A 120.3(9) . . ?
N8A N8A C5A 111.2(11) 5_656 . ?
C1B O1B Cd1 160.5(7) . . ?
C1B O1B Cd1 84.3(6) . 7_657 ?
Cd1 O1B Cd1 108.9(3) . 7_657 ?
C1B O2B Cd1 101.6(6) . 7_657 ?
O2B C1B O1B 121.5(9) . . ?
O2B C1B C2B 119.6(9) . . ?
O1B C1B C2B 118.7(9) . . ?
C7B C2B C3B 120.3(9) . . ?
C7B C2B C1B 121.3(9) . . ?
C3B C2B C1B 118.4(9) . . ?
C2B C3B C4B 118.9(10) . . ?
C5B C4B C3B 119.9(10) . . ?
C6B C5B C4B 121.2(10) . . ?
C6B C5B N8B 113.5(9) . . ?
C4B C5B N8B 125.3(9) . . ?
C5B C6B C7B 118.7(10) . . ?
C2B C7B C6B 120.9(9) . . ?
N8B N8B C5B 110.6(11) 5_667 . ?
S2C O1C Cd1 119.8(4) . . ?
O1C S2C C4C 104.1(5) . . ?
O1C S2C C3C 106.0(5) . . ?
C4C S2C C3C 99.1(6) . . ?
S2D O1D Cd1 125.0(4) . . ?
O1D S2D C4D 103.8(7) . . ?
O1D S2D C3D 105.0(6) . . ?
C4D S2D C3D 99.3(8) . . ?
S2E O1E S2E 47.1(7) . 2_656 ?
O1E S2E C3E 111.3(9) . . ?
O1E S2E C3E 110.3(8) . 2_656 ?
C3E S2E C3E 101.8(13) . 2_656 ?
S2E C3E S2E 39.1(6) . 2_656 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        23.30
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.168

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dimethylsulfoxide'
_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 1415513'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{[tris(mu4-4,4'-azobenzenedicarboxylate-kO:kO,O':kO'':kO'',O''')bis(dimethylformamide)tricadmium(II)]}
_chemical_formula_moiety         'C48 H38 Cd3 N8 O14'
_chemical_formula_structural     'C48 H38 Cd3 N8 O14'
_chemical_formula_sum            'C48 H38 Cd3 N8 O14'
_chemical_formula_weight         1288.09
_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'
Cd Cd -0.8075 1.2024 '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'

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

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

_cell_length_a                   10.7515(7)
_cell_length_b                   10.7424(7)
_cell_length_c                   11.0098(8)
_cell_angle_alpha                95.683(2)
_cell_angle_beta                 96.940(2)
_cell_angle_gamma                96.596(2)
_cell_volume                     1245.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15005
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      23.29

_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    1.717
_exptl_crystal_density_method    none
_exptl_crystal_F_000             638
_exptl_absorpt_coefficient_mu    1.343
_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  0.828
_exptl_absorpt_correction_T_max  0.926

_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  Xcalibur
_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            15005
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         23.29
_reflns_number_total             3575
_reflns_number_gt                3373
_reflns_threshold_expression     >2sigma(I)

_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          
;
 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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0158P)²+1.3588P] 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         3575
_refine_ls_number_parameters     333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0176
_refine_ls_wR_factor_ref         0.0433
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.5000 0.5000 0.5000 0.00616(7) Uani 1 2 d S . .
Cd2 Cd 0.294769(14) 0.286100(14) 0.300824(14) 0.00871(6) Uani 1 1 d . . .
O1A O 0.64772(14) 0.66367(14) 0.47099(14) 0.0117(3) Uani 1 1 d . . .
O2A O 0.64652(15) 0.85425(14) 0.56808(14) 0.0151(4) Uani 1 1 d . . .
C1A C 0.6345(2) 0.7797(2) 0.4706(2) 0.0109(5) Uani 1 1 d . . .
C2A C 0.6084(2) 0.8298(2) 0.3488(2) 0.0129(5) Uani 1 1 d . . .
C3A C 0.6301(2) 0.7603(2) 0.2416(2) 0.0175(5) Uani 1 1 d . . .
H3A H 0.6574 0.6815 0.2452 0.021 Uiso 1 1 calc R . .
C4A C 0.6112(3) 0.8083(2) 0.1293(2) 0.0217(6) Uani 1 1 d . . .
H4A H 0.6307 0.7647 0.0582 0.026 Uiso 1 1 calc R . .
C5A C 0.5626(2) 0.9225(2) 0.1244(2) 0.0205(6) Uani 1 1 d . . .
C6A C 0.5401(3) 0.9925(2) 0.2311(2) 0.0217(6) Uani 1 1 d . . .
H6A H 0.5083 1.0691 0.2269 0.026 Uiso 1 1 calc R . .
C7A C 0.5657(2) 0.9468(2) 0.3432(2) 0.0183(5) Uani 1 1 d . . .
H7A H 0.5544 0.9945 0.4153 0.022 Uiso 1 1 calc R . .
N8A N 0.5427(2) 0.9643(2) 0.00452(19) 0.0246(5) Uani 1 1 d . . .
O1B O 0.34930(14) 0.54719(14) 0.35811(14) 0.0127(3) Uani 1 1 d . . .
O2B O 0.16356(15) 0.42587(14) 0.32974(15) 0.0153(4) Uani 1 1 d . . .
C1B C 0.2308(2) 0.5316(2) 0.3587(2) 0.0113(5) Uani 1 1 d . . .
C2B C 0.1656(2) 0.6429(2) 0.3943(2) 0.0125(5) Uani 1 1 d . . .
C3B C 0.2309(2) 0.7644(2) 0.4112(2) 0.0181(5) Uani 1 1 d . . .
H3B H 0.3158 0.7765 0.4008 0.022 Uiso 1 1 calc R . .
C4B C 0.1701(2) 0.8671(2) 0.4435(2) 0.0210(6) Uani 1 1 d . . .
H4B H 0.2132 0.9483 0.4533 0.025 Uiso 1 1 calc R . .
C5B C 0.0432(2) 0.8472(2) 0.4613(2) 0.0191(6) Uani 1 1 d . . .
C6B C -0.0220(2) 0.7266(2) 0.4461(2) 0.0206(6) Uani 1 1 d . . .
H6B H -0.1062 0.7141 0.4590 0.025 Uiso 1 1 calc R . .
C7B C 0.0392(2) 0.6252(2) 0.4117(2) 0.0165(5) Uani 1 1 d . . .
H7B H -0.0047 0.5442 0.4000 0.020 Uiso 1 1 calc R . .
N8B N -0.0299(2) 0.94608(19) 0.4945(2) 0.0234(5) Uani 1 1 d . . .
O1C O 0.55697(15) 0.36346(14) 0.35180(14) 0.0143(4) Uani 1 1 d . . .
O2C O 0.43107(15) 0.32110(16) 0.17250(15) 0.0179(4) Uani 1 1 d . . .
C1C C 0.5382(2) 0.3549(2) 0.2360(2) 0.0128(5) Uani 1 1 d . . .
C2C C 0.6487(2) 0.3848(2) 0.1680(2) 0.0164(5) Uani 1 1 d . . .
C3C C 0.7711(2) 0.3886(3) 0.2261(2) 0.0263(6) Uani 1 1 d . . .
H3C H 0.7853 0.3708 0.3072 0.032 Uiso 1 1 calc R . .
C4C C 0.8725(2) 0.4193(3) 0.1628(3) 0.0325(7) Uani 1 1 d . . .
H4C H 0.9548 0.4202 0.2006 0.039 Uiso 1 1 calc R . .
C5C C 0.8500(3) 0.4487(3) 0.0426(2) 0.0283(7) Uani 1 1 d . . .
C6C C 0.7282(3) 0.4422(3) -0.0166(3) 0.0341(7) Uani 1 1 d . . .
H6C H 0.7139 0.4597 -0.0978 0.041 Uiso 1 1 calc R . .
C7C C 0.6278(3) 0.4094(3) 0.0461(2) 0.0268(6) Uani 1 1 d . . .
H7C H 0.5456 0.4037 0.0065 0.032 Uiso 1 1 calc R . .
N8C N 0.9479(2) 0.4860(3) -0.0303(2) 0.0352(6) Uani 1 1 d . . .
O1D O 0.14136(17) 0.14672(17) 0.19529(17) 0.0288(4) Uani 1 1 d . . .
C2D C 0.1361(3) 0.0308(3) 0.1740(3) 0.0370(8) Uani 1 1 d . . .
H2D H 0.2186 -0.0144 0.1736 0.044 Uiso 1 1 d . . .
N3D N 0.0277(3) -0.0464(3) 0.1539(3) 0.0555(9) Uani 1 1 d . . .
C4D C -0.0922(4) 0.0022(5) 0.1664(4) 0.0752(14) Uani 1 1 d . . .
H4D1 H -0.0771 0.0921 0.1872 0.113 Uiso 1 1 calc R . .
H4D2 H -0.1308 -0.0358 0.2302 0.113 Uiso 1 1 calc R . .
H4D3 H -0.1474 -0.0177 0.0899 0.113 Uiso 1 1 calc R . .
C5D C 0.0251(6) -0.1818(3) 0.1207(4) 0.101(2) Uani 1 1 d . . .
H5D1 H 0.1099 -0.2015 0.1202 0.151 Uiso 1 1 calc R . .
H5D2 H -0.0219 -0.2059 0.0404 0.151 Uiso 1 1 calc R . .
H5D3 H -0.0144 -0.2270 0.1798 0.151 Uiso 1 1 calc R . .


_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 O1B 2.2487(15) 2_666 ?
Cd1 O1B 2.2487(15) . ?
Cd1 O1C 2.2722(15) . ?
Cd1 O1C 2.2722(15) 2_666 ?
Cd1 O1A 2.3039(15) . ?
Cd1 O1A 2.3039(15) 2_666 ?
Cd1 Cd2 3.4096(2) 2_666 ?
Cd1 Cd2 3.4096(2) . ?
Cd2 O2C 2.1826(16) . ?
Cd2 O2B 2.2014(15) . ?
Cd2 O1D 2.2220(17) . ?
Cd2 O2A 2.2769(15) 2_666 ?
Cd2 O1A 2.5030(15) 2_666 ?
Cd2 C1A 2.725(2) 2_666 ?
O1A C1A 1.271(3) . ?
O1A Cd2 2.5030(15) 2_666 ?
O2A C1A 1.258(3) . ?
O2A Cd2 2.2769(15) 2_666 ?
C1A C2A 1.500(3) . ?
C1A Cd2 2.725(2) 2_666 ?
C2A C7A 1.391(3) . ?
C2A C3A 1.393(3) . ?
C3A C4A 1.388(3) . ?
C4A C5A 1.391(4) . ?
C5A C6A 1.392(4) . ?
C5A N8A 1.435(3) . ?
C6A C7A 1.382(3) . ?
N8A N8A 1.262(4) 2_675 ?
O1B C1B 1.267(3) . ?
O2B C1B 1.264(3) . ?
C1B C2B 1.497(3) . ?
C2B C7B 1.389(3) . ?
C2B C3B 1.393(3) . ?
C3B C4B 1.384(3) . ?
C4B C5B 1.397(4) . ?
C5B C6B 1.385(4) . ?
C5B N8B 1.437(3) . ?
C6B C7B 1.381(3) . ?
N8B N8B 1.246(4) 2_576 ?
O1C C1C 1.259(3) . ?
O2C C1C 1.268(3) . ?
C1C C2C 1.500(3) . ?
C2C C3C 1.386(4) . ?
C2C C7C 1.390(4) . ?
C3C C4C 1.388(4) . ?
C4C C5C 1.390(4) . ?
C5C C6C 1.382(4) . ?
C5C N8C 1.444(3) . ?
C6C C7C 1.381(4) . ?
N8C N8C 1.222(5) 2_765 ?
O1D C2D 1.238(3) . ?
C2D N3D 1.331(4) . ?
N3D C5D 1.460(5) . ?
N3D C4D 1.462(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
O1B Cd1 O1B 180.0 2_666 . ?
O1B Cd1 O1C 91.74(6) 2_666 . ?
O1B Cd1 O1C 88.26(6) . . ?
O1B Cd1 O1C 88.26(6) 2_666 2_666 ?
O1B Cd1 O1C 91.74(6) . 2_666 ?
O1C Cd1 O1C 180.0 . 2_666 ?
O1B Cd1 O1A 85.32(5) 2_666 . ?
O1B Cd1 O1A 94.68(5) . . ?
O1C Cd1 O1A 94.02(6) . . ?
O1C Cd1 O1A 85.98(6) 2_666 . ?
O1B Cd1 O1A 94.68(5) 2_666 2_666 ?
O1B Cd1 O1A 85.32(5) . 2_666 ?
O1C Cd1 O1A 85.98(6) . 2_666 ?
O1C Cd1 O1A 94.02(6) 2_666 2_666 ?
O1A Cd1 O1A 180.0 . 2_666 ?
O1B Cd1 Cd2 54.56(4) 2_666 2_666 ?
O1B Cd1 Cd2 125.44(4) . 2_666 ?
O1C Cd1 Cd2 124.82(4) . 2_666 ?
O1C Cd1 Cd2 55.18(4) 2_666 2_666 ?
O1A Cd1 Cd2 47.23(4) . 2_666 ?
O1A Cd1 Cd2 132.77(4) 2_666 2_666 ?
O1B Cd1 Cd2 125.44(4) 2_666 . ?
O1B Cd1 Cd2 54.56(4) . . ?
O1C Cd1 Cd2 55.18(4) . . ?
O1C Cd1 Cd2 124.82(4) 2_666 . ?
O1A Cd1 Cd2 132.77(4) . . ?
O1A Cd1 Cd2 47.23(4) 2_666 . ?
Cd2 Cd1 Cd2 180.000(4) 2_666 . ?
O2C Cd2 O2B 117.83(6) . . ?
O2C Cd2 O1D 105.02(7) . . ?
O2B Cd2 O1D 91.92(6) . . ?
O2C Cd2 O2A 112.07(6) . 2_666 ?
O2B Cd2 O2A 126.67(6) . 2_666 ?
O1D Cd2 O2A 92.50(6) . 2_666 ?
O2C Cd2 O1A 122.25(5) . 2_666 ?
O2B Cd2 O1A 82.36(5) . 2_666 ?
O1D Cd2 O1A 129.22(6) . 2_666 ?
O2A Cd2 O1A 54.99(5) 2_666 2_666 ?
O2C Cd2 C1A 121.74(6) . 2_666 ?
O2B Cd2 C1A 104.79(6) . 2_666 ?
O1D Cd2 C1A 111.55(7) . 2_666 ?
O2A Cd2 C1A 27.30(6) 2_666 2_666 ?
O1A Cd2 C1A 27.72(6) 2_666 2_666 ?
O2C Cd2 Cd1 84.25(4) . . ?
O2B Cd2 Cd1 82.98(4) . . ?
O1D Cd2 Cd1 170.70(5) . . ?
O2A Cd2 Cd1 84.41(4) 2_666 . ?
O1A Cd2 Cd1 42.51(3) 2_666 . ?
C1A Cd2 Cd1 62.71(5) 2_666 . ?
C1A O1A Cd1 128.02(13) . . ?
C1A O1A Cd2 85.91(13) . 2_666 ?
Cd1 O1A Cd2 90.26(5) . 2_666 ?
C1A O2A Cd2 96.61(13) . 2_666 ?
O2A C1A O1A 122.3(2) . . ?
O2A C1A C2A 119.17(19) . . ?
O1A C1A C2A 118.4(2) . . ?
O2A C1A Cd2 56.09(11) . 2_666 ?
O1A C1A Cd2 66.37(11) . 2_666 ?
C2A C1A Cd2 172.76(15) . 2_666 ?
C7A C2A C3A 119.9(2) . . ?
C7A C2A C1A 120.2(2) . . ?
C3A C2A C1A 119.8(2) . . ?
C4A C3A C2A 120.2(2) . . ?
C3A C4A C5A 119.1(2) . . ?
C4A C5A C6A 121.0(2) . . ?
C4A C5A N8A 115.8(2) . . ?
C6A C5A N8A 123.1(2) . . ?
C7A C6A C5A 119.2(2) . . ?
C6A C7A C2A 120.4(2) . . ?
N8A N8A C5A 112.5(3) 2_675 . ?
C1B O1B Cd1 127.82(13) . . ?
C1B O2B Cd2 106.49(14) . . ?
O2B C1B O1B 123.2(2) . . ?
O2B C1B C2B 117.7(2) . . ?
O1B C1B C2B 119.1(2) . . ?
C7B C2B C3B 119.6(2) . . ?
C7B C2B C1B 119.9(2) . . ?
C3B C2B C1B 120.5(2) . . ?
C4B C3B C2B 120.3(2) . . ?
C3B C4B C5B 119.2(2) . . ?
C6B C5B C4B 120.8(2) . . ?
C6B C5B N8B 114.9(2) . . ?
C4B C5B N8B 124.3(2) . . ?
C7B C6B C5B 119.4(2) . . ?
C6B C7B C2B 120.6(2) . . ?
N8B N8B C5B 113.8(3) 2_576 . ?
C1C O1C Cd1 132.13(14) . . ?
C1C O2C Cd2 107.33(14) . . ?
O1C C1C O2C 123.9(2) . . ?
O1C C1C C2C 118.6(2) . . ?
O2C C1C C2C 117.5(2) . . ?
C3C C2C C7C 120.0(2) . . ?
C3C C2C C1C 120.4(2) . . ?
C7C C2C C1C 119.6(2) . . ?
C2C C3C C4C 119.8(2) . . ?
C3C C4C C5C 119.5(2) . . ?
C6C C5C C4C 120.9(2) . . ?
C6C C5C N8C 114.9(2) . . ?
C4C C5C N8C 124.3(2) . . ?
C7C C6C C5C 119.2(3) . . ?
C6C C7C C2C 120.5(2) . . ?
N8C N8C C5C 113.3(3) 2_765 . ?
C2D O1D Cd2 129.58(18) . . ?
O1D C2D N3D 123.0(3) . . ?
C2D N3D C5D 121.3(4) . . ?
C2D N3D C4D 120.7(3) . . ?
C5D N3D C4D 118.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        23.29
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.062

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dimethylformamide'
_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 1415514'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{[(mu3-4,4'-azobenzenedicarboxylate-kO:kO':kO'')(mu-3,6-bis(4-pyridyl)-1,2,4,5-tetrazine)zinc(II)]}
_chemical_formula_moiety         'C20 H12 N5 O4 Zn'
_chemical_formula_structural     'C20 H12 N5 O4 Zn'
_chemical_formula_sum            'C20 H12 N5 O4 Zn'
_chemical_formula_weight         451.72
_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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   6.981(1)
_cell_length_b                   26.778(4)
_cell_length_c                   13.660(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.150(5)
_cell_angle_gamma                90.00
_cell_volume                     2527.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5236
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      23.30

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    none
_exptl_crystal_F_000             916
_exptl_absorpt_coefficient_mu    1.001
_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  0.859
_exptl_absorpt_correction_T_max  0.941

# 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 -0.024 0.188 0.569 221.0 26.9
2 -0.075 0.312 0.069 221.0 26.7
3 -0.039 0.688 -0.069 221.0 27.9
4 0.002 0.812 0.431 221.0 27.6
_platon_squeeze_details          
;
;

_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  Xcalibur
_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            5236
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         23.30
_reflns_number_total             2831
_reflns_number_gt                1805
_reflns_threshold_expression     >2sigma(I)

_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     
'calc w=1/[σ²(Fo²)+(0.0840P)²+0.0000P] 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         2831
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0612
_refine_ls_wR_factor_ref         0.1560
_refine_ls_wR_factor_gt          0.1436
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.86657(10) 0.02820(3) 0.89347(5) 0.0294(3) Uani 1 1 d . . .
O1A O 1.0326(7) 0.0855(2) 0.9000(3) 0.0439(15) Uani 1 1 d . . .
O2A O 0.7647(8) 0.1295(3) 0.8881(5) 0.077(2) Uani 1 1 d . . .
C1A C 0.9382(12) 0.1256(4) 0.8898(6) 0.051(3) Uani 1 1 d . . .
C2A C 1.0605(11) 0.1713(4) 0.8796(7) 0.060(3) Uani 1 1 d . . .
C3A C 0.9788(12) 0.2174(4) 0.8526(9) 0.098(4) Uani 1 1 d . . .
H3A H 0.8475 0.2221 0.8548 0.118 Uiso 1 1 calc R . .
C4A C 1.0856(15) 0.2564(5) 0.8226(7) 0.091(3) Uani 1 1 d . . .
H4A H 1.0267 0.2848 0.7932 0.109 Uiso 1 1 calc R . .
C5A C 1.2886(10) 0.2509(4) 0.8387(7) 0.065(3) Uani 1 1 d . . .
C6A C 1.3753(11) 0.2101(4) 0.8772(6) 0.061(3) Uani 1 1 d . . .
H6A H 1.5094 0.2089 0.8917 0.073 Uiso 1 1 calc R . .
C7A C 1.2610(11) 0.1683(4) 0.8961(6) 0.057(3) Uani 1 1 d . . .
H7A H 1.3207 0.1387 0.9196 0.068 Uiso 1 1 calc R . .
N8A N 1.4133(9) 0.2899(3) 0.8117(6) 0.065(2) Uani 1 1 d . . .
N9A N 1.3316(9) 0.3224(3) 0.7553(5) 0.056(2) Uani 1 1 d . . .
C10A C 1.4644(10) 0.3570(4) 0.7228(6) 0.045(2) Uani 1 1 d . . .
C11A C 1.6531(11) 0.3640(4) 0.7644(6) 0.053(3) Uani 1 1 d . . .
H11A H 1.7036 0.3450 0.8190 0.064 Uiso 1 1 calc R . .
C12A C 1.7688(9) 0.3985(3) 0.7269(5) 0.036(2) Uani 1 1 d . . .
H12A H 1.8950 0.4037 0.7573 0.043 Uiso 1 1 calc R . .
C13A C 1.6951(9) 0.4257(3) 0.6426(5) 0.032(2) Uani 1 1 d . . .
C14A C 1.5010(9) 0.4209(3) 0.6018(5) 0.0291(19) Uani 1 1 d . . .
H14A H 1.4482 0.4403 0.5484 0.035 Uiso 1 1 calc R . .
C15A C 1.3875(10) 0.3856(4) 0.6441(5) 0.044(2) Uani 1 1 d . . .
H15A H 1.2580 0.3817 0.6180 0.052 Uiso 1 1 calc R . .
C16A C 1.8174(8) 0.4621(3) 0.5954(5) 0.0263(19) Uani 1 1 d . . .
O3A O 1.9845(6) 0.4704(2) 0.6446(3) 0.0355(13) Uani 1 1 d . . .
O4A O 1.7552(6) 0.48176(19) 0.5152(3) 0.0279(13) Uani 1 1 d . . .
N1B N 0.6375(8) 0.0221(2) 0.7889(4) 0.0330(17) Uani 1 1 d . . .
C2B C 0.6392(9) -0.0081(3) 0.7119(5) 0.039(2) Uani 1 1 d . . .
H2B H 0.7515 -0.0260 0.7066 0.047 Uiso 1 1 calc R . .
C3B C 0.4834(10) -0.0142(3) 0.6402(5) 0.043(2) Uani 1 1 d . . .
H3B H 0.4912 -0.0358 0.5876 0.052 Uiso 1 1 calc R . .
C4B C 0.3159(9) 0.0116(4) 0.6458(5) 0.043(3) Uani 1 1 d . . .
C5B C 0.3123(10) 0.0436(3) 0.7254(5) 0.043(2) Uani 1 1 d . . .
H5B H 0.2022 0.0622 0.7317 0.051 Uiso 1 1 calc R . .
C6B C 0.4755(10) 0.0472(4) 0.7948(5) 0.050(3) Uani 1 1 d . . .
H6B H 0.4720 0.0684 0.8486 0.060 Uiso 1 1 calc R . .
C7B C 0.1428(10) 0.0056(4) 0.5673(6) 0.045(2) Uani 1 1 d . . .
N8B N 0.1664(9) -0.0246(3) 0.4914(5) 0.066(3) Uani 1 1 d . . .
N9B N -0.0117(10) 0.0287(3) 0.5813(5) 0.058(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1A 1.918(6) . ?
Zn1 O4A 1.951(4) 4_466 ?
Zn1 O3A 1.975(5) 2_846 ?
Zn1 N1B 1.994(6) . ?
O1A C1A 1.257(10) . ?
O2A C1A 1.213(9) . ?
C1A C2A 1.509(12) . ?
C2A C3A 1.388(12) . ?
C2A C7A 1.388(10) . ?
C3A C4A 1.378(14) . ?
C4A C5A 1.410(12) . ?
C5A C6A 1.321(11) . ?
C5A N8A 1.440(11) . ?
C6A C7A 1.421(12) . ?
N8A N9A 1.247(9) . ?
N9A C10A 1.426(10) . ?
C10A C15A 1.366(10) . ?
C10A C11A 1.372(10) . ?
C11A C12A 1.373(10) . ?
C12A C13A 1.398(9) . ?
C13A C14A 1.396(9) . ?
C13A C16A 1.500(10) . ?
C14A C15A 1.408(10) . ?
C16A O4A 1.238(8) . ?
C16A O3A 1.280(7) . ?
O3A Zn1 1.975(5) 2_856 ?
O4A Zn1 1.951(4) 4_665 ?
N1B C6B 1.328(9) . ?
N1B C2B 1.329(9) . ?
C2B C3B 1.366(9) . ?
C3B C4B 1.369(10) . ?
C4B C5B 1.388(11) . ?
C4B C7B 1.506(10) . ?
C5B C6B 1.379(10) . ?
C7B N9B 1.281(9) . ?
C7B N8B 1.345(11) . ?
N8B N9B 1.364(9) 3_556 ?
N9B N8B 1.364(9) 3_556 ?

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 O4A 112.38(19) . 4_466 ?
O1A Zn1 O3A 107.6(2) . 2_846 ?
O4A Zn1 O3A 113.9(2) 4_466 2_846 ?
O1A Zn1 N1B 121.1(2) . . ?
O4A Zn1 N1B 102.89(18) 4_466 . ?
O3A Zn1 N1B 98.4(2) 2_846 . ?
C1A O1A Zn1 112.0(5) . . ?
O2A C1A O1A 125.5(8) . . ?
O2A C1A C2A 120.4(9) . . ?
O1A C1A C2A 114.1(7) . . ?
C3A C2A C7A 117.5(8) . . ?
C3A C2A C1A 121.9(8) . . ?
C7A C2A C1A 120.6(8) . . ?
C4A C3A C2A 122.2(8) . . ?
C3A C4A C5A 116.7(11) . . ?
C6A C5A C4A 122.8(9) . . ?
C6A C5A N8A 116.2(7) . . ?
C4A C5A N8A 121.0(9) . . ?
C5A C6A C7A 119.1(8) . . ?
C2A C7A C6A 120.3(9) . . ?
N9A N8A C5A 115.1(7) . . ?
N8A N9A C10A 112.8(7) . . ?
C15A C10A C11A 119.8(7) . . ?
C15A C10A N9A 114.2(7) . . ?
C11A C10A N9A 126.0(8) . . ?
C10A C11A C12A 121.2(7) . . ?
C11A C12A C13A 119.4(7) . . ?
C12A C13A C14A 120.2(6) . . ?
C12A C13A C16A 121.8(6) . . ?
C14A C13A C16A 117.9(6) . . ?
C13A C14A C15A 118.0(7) . . ?
C10A C15A C14A 121.2(6) . . ?
O4A C16A O3A 124.7(6) . . ?
O4A C16A C13A 120.5(6) . . ?
O3A C16A C13A 114.8(6) . . ?
C16A O3A Zn1 118.2(4) . 2_856 ?
C16A O4A Zn1 124.3(4) . 4_665 ?
C6B N1B C2B 117.4(6) . . ?
C6B N1B Zn1 121.2(5) . . ?
C2B N1B Zn1 121.4(5) . . ?
N1B C2B C3B 123.0(7) . . ?
C4B C3B C2B 120.0(7) . . ?
C3B C4B C5B 117.8(7) . . ?
C3B C4B C7B 120.8(8) . . ?
C5B C4B C7B 121.4(7) . . ?
C6B C5B C4B 118.5(7) . . ?
N1B C6B C5B 123.4(7) . . ?
N9B C7B N8B 127.1(8) . . ?
N9B C7B C4B 116.8(8) . . ?
N8B C7B C4B 116.0(7) . . ?
C7B N8B N9B 116.0(7) . 3_556 ?
C7B N9B N8B 116.7(7) . 3_556 ?

_diffrn_measured_fraction_theta_max 0.777
_diffrn_reflns_theta_full        20.00
_diffrn_measured_fraction_theta_full 0.810
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.082

# start Validation Reply Form
_vrf_PLAT027_Compound4           
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............      20.00 Degree
RESPONSE: Single crystals only diffract up to low theta angles given
that the crystal structure contains a high percentage of voids occupied by
disordered solvent molecules.
;
_vrf_PLAT029_Compound4           
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.810 Note  
RESPONSE: Single crystals only diffract up to low theta angles given
that the crystal structure contains a high percentage of voids occupied by
disordered solvent molecules.
;
_vrf_PLAT213_Compound4           
;
PROBLEM: Atom C5A             has ADP max/min Ratio .....        3.2 prolat
RESPONSE: Crystal structure contains a high percentage of voids
occupied by disordered solvent molecules that could not be refined. The
residual electron density placed in the voids, although mainly removed by
the SQUEEZE routine, affects thermal ellipsoids of backbone atoms.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dimethylformamide'
_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_Compound5
_database_code_depnum_ccdc_archive 'CCDC 1415515'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{[tris(mu4-4,4'-azobenzenedicarboxylate-kO:kO':kO'':kO''')bis(mu-3,6-bis(4-pyridyl)-1,2,4,5-tetrazine)trizinc(II)]}
_chemical_formula_moiety         'C60 H36 N14.50 O12 Zn3'
_chemical_formula_structural     'C60 H36 N14.50 O12 Zn3'
_chemical_formula_sum            'C60 H36 N14.50 O12 Zn3'
_chemical_formula_weight         1348.14
_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

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

_cell_length_a                   16.945(5)
_cell_length_b                   16.958(5)
_cell_length_c                   17.880(5)
_cell_angle_alpha                83.348(7)
_cell_angle_beta                 73.542(7)
_cell_angle_gamma                65.791(7)
_cell_volume                     4494(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7052
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      18.89

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.996
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1367
_exptl_absorpt_coefficient_mu    0.844
_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  0.859
_exptl_absorpt_correction_T_max  0.941

# 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 -0.222 -0.089 0.222 2103.7 17.1
_platon_squeeze_details          
;
;

_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  Xcalibur
_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            7052
_diffrn_reflns_av_R_equivalents  0.1364
_diffrn_reflns_av_unetI/netI     0.1494
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         18.89
_reflns_number_total             7052
_reflns_number_gt                3076
_reflns_threshold_expression     >2sigma(I)

_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     
'calc w=1/[σ²(Fo²)+(0.1548P)²+0.0000P] 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         7052
_refine_ls_number_parameters     787
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0916
_refine_ls_wR_factor_ref         0.2653
_refine_ls_wR_factor_gt          0.2381
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_restrained_S_all      0.870
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.12165(11) 0.22831(12) 0.42561(8) 0.0392(6) Uani 1 1 d . . .
Zn2 Zn 0.16250(11) 0.23127(12) 0.25406(8) 0.0398(7) Uani 1 1 d . . .
Zn3 Zn 0.47907(11) -0.00031(12) 0.08542(9) 0.0333(6) Uani 1 1 d . . .
O1A O -0.0060(6) 0.2518(6) 0.4343(5) 0.047(3) Uani 1 1 d . . .
O2A O 0.0345(6) 0.2433(6) 0.3037(5) 0.040(3) Uani 1 1 d . . .
C1A C -0.0233(10) 0.2501(9) 0.3655(8) 0.042(4) Uani 1 1 d . . .
C2A C -0.1087(9) 0.2505(9) 0.3674(8) 0.042(4) Uani 1 1 d . . .
C3A C -0.1783(9) 0.2675(8) 0.4319(8) 0.039(4) Uani 1 1 d . . .
H3A H -0.1713 0.2802 0.4782 0.047 Uiso 1 1 calc R . .
C4A C -0.2579(10) 0.2666(9) 0.4317(9) 0.053(5) Uani 1 1 d . . .
H4A H -0.3050 0.2789 0.4766 0.063 Uiso 1 1 calc R . .
C5A C -0.2665(10) 0.2467(11) 0.3617(9) 0.057(5) Uani 1 1 d D . .
C6A C -0.1986(10) 0.2258(10) 0.2961(9) 0.048(5) Uani 1 1 d . . .
H6A H -0.2047 0.2100 0.2506 0.057 Uiso 1 1 calc R . .
C7A C -0.1216(9) 0.2287(8) 0.2996(7) 0.033(4) Uani 1 1 d . . .
H7A H -0.0744 0.2156 0.2548 0.040 Uiso 1 1 calc R . .
N8A N -0.3561(8) 0.2425(10) 0.3725(6) 0.069(5) Uani 1 1 d D . .
N9A N 0.6410(7) 0.2182(7) 0.3105(7) 0.042(3) Uani 1 1 d D . .
C10A C 0.5533(8) 0.2148(8) 0.3156(8) 0.032(4) Uani 1 1 d D . .
C11A C 0.4862(8) 0.2278(9) 0.3838(8) 0.044(4) Uani 1 1 d . . .
H11A H 0.4939 0.2365 0.4312 0.053 Uiso 1 1 calc R . .
C12A C 0.4090(9) 0.2273(8) 0.3784(8) 0.035(4) Uani 1 1 d . . .
H12A H 0.3622 0.2369 0.4234 0.041 Uiso 1 1 calc R . .
C13A C 0.3956(8) 0.2132(8) 0.3096(7) 0.029(4) Uani 1 1 d . . .
C14A C 0.4628(8) 0.2001(8) 0.2434(7) 0.026(4) Uani 1 1 d . . .
H14A H 0.4540 0.1915 0.1965 0.031 Uiso 1 1 calc R . .
C15A C 0.5421(9) 0.1994(8) 0.2444(8) 0.038(4) Uani 1 1 d . . .
H15A H 0.5886 0.1891 0.1991 0.046 Uiso 1 1 calc R . .
C16A C 0.3097(9) 0.2092(8) 0.3089(8) 0.031(4) Uani 1 1 d . . .
O3A O 0.2520(5) 0.2091(5) 0.3748(5) 0.027(2) Uani 1 1 d . . .
O4A O 0.2902(6) 0.2148(6) 0.2437(5) 0.039(3) Uani 1 1 d . . .
O1B O 0.1537(6) 0.1032(5) 0.4029(4) 0.035(3) Uani 1 1 d . . .
O2B O 0.1966(5) 0.1024(5) 0.2703(4) 0.024(2) Uani 1 1 d . . .
C1B C 0.1753(9) 0.0684(9) 0.3376(9) 0.039(4) Uani 1 1 d . . .
C2B C 0.1769(7) -0.0185(5) 0.3374(6) 0.029(4) Uani 1 1 d G . .
C3B C 0.1284(6) -0.0479(8) 0.4022(5) 0.072(6) Uani 1 1 d G . .
H3B H 0.0957 -0.0128 0.4459 0.087 Uiso 1 1 calc R . .
C4B C 0.1287(7) -0.1300(8) 0.4018(6) 0.105(8) Uani 1 1 d G . .
H4B H 0.0962 -0.1497 0.4452 0.126 Uiso 1 1 calc R . .
C5B C 0.1775(8) -0.1825(6) 0.3365(8) 0.079(6) Uani 1 1 d GD . .
C6B C 0.2260(7) -0.1531(6) 0.2716(6) 0.063(5) Uani 1 1 d G . .
H6B H 0.2586 -0.1883 0.2279 0.075 Uiso 1 1 calc R . .
C7B C 0.2257(6) -0.0711(7) 0.2721(5) 0.068(5) Uani 1 1 d G . .
H7B H 0.2582 -0.0514 0.2287 0.081 Uiso 1 1 calc R . .
N8B N 0.1583(12) -0.2673(10) 0.3632(11) 0.131(7) Uani 1 1 d D . .
N9B N 0.1826(12) 0.7012(10) 0.3060(11) 0.120(6) Uani 1 1 d D . .
C10B C 0.1558(8) 0.6227(6) 0.3378(8) 0.084(6) Uani 1 1 d GD . .
C11B C 0.1250(8) 0.5892(7) 0.4094(6) 0.121(8) Uani 1 1 d G . .
H11B H 0.1124 0.6181 0.4552 0.145 Uiso 1 1 calc R . .
C12B C 0.1130(7) 0.5124(7) 0.4125(5) 0.071(5) Uani 1 1 d G . .
H12B H 0.0924 0.4900 0.4605 0.085 Uiso 1 1 calc R . .
C13B C 0.1318(6) 0.4692(5) 0.3441(6) 0.043(4) Uani 1 1 d G . .
C14B C 0.1626(6) 0.5028(7) 0.2725(5) 0.049(4) Uani 1 1 d G . .
H14B H 0.1752 0.4739 0.2266 0.059 Uiso 1 1 calc R . .
C15B C 0.1746(7) 0.5795(7) 0.2693(6) 0.098(7) Uani 1 1 d G . .
H15B H 0.1953 0.6020 0.2214 0.117 Uiso 1 1 calc R . .
C16B C 0.1131(10) 0.3869(10) 0.3482(11) 0.047(4) Uani 1 1 d . . .
O3B O 0.0949(6) 0.3550(6) 0.4141(5) 0.048(3) Uani 1 1 d . . .
O4B O 0.1274(6) 0.3570(6) 0.2791(5) 0.050(3) Uani 1 1 d . . .
N1C N 0.1348(7) 0.2118(6) 0.5375(6) 0.030(3) Uani 1 1 d . . .
C2C C 0.0626(8) 0.2282(8) 0.5938(7) 0.022(3) Uani 1 1 d . . .
H2C H 0.0086 0.2397 0.5826 0.027 Uiso 1 1 calc R . .
C3C C 0.0651(9) 0.2289(9) 0.6716(8) 0.043(4) Uani 1 1 d . . .
H3C H 0.0120 0.2448 0.7111 0.051 Uiso 1 1 calc R . .
C4C C 0.1402(9) 0.2079(9) 0.6890(8) 0.034(4) Uani 1 1 d . . .
C5C C 0.2184(9) 0.1863(9) 0.6262(8) 0.049(5) Uani 1 1 d . . .
H5C H 0.2742 0.1687 0.6360 0.058 Uiso 1 1 calc R . .
C6C C 0.2122(9) 0.1913(8) 0.5510(7) 0.027(4) Uani 1 1 d . . .
H6C H 0.2633 0.1800 0.5098 0.032 Uiso 1 1 calc R . .
C7C C 0.1495(10) 0.2039(9) 0.7695(8) 0.046(4) Uani 1 1 d . . .
N8C N 0.0737(9) 0.2119(9) 0.8260(8) 0.072(4) Uani 1 1 d . . .
N9C N 0.0810(9) 0.2177(8) -0.1014(8) 0.069(4) Uani 1 1 d . . .
C10C C 0.1518(10) 0.2213(9) -0.0907(8) 0.041(4) Uani 1 1 d . . .
N11C N 0.2265(9) 0.2114(9) -0.1457(8) 0.074(4) Uani 1 1 d . . .
N12C N 0.2229(9) 0.1998(8) 0.7801(7) 0.066(4) Uani 1 1 d . . .
C13C C 0.1569(9) 0.2342(8) -0.0112(7) 0.030(4) Uani 1 1 d . . .
C14C C 0.0765(10) 0.2573(9) 0.0470(8) 0.048(4) Uani 1 1 d . . .
H14C H 0.0225 0.2697 0.0355 0.058 Uiso 1 1 calc R . .
C15C C 0.0806(9) 0.2612(8) 0.1251(7) 0.034(4) Uani 1 1 d . . .
H15C H 0.0282 0.2782 0.1653 0.041 Uiso 1 1 calc R . .
N16C N 0.1577(7) 0.2408(6) 0.1405(6) 0.027(3) Uani 1 1 d . . .
C17C C 0.2258(8) 0.2227(7) 0.0853(6) 0.013(3) Uani 1 1 d . . .
H17C H 0.2789 0.2120 0.0978 0.015 Uiso 1 1 calc R . .
C18C C 0.2321(8) 0.2164(8) 0.0089(7) 0.026(4) Uani 1 1 d . . .
H18C H 0.2871 0.2003 -0.0281 0.032 Uiso 1 1 calc R . .
O1D O 0.3524(5) 0.0135(5) 0.0951(5) 0.031(2) Uani 1 1 d . . .
O2D O 0.3922(6) 0.0119(6) -0.0337(5) 0.041(3) Uani 1 1 d . . .
C1D C 0.3357(9) 0.0123(8) 0.0323(8) 0.031(4) Uani 1 1 d . . .
C2D C 0.2502(8) 0.0128(8) 0.0296(7) 0.020(3) Uani 1 1 d . . .
C3D C 0.1779(8) 0.0352(8) 0.0966(7) 0.029(4) Uani 1 1 d . . .
H3D H 0.1844 0.0495 0.1425 0.035 Uiso 1 1 calc R . .
C4D C 0.0996(9) 0.0358(8) 0.0938(7) 0.032(4) Uani 1 1 d . . .
H4D H 0.0514 0.0508 0.1379 0.039 Uiso 1 1 calc R . .
C5D C 0.0899(9) 0.0140(9) 0.0247(8) 0.044(4) Uani 1 1 d D . .
C6D C 0.1564(9) -0.0091(10) -0.0430(7) 0.046(5) Uani 1 1 d . . .
H6D H 0.1484 -0.0236 -0.0881 0.055 Uiso 1 1 calc R . .
C7D C 0.2383(9) -0.0091(8) -0.0385(8) 0.038(4) Uani 1 1 d . . .
H7D H 0.2865 -0.0242 -0.0827 0.045 Uiso 1 1 calc R . .
N8D N 0.0008(8) 0.0138(8) 0.0298(6) 0.053(4) Uani 1 1 d D . .
O1E O 0.4458(5) 0.1279(5) 0.0674(4) 0.029(2) Uani 1 1 d . . .
O2E O 0.4877(5) 0.1254(6) -0.0652(4) 0.036(3) Uani 1 1 d . . .
C1E C 0.4645(9) 0.1615(9) 0.0013(9) 0.031(4) Uani 1 1 d . . .
C2E C 0.4584(10) 0.2523(10) 0.0018(9) 0.046(4) Uani 1 1 d . . .
C3E C 0.5153(13) 0.2724(13) -0.0617(11) 0.103(7) Uani 1 1 d . . .
H3E H 0.5479 0.2349 -0.1039 0.123 Uiso 1 1 calc R . .
C4E C 0.5226(13) 0.3612(13) -0.0597(12) 0.099(7) Uani 1 1 d . . .
H4E H 0.5552 0.3805 -0.1033 0.119 Uiso 1 1 calc R . .
C5E C 0.4793(15) 0.4122(13) 0.0092(13) 0.112(7) Uani 1 1 d D . .
C6E C 0.4194(14) 0.3810(14) 0.0654(12) 0.111(7) Uani 1 1 d . . .
H6E H 0.3781 0.4186 0.1054 0.133 Uiso 1 1 calc R . .
C7E C 0.4172(9) 0.3011(10) 0.0657(8) 0.047(4) Uani 1 1 d . . .
H7E H 0.3869 0.2811 0.1104 0.056 Uiso 1 1 calc R . .
N8E N 0.4733(11) 0.5021(12) 0.0214(10) 0.015(5) Uani 0.50 1 d PD . .
N1F N 0.4847(7) -0.0071(6) 0.1980(6) 0.028(3) Uani 1 1 d . . .
C2F C 0.4169(9) 0.0089(8) 0.2547(7) 0.026(4) Uani 1 1 d . . .
H2F H 0.3632 0.0206 0.2429 0.031 Uiso 1 1 calc R . .
C3F C 0.4127(9) 0.0111(8) 0.3320(7) 0.032(4) Uani 1 1 d . . .
H3F H 0.3595 0.0228 0.3708 0.038 Uiso 1 1 calc R . .
C4F C 0.4912(8) -0.0050(8) 0.3482(6) 0.025(4) Uani 1 1 d . . .
C5F C 0.5694(9) -0.0274(8) 0.2893(7) 0.035(4) Uani 1 1 d . . .
H5F H 0.6247 -0.0426 0.2996 0.042 Uiso 1 1 calc R . .
C6F C 0.5619(8) -0.0263(8) 0.2144(7) 0.022(4) Uani 1 1 d . . .
H6F H 0.6135 -0.0396 0.1735 0.027 Uiso 1 1 calc R . .
C7F C 0.4982(8) -0.0029(8) 0.4309(7) 0.021(4) Uani 1 1 d . . .
N8F N 0.4220(7) 0.0076(7) 0.4855(6) 0.039(3) Uani 1 1 d . . .
N9F N 0.5732(7) -0.0089(7) 0.4396(6) 0.033(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1A 1.994(9) . ?
Zn1 O3B 2.004(9) . ?
Zn1 O1B 2.023(8) . ?
Zn1 O3A 2.037(8) . ?
Zn1 N1C 2.050(10) . ?
Zn1 Zn2 2.946(2) . ?
Zn2 O4A 2.020(8) . ?
Zn2 O2B 2.027(8) . ?
Zn2 O2A 2.031(9) . ?
Zn2 O4B 2.032(9) . ?
Zn2 N16C 2.039(10) . ?
Zn3 O2E 2.007(9) 2_655 ?
Zn3 O1D 2.020(8) . ?
Zn3 O1E 2.020(9) . ?
Zn3 N1F 2.029(10) . ?
Zn3 O2D 2.049(9) 2_655 ?
Zn3 Zn3 2.934(3) 2_655 ?
O1A C1A 1.350(14) . ?
O2A C1A 1.231(14) . ?
C1A C2A 1.435(17) . ?
C2A C3A 1.354(16) . ?
C2A C7A 1.405(16) . ?
C3A C4A 1.356(16) . ?
C4A C5A 1.395(17) . ?
C5A C6A 1.350(17) . ?
C5A N8A 1.504(12) . ?
C6A C7A 1.345(16) . ?
N8A N9A 1.246(13) 1_455 ?
N9A N8A 1.246(13) 1_655 ?
N9A C10A 1.488(12) . ?
C10A C11A 1.379(16) . ?
C10A C15A 1.407(16) . ?
C11A C12A 1.342(15) . ?
C12A C13A 1.376(15) . ?
C13A C14A 1.356(15) . ?
C13A C16A 1.489(16) . ?
C14A C15A 1.345(15) . ?
C16A O4A 1.282(13) . ?
C16A O3A 1.301(13) . ?
O1B C1B 1.260(15) . ?
O2B C1B 1.295(14) . ?
C1B C2B 1.462(15) . ?
C2B C3B 1.3900 . ?
C2B C7B 1.3900 . ?
C3B C4B 1.3900 . ?
C4B C5B 1.3900 . ?
C5B C6B 1.3900 . ?
C5B N8B 1.592(12) . ?
C6B C7B 1.3900 . ?
N8B N9B 1.10(2) 1_545 ?
N9B N8B 1.10(2) 1_565 ?
N9B C10B 1.573(12) . ?
C10B C11B 1.3900 . ?
C10B C15B 1.3900 . ?
C11B C12B 1.3900 . ?
C12B C13B 1.3900 . ?
C13B C14B 1.3900 . ?
C13B C16B 1.543(16) . ?
C14B C15B 1.3900 . ?
C16B O3B 1.249(16) . ?
C16B O4B 1.310(16) . ?
N1C C2C 1.294(13) . ?
N1C C6C 1.298(13) . ?
C2C C3C 1.406(16) . ?
C3C C4C 1.292(15) . ?
C4C C5C 1.417(17) . ?
C4C C7C 1.483(18) . ?
C5C C6C 1.367(16) . ?
C7C N12C 1.284(15) . ?
C7C N8C 1.357(17) . ?
N8C N9C 1.357(15) 1_556 ?
N9C C10C 1.293(15) . ?
N9C N8C 1.357(15) 1_554 ?
C10C N11C 1.325(16) . ?
C10C C13C 1.495(17) . ?
N11C N12C 1.384(15) 1_554 ?
N12C N11C 1.384(15) 1_556 ?
C13C C18C 1.329(15) . ?
C13C C14C 1.394(16) . ?
C14C C15C 1.428(16) . ?
C15C N16C 1.308(13) . ?
N16C C17C 1.240(12) . ?
C17C C18C 1.352(14) . ?
O1D C1D 1.236(13) . ?
O2D C1D 1.291(13) . ?
O2D Zn3 2.049(9) 2_655 ?
C1D C2D 1.460(15) . ?
C2D C7D 1.402(15) . ?
C2D C3D 1.406(15) . ?
C3D C4D 1.338(15) . ?
C4D C5D 1.400(16) . ?
C5D C6D 1.366(17) . ?
C5D N8D 1.488(12) . ?
C6D C7D 1.413(16) . ?
N8D N8D 1.225(18) 2 ?
O1E C1E 1.266(15) . ?
O2E C1E 1.285(15) . ?
O2E Zn3 2.007(9) 2_655 ?
C1E C2E 1.502(18) . ?
C2E C7E 1.330(17) . ?
C2E C3E 1.38(2) . ?
C3E C4E 1.57(2) . ?
C4E C5E 1.42(2) . ?
C5E C6E 1.44(2) . ?
C5E N8E 1.524(15) . ?
C5E N8E 1.89(3) 2_665 ?
C6E C7E 1.37(2) . ?
N8E N8E 0.99(3) 2_665 ?
N8E C5E 1.89(3) 2_665 ?
N1F C2F 1.252(13) . ?
N1F C6F 1.324(13) . ?
C2F C3F 1.368(15) . ?
C3F C4F 1.352(15) . ?
C4F C5F 1.378(16) . ?
C4F C7F 1.523(15) . ?
C5F C6F 1.377(15) . ?
C7F N9F 1.286(13) . ?
C7F N8F 1.337(14) . ?
N8F N9F 1.367(13) 2_656 ?
N9F N8F 1.367(13) 2_656 ?

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 O3B 90.5(4) . . ?
O1A Zn1 O1B 88.5(4) . . ?
O3B Zn1 O1B 163.1(3) . . ?
O1A Zn1 O3A 158.9(3) . . ?
O3B Zn1 O3A 86.3(4) . . ?
O1B Zn1 O3A 88.5(3) . . ?
O1A Zn1 N1C 106.0(4) . . ?
O3B Zn1 N1C 98.8(4) . . ?
O1B Zn1 N1C 97.6(4) . . ?
O3A Zn1 N1C 95.1(4) . . ?
O1A Zn1 Zn2 91.2(3) . . ?
O3B Zn1 Zn2 84.0(3) . . ?
O1B Zn1 Zn2 79.1(2) . . ?
O3A Zn1 Zn2 67.8(2) . . ?
N1C Zn1 Zn2 162.5(3) . . ?
O4A Zn2 O2B 90.2(3) . . ?
O4A Zn2 O2A 160.2(3) . . ?
O2B Zn2 O2A 85.8(3) . . ?
O4A Zn2 O4B 86.6(4) . . ?
O2B Zn2 O4B 159.3(3) . . ?
O2A Zn2 O4B 90.3(4) . . ?
O4A Zn2 N16C 102.2(4) . . ?
O2B Zn2 N16C 99.7(4) . . ?
O2A Zn2 N16C 97.6(4) . . ?
O4B Zn2 N16C 100.9(4) . . ?
O4A Zn2 Zn1 91.9(2) . . ?
O2B Zn2 Zn1 81.6(2) . . ?
O2A Zn2 Zn1 68.3(2) . . ?
O4B Zn2 Zn1 78.1(3) . . ?
N16C Zn2 Zn1 165.8(3) . . ?
O2E Zn3 O1D 85.1(3) 2_655 . ?
O2E Zn3 O1E 160.6(3) 2_655 . ?
O1D Zn3 O1E 91.4(3) . . ?
O2E Zn3 N1F 100.1(4) 2_655 . ?
O1D Zn3 N1F 103.3(4) . . ?
O1E Zn3 N1F 99.2(4) . . ?
O2E Zn3 O2D 91.4(3) 2_655 2_655 ?
O1D Zn3 O2D 159.0(3) . 2_655 ?
O1E Zn3 O2D 85.1(3) . 2_655 ?
N1F Zn3 O2D 97.7(4) . 2_655 ?
O2E Zn3 Zn3 79.7(2) 2_655 2_655 ?
O1D Zn3 Zn3 91.7(2) . 2_655 ?
O1E Zn3 Zn3 81.4(2) . 2_655 ?
N1F Zn3 Zn3 165.0(3) . 2_655 ?
O2D Zn3 Zn3 67.3(2) 2_655 2_655 ?
C1A O1A Zn1 113.9(8) . . ?
C1A O2A Zn2 145.3(9) . . ?
O2A C1A O1A 120.7(12) . . ?
O2A C1A C2A 121.5(12) . . ?
O1A C1A C2A 117.7(12) . . ?
C3A C2A C7A 116.5(13) . . ?
C3A C2A C1A 124.2(13) . . ?
C7A C2A C1A 119.2(13) . . ?
C4A C3A C2A 122.6(14) . . ?
C3A C4A C5A 117.6(14) . . ?
C6A C5A C4A 122.7(13) . . ?
C6A C5A N8A 126.0(12) . . ?
C4A C5A N8A 111.0(13) . . ?
C7A C6A C5A 116.9(13) . . ?
C6A C7A C2A 123.6(13) . . ?
N9A N8A C5A 109.3(10) 1_455 . ?
N8A N9A C10A 112.7(10) 1_655 . ?
C11A C10A C15A 121.5(11) . . ?
C11A C10A N9A 123.6(11) . . ?
C15A C10A N9A 114.9(11) . . ?
C12A C11A C10A 116.6(12) . . ?
C11A C12A C13A 123.3(13) . . ?
C14A C13A C12A 119.0(12) . . ?
C14A C13A C16A 120.8(11) . . ?
C12A C13A C16A 120.2(12) . . ?
C15A C14A C13A 121.1(12) . . ?
C14A C15A C10A 118.5(12) . . ?
O4A C16A O3A 121.1(11) . . ?
O4A C16A C13A 119.3(12) . . ?
O3A C16A C13A 119.2(11) . . ?
C16A O3A Zn1 144.5(8) . . ?
C16A O4A Zn2 114.3(8) . . ?
C1B O1B Zn1 128.0(9) . . ?
C1B O2B Zn2 123.0(8) . . ?
O1B C1B O2B 125.9(13) . . ?
O1B C1B C2B 117.4(12) . . ?
O2B C1B C2B 116.7(12) . . ?
C3B C2B C7B 120.0 . . ?
C3B C2B C1B 119.8(10) . . ?
C7B C2B C1B 120.2(10) . . ?
C2B C3B C4B 120.0 . . ?
C5B C4B C3B 120.0 . . ?
C4B C5B C6B 120.0 . . ?
C4B C5B N8B 101.8(12) . . ?
C6B C5B N8B 138.2(12) . . ?
C5B C6B C7B 120.0 . . ?
C6B C7B C2B 120.0 . . ?
N9B N8B C5B 98.7(14) 1_545 . ?
N8B N9B C10B 94.6(14) 1_565 . ?
C11B C10B C15B 120.0 . . ?
C11B C10B N9B 138.2(11) . . ?
C15B C10B N9B 101.8(11) . . ?
C10B C11B C12B 120.0 . . ?
C13B C12B C11B 120.0 . . ?
C14B C13B C12B 120.0 . . ?
C14B C13B C16B 120.5(10) . . ?
C12B C13B C16B 119.4(10) . . ?
C15B C14B C13B 120.0 . . ?
C14B C15B C10B 120.0 . . ?
O3B C16B O4B 129.9(14) . . ?
O3B C16B C13B 117.1(13) . . ?
O4B C16B C13B 112.7(13) . . ?
C16B O3B Zn1 120.3(9) . . ?
C16B O4B Zn2 125.2(9) . . ?
C2C N1C C6C 121.4(11) . . ?
C2C N1C Zn1 117.6(8) . . ?
C6C N1C Zn1 120.8(9) . . ?
N1C C2C C3C 120.6(12) . . ?
C4C C3C C2C 120.8(13) . . ?
C3C C4C C5C 116.9(13) . . ?
C3C C4C C7C 124.5(14) . . ?
C5C C4C C7C 118.6(12) . . ?
C6C C5C C4C 120.3(12) . . ?
N1C C6C C5C 119.8(12) . . ?
N12C C7C N8C 126.2(14) . . ?
N12C C7C C4C 119.5(14) . . ?
N8C C7C C4C 114.1(13) . . ?
N9C N8C C7C 112.9(13) 1_556 . ?
C10C N9C N8C 121.4(13) . 1_554 ?
N9C C10C N11C 125.3(14) . . ?
N9C C10C C13C 121.2(13) . . ?
N11C C10C C13C 113.5(13) . . ?
C10C N11C N12C 114.3(13) . 1_554 ?
C7C N12C N11C 119.5(13) . 1_556 ?
C18C C13C C14C 118.7(12) . . ?
C18C C13C C10C 125.0(12) . . ?
C14C C13C C10C 115.8(12) . . ?
C13C C14C C15C 117.3(12) . . ?
N16C C15C C14C 120.4(12) . . ?
C17C N16C C15C 118.2(11) . . ?
C17C N16C Zn2 122.6(8) . . ?
C15C N16C Zn2 119.0(9) . . ?
N16C C17C C18C 127.8(12) . . ?
C13C C18C C17C 117.5(12) . . ?
C1D O1D Zn3 114.5(8) . . ?
C1D O2D Zn3 144.2(8) . 2_655 ?
O1D C1D O2D 121.8(12) . . ?
O1D C1D C2D 121.3(12) . . ?
O2D C1D C2D 116.9(11) . . ?
C7D C2D C3D 118.8(11) . . ?
C7D C2D C1D 121.6(11) . . ?
C3D C2D C1D 119.6(11) . . ?
C4D C3D C2D 119.4(12) . . ?
C3D C4D C5D 120.3(12) . . ?
C6D C5D C4D 124.4(12) . . ?
C6D C5D N8D 120.3(12) . . ?
C4D C5D N8D 115.2(12) . . ?
C5D C6D C7D 114.2(12) . . ?
C2D C7D C6D 122.9(12) . . ?
N8D N8D C5D 112.1(14) 2 . ?
C1E O1E Zn3 124.1(8) . . ?
C1E O2E Zn3 127.1(9) . 2_655 ?
O1E C1E O2E 126.2(13) . . ?
O1E C1E C2E 116.1(13) . . ?
O2E C1E C2E 117.7(13) . . ?
C7E C2E C3E 122.6(16) . . ?
C7E C2E C1E 121.7(15) . . ?
C3E C2E C1E 114.1(15) . . ?
C2E C3E C4E 116.9(17) . . ?
C5E C4E C3E 119.6(18) . . ?
C4E C5E C6E 112.7(18) . . ?
C4E C5E N8E 127.7(19) . . ?
C6E C5E N8E 118.0(19) . . ?
C4E C5E N8E 98.3(16) . 2_665 ?
C6E C5E N8E 148.9(19) . 2_665 ?
N8E C5E N8E 31.3(11) . 2_665 ?
C7E C6E C5E 126(2) . . ?
C2E C7E C6E 119.8(16) . . ?
N8E N8E C5E 95(2) 2_665 . ?
N8E N8E C5E 53.3(16) 2_665 2_665 ?
C5E N8E C5E 148.7(11) . 2_665 ?
C2F N1F C6F 116.6(11) . . ?
C2F N1F Zn3 123.1(9) . . ?
C6F N1F Zn3 120.3(9) . . ?
N1F C2F C3F 127.6(13) . . ?
C4F C3F C2F 115.5(12) . . ?
C3F C4F C5F 120.2(11) . . ?
C3F C4F C7F 122.4(11) . . ?
C5F C4F C7F 117.4(11) . . ?
C6F C5F C4F 116.8(12) . . ?
N1F C6F C5F 123.1(12) . . ?
N9F C7F N8F 128.7(11) . . ?
N9F C7F C4F 117.7(11) . . ?
N8F C7F C4F 113.6(11) . . ?
C7F N8F N9F 114.7(10) . 2_656 ?
C7F N9F N8F 116.6(10) . 2_656 ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        18.89
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.111

# start Validation Reply Form
_vrf_THETM01_Compound5           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Single crystals only diffract up to low theta angles given that
the crystal structure contains a high percentage of voids occupied by 
disordered solvent molecules.
;
_vrf_PLAT213_Compound5           
;
PROBLEM: Atom N8A             has ADP max/min Ratio .....        5.7 prolat
RESPONSE: Crystal structure contains a high percentage of voids occupied by 
disordered solvent molecules that could not be refined. The residual electron 
density placed in the voids, although mainly removed by the SQUEEZE routine, 
affects thermal ellipsoids of backbone atoms.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dimethylformamide'
_exptl_crystal_preparation       Luminescent
