# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_1-Zn
_database_code_depnum_ccdc_archive 'CCDC 2061897'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPVEHU)
Spain
;
_audit_update_record             
;
2021-05-21 deposited with the CCDC.	2021-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
Poly[(mu4-1,4-benzenedicarboxylato-kO:kO':kO'':kO''')(mu-3,6-bis(4-pyridyl)-1,2,4,5-tetrazine)bis(dimethylformamide)bis(nitrato-k2O,O')dizinc(II)]
_chemical_formula_moiety         'C13 H13 N5 O6 Zn'
_chemical_formula_structural     'C13 H13 N5 O6 Zn'
_chemical_formula_sum            'C13 H13 N5 O6 Zn'
_chemical_formula_weight         400.66
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

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

_cell_length_a                   15.0270(5)
_cell_length_b                   10.4796(3)
_cell_length_c                   9.4372(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.705(3)
_cell_angle_gamma                90
_cell_volume                     1485.48(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5690
_cell_measurement_theta_min      4.688
_cell_measurement_theta_max      74.727

_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_colour            'light red'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    none
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    2.735
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_T_max  0.744


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_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            5690
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.688
_diffrn_reflns_theta_max         74.727
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1587
_reflns_number_gt                1453
_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 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0450P)²+2.8259P] 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         1587
_refine_ls_number_parameters     132
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   1.474
_refine_ls_restrained_S_all      1.511
_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 0.62042(3) 0.500000 0.43912(6) 0.0195(2) Uani 1 2 d S T P A .
O1A O 0.57478(13) 0.3314(2) 0.5108(2) 0.0247(5) Uani 1 1 d . . . . .
C1A C 0.500000 0.2768(4) 0.500000 0.0200(8) Uani 1 2 d S T P . .
C2A C 0.500000 0.1331(4) 0.500000 0.0194(8) Uani 1 2 d S T P . .
C3A C 0.43394(18) 0.0665(3) 0.4245(3) 0.0208(6) Uani 1 1 d . . . . .
H3A H 0.389752 0.110810 0.373979 0.025 Uiso 1 1 calc R U . . .
N1B N 0.7250(2) 0.500000 0.5941(4) 0.0197(7) Uani 1 2 d S T P . .
C2B C 0.7606(2) 0.6096(3) 0.6427(3) 0.0252(6) Uani 1 1 d . . . . .
H2B H 0.737106 0.686226 0.608910 0.030 Uiso 1 1 calc R U . . .
C3B C 0.8310(2) 0.6136(3) 0.7413(3) 0.0268(7) Uani 1 1 d . . . . .
H3B H 0.853938 0.691259 0.772884 0.032 Uiso 1 1 calc R U . . .
C4B C 0.8662(3) 0.500000 0.7916(5) 0.0241(9) Uani 1 2 d S T P . .
C5B C 0.9390(3) 0.500000 0.9030(5) 0.0256(9) Uani 1 2 d S T P . .
N6B N 0.9685(2) 0.6129(3) 0.9494(3) 0.0347(7) Uani 1 1 d . . . . .
N1N N 0.7447(2) 0.500000 0.2386(4) 0.0260(8) Uani 1 2 d S T P . .
O1N O 0.71493(17) 0.6018(2) 0.2902(3) 0.0359(6) Uani 1 1 d . . . . .
O2N O 0.7996(3) 0.500000 0.1458(4) 0.0487(11) Uani 1 2 d S T P . .
O1D O 0.5321(3) 0.500000 0.2677(5) 0.0551(11) Uani 1 2 d S TU P . .
C2D C 0.4828(4) 0.4451(7) 0.2073(6) 0.0263(12) Uani 0.5 1 d . . P A -1
H2D H 0.485026 0.356581 0.213577 0.032 Uiso 0.5 1 calc R U P A -1
N3D N 0.4162(3) 0.500000 0.1209(5) 0.0580(18) Uani 1 2 d S T P . .
C4D C 0.3788(5) 0.3840(6) 0.0689(7) 0.083(2) Uani 1 1 d . . . . .
H4D1 H 0.405926 0.313349 0.118421 0.124 Uiso 1 1 calc R U . . .
H4D2 H 0.389297 0.376466 -0.030629 0.124 Uiso 1 1 calc R U . . .
H4D3 H 0.315851 0.383741 0.083638 0.124 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 2.019(2) 6_565 ?
Zn1 O1A 2.019(2) . ?
Zn1 O1D 2.062(5) . ?
Zn1 N1B 2.115(3) . ?
Zn1 O1N 2.291(3) . ?
Zn1 O1N 2.291(3) 6_565 ?
O1A C1A 1.262(3) . ?
C1A C2A 1.506(6) . ?
C2A C3A 1.392(3) . ?
C2A C3A 1.392(3) 2_656 ?
C3A C3A 1.394(6) 6 ?
N1B C2B 1.342(4) 6_565 ?
N1B C2B 1.342(4) . ?
C2B C3B 1.388(4) . ?
C3B C4B 1.381(4) . ?
C4B C5B 1.495(6) . ?
C5B N6B 1.333(3) . ?
C5B N6B 1.333(3) 6_565 ?
N6B N6B 1.324(5) 2_757 ?
N1N O2N 1.221(6) . ?
N1N O1N 1.260(3) . ?
N1N O1N 1.260(3) 6_565 ?
O1D C2D 1.086(7) . ?
C2D N3D 1.396(7) . ?
N3D C4D 1.421(8) 6_565 ?
N3D C4D 1.421(8) . ?

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 O1A 122.11(13) 6_565 . ?
O1A Zn1 O1D 92.61(9) 6_565 . ?
O1A Zn1 O1D 92.61(9) . . ?
O1A Zn1 N1B 91.22(8) 6_565 . ?
O1A Zn1 N1B 91.22(8) . . ?
O1D Zn1 N1B 172.08(17) . . ?
O1A Zn1 O1N 91.20(9) 6_565 . ?
O1A Zn1 O1N 146.69(9) . . ?
O1D Zn1 O1N 85.12(14) . . ?
N1B Zn1 O1N 87.87(11) . . ?
O1A Zn1 O1N 146.69(9) 6_565 6_565 ?
O1A Zn1 O1N 91.20(9) . 6_565 ?
O1D Zn1 O1N 85.12(13) . 6_565 ?
N1B Zn1 O1N 87.87(11) . 6_565 ?
O1N Zn1 O1N 55.49(13) . 6_565 ?
C1A O1A Zn1 132.8(2) . . ?
O1A C1A O1A 126.1(4) . 2_656 ?
O1A C1A C2A 116.9(2) . . ?
O1A C1A C2A 116.9(2) 2_656 . ?
C3A C2A C3A 119.8(4) . 2_656 ?
C3A C2A C1A 120.1(2) . . ?
C3A C2A C1A 120.1(2) 2_656 . ?
C3A C3A C2A 120.1(2) 6 . ?
C2B N1B C2B 117.7(4) 6_565 . ?
C2B N1B Zn1 121.13(18) 6_565 . ?
C2B N1B Zn1 121.13(18) . . ?
N1B C2B C3B 122.9(3) . . ?
C4B C3B C2B 118.8(3) . . ?
C3B C4B C3B 119.0(4) . 6_565 ?
C3B C4B C5B 120.5(2) . . ?
C3B C4B C5B 120.5(2) 6_565 . ?
N6B C5B N6B 125.2(4) . 6_565 ?
N6B C5B C4B 117.4(2) . . ?
N6B C5B C4B 117.4(2) 6_565 . ?
N6B N6B C5B 117.4(2) 2_757 . ?
O2N N1N O1N 122.17(19) . . ?
O2N N1N O1N 122.17(19) . 6_565 ?
O1N N1N O1N 115.7(4) . 6_565 ?
N1N O1N Zn1 94.4(2) . . ?
C2D O1D Zn1 145.6(4) . . ?
O1D C2D N3D 123.6(6) . . ?
C2D N3D C4D 145.5(5) . 6_565 ?
C2D N3D C4D 96.8(4) . . ?
C4D N3D C4D 117.7(6) 6_565 . ?

_refine_diff_density_max         1.900
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.098



_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_2-Cd
_database_code_depnum_ccdc_archive 'CCDC 2061898'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPVEHU)
Spain
;
_audit_update_record             
;
2021-05-21 deposited with the CCDC.	2021-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[(mu3-1,4-benzenedicarboxylato-k2O,O':k2O'',O''':kO'')(mu-3,6-bis(4-pyridyl)-1,2,4,5-tetrazine)cadmium(II)] dimethylformamide}"
_chemical_formula_moiety         'C20 H12 Cd N6 O4, (C3 H7 N O)'
_chemical_formula_structural     'C20 H12 Cd N6 O4, (C3 H7 N O)'
_chemical_formula_sum            'C23 H19 Cd N7 O5'
_chemical_formula_weight         585.85
_chemical_compound_source        'synthesis as described'


_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'

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

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

_cell_length_a                   14.1969(6)
_cell_length_b                   15.7861(7)
_cell_length_c                   21.0190(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4710.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19080
_cell_measurement_theta_min      1.289
_cell_measurement_theta_max      23.383

# SQUEEZE RESULTS (Version = 130220)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.009 0.500 0.000 446 119 ' '
2 -0.012 0.500 0.500 446 119 ' '
3 0.007 0.000 0.500 215 39 ' '
4 0.007 0.000 1.000 215 39 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL mo_AC2200R_0m in P2/c                  New:Pcca
CELL   14.1969   15.7861   21.0190     90.00     90.00     90.00
SPGR Pcca
# Solvent Accessible Volume =      1327
# Electrons Found in S.A.V. =       315
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
Q101 0.394 0.732 0.189 !       4.16 eA-3
Q102 0.312 0.611 0.825 !       2.56 eA-3
Q103 0.312 0.392 0.300 !       2.53 eA-3
Q104 0.312 0.234 0.313 !       2.29 eA-3
Q105 0.904 0.690 0.306 !       2.17 eA-3
Q106 0.313 0.173 0.310 !       2.04 eA-3
C107 0.734 0.579 0.020 !       1.79 eA-3
C108 0.379 0.492 0.474 !       1.78 eA-3
C109 0.379 0.492 0.995 !       1.78 eA-3
Q110 0.062 0.418 0.017 !       1.74 eA-3
C111 0.750 0.999 0.109 !       1.74 eA-3
C112 0.439 0.580 0.483 !       1.64 eA-3
Q113 0.298 0.226 0.857 !       1.63 eA-3
C114 0.374 0.456 0.971 !       1.60 eA-3
C115 0.204 0.391 0.987 !       1.56 eA-3
Q116 0.907 0.232 0.067 !       1.55 eA-3
C117 0.169 0.581 0.451 !       1.55 eA-3
Q118 0.184 0.346 0.623 !       1.47 eA-3
C119 0.624 0.391 0.531 !       1.44 eA-3
Q120 0.106 0.841 0.692 !       1.44 eA-3
C121 0.201 0.487 0.488 !       1.44 eA-3
Q122 0.251 0.583 0.339 !       1.42 eA-3
C123 0.170 0.523 0.452 !       1.41 eA-3
Q124 0.810 0.654 0.447 !       1.40 eA-3
Q125 0.292 0.652 0.276 !       1.38 eA-3
C126 0.484 0.337 0.502 !       1.36 eA-3
C127 0.019 0.580 0.475 !       1.30 eA-3
C128 0.328 0.018 0.005 !       1.29 eA-3
Q129 0.080 0.374 0.446 !       1.28 eA-3
C130 0.576 0.388 0.031 !       1.27 eA-3
Q131 0.125 0.364 0.158 !       1.25 eA-3
C132 0.638 0.016 0.030 !       1.25 eA-3
Q133 0.876 0.798 0.260 !       1.24 eA-3
Q134 0.313 0.063 0.322 !       1.24 eA-3
Q135 0.234 0.635 0.385 !       1.23 eA-3
C136 0.892 0.988 0.010 !       1.23 eA-3
Q137 0.734 0.621 0.523 !       1.22 eA-3
Q138 0.079 0.411 0.177 !       1.21 eA-3
C139 0.779 0.560 0.592 !       1.21 eA-3
Q140 0.124 0.016 0.188 !       1.21 eA-3
C141 0.419 0.030 0.499 !       1.21 eA-3
Q142 0.155 0.795 0.273 !       1.20 eA-3
Q143 0.175 0.391 0.349 !       1.18 eA-3
Q144 0.718 0.636 0.026 !       1.17 eA-3
Q145 0.799 0.205 0.932 !       1.17 eA-3
C146 0.767 0.470 0.504 !       1.16 eA-3
Q147 0.018 0.386 0.031 !       1.16 eA-3
Q148 0.312 1.002 0.307 !       1.16 eA-3
Q149 0.156 0.345 0.446 !       1.14 eA-3
Q150 0.467 0.388 0.444 !       1.13 eA-3
Q151 0.753 0.716 0.144 !       1.13 eA-3
Q152 0.702 0.546 0.197 !       1.12 eA-3
Q153 0.328 0.376 0.373 !       1.12 eA-3
C154 0.720 0.394 0.486 !       1.11 eA-3
Q155 0.986 0.391 0.862 !       1.10 eA-3
Q156 0.986 0.238 0.218 !       1.09 eA-3
Q157 0.248 0.895 0.370 !       1.09 eA-3
Q158 0.138 0.387 0.432 !       1.09 eA-3
Q159 0.329 0.024 0.146 !       1.09 eA-3
C160 0.706 0.433 0.151 !       1.08 eA-3
Q161 0.411 0.645 0.888 !       1.08 eA-3
C162 0.747 0.593 0.914 !       1.08 eA-3
Q163 0.610 0.921 0.531 !       1.07 eA-3
C164 0.278 0.573 0.030 !       1.07 eA-3
Q165 0.871 0.639 0.801 !       1.07 eA-3
Q166 0.844 0.455 0.466 !       1.06 eA-3
Q167 0.299 0.199 0.525 !       1.05 eA-3
Q168 0.623 0.802 0.565 !       1.04 eA-3
Q169 0.983 0.653 0.185 !       1.04 eA-3
Q170 0.701 0.198 0.360 !       1.03 eA-3
Q171 0.441 0.198 0.329 !       1.03 eA-3
Q172 0.439 0.160 0.175 !       1.03 eA-3
Q173 0.702 0.805 0.200 !       1.03 eA-3
Q174 0.860 0.640 0.480 !       1.03 eA-3
Q175 0.891 0.175 0.048 !       1.03 eA-3
Q176 0.123 0.908 0.684 !       1.02 eA-3
Q177 0.374 0.231 0.202 !       1.02 eA-3
Q178 0.614 0.795 0.676 !       1.00 eA-3
Q179 0.502 0.551 0.020 !       0.99 eA-3
Q180 0.926 1.004 0.111 !       0.99 eA-3
C181 0.140 0.422 0.905 !       0.98 eA-3
Q182 0.095 0.844 0.185 !       0.98 eA-3
C183 0.765 0.015 0.004 !       0.98 eA-3
Q184 0.438 0.201 0.134 !       0.98 eA-3
Q185 0.831 0.236 0.262 !       0.97 eA-3
Q186 0.844 0.608 0.260 !       0.97 eA-3
Q187 0.317 0.615 0.905 !       0.97 eA-3
Q188 0.956 0.413 0.205 !       0.97 eA-3
Q189 0.796 0.768 0.010 !       0.97 eA-3
Q190 0.831 0.768 0.770 !       0.97 eA-3
Q191 0.074 0.362 0.204 !       0.96 eA-3
Q192 0.031 0.864 0.135 !       0.96 eA-3
Q193 0.252 0.046 0.347 !       0.96 eA-3
Q194 0.559 0.919 0.394 !       0.96 eA-3
Q195 0.079 0.414 0.715 !       0.96 eA-3
C196 0.752 0.460 0.138 !       0.96 eA-3
C197 0.248 0.540 0.862 !       0.96 eA-3
Q198 0.748 0.048 0.127 !       0.95 eA-3
Q199 0.313 0.156 0.112 !       0.95 eA-3
;

_exptl_crystal_description       needle
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    none
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_T_max  0.982


_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            165009
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.328
_diffrn_reflns_theta_max         28.773
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6138
_reflns_number_gt                5402
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0168P)²+124.5668P] 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         6138
_refine_ls_number_parameters     280
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.1075
_refine_ls_wR_factor_ref         0.2370
_refine_ls_wR_factor_gt          0.2302
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_restrained_S_all      1.283
_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 0.10410(4) 0.20623(4) 0.18599(3) 0.02035(17) Uani 1 1 d . . . . .
O1A O 0.2416(5) 0.2104(6) 0.1184(3) 0.0400(19) Uani 1 1 d . . . . .
O2A O 0.1013(4) 0.2059(5) 0.0753(3) 0.0305(15) Uani 1 1 d . . . . .
C11A C 0.1893(6) 0.2086(7) 0.0705(4) 0.0251(18) Uani 1 1 d . . . . .
C1A C 0.2324(6) 0.2056(6) 0.0057(4) 0.0234(17) Uani 1 1 d . . . . .
C2A C 0.3294(6) 0.2036(7) -0.0024(4) 0.032(2) Uani 1 1 d . . . . .
H2A H 0.367957 0.200753 0.033290 0.038 Uiso 1 1 calc R U . . .
C3A C 0.3707(7) 0.2058(9) -0.0630(4) 0.045(3) Uani 1 1 d . . . . .
H3A H 0.435809 0.207093 -0.067847 0.054 Uiso 1 1 calc R U . . .
C4A C 0.3106(6) 0.2058(6) -0.1158(4) 0.0232(17) Uani 1 1 d . . . . .
C41A C 0.3531(6) 0.2078(6) -0.1818(4) 0.0250(17) Uani 1 1 d . . . . .
O3A O 0.4399(5) 0.2099(6) -0.1890(3) 0.0371(17) Uani 1 1 d . . . . .
O4A O 0.2979(5) 0.2005(5) -0.2284(3) 0.0339(16) Uani 1 1 d . . . . .
C5A C 0.2144(6) 0.2086(7) -0.1086(4) 0.031(2) Uani 1 1 d . . . . .
H5A H 0.175908 0.208998 -0.144423 0.037 Uiso 1 1 calc R U . . .
C6A C 0.1742(6) 0.2109(7) -0.0484(4) 0.030(2) Uani 1 1 d . . . . .
H6A H 0.109298 0.215835 -0.043814 0.036 Uiso 1 1 calc R U . . .
N1B N 0.0897(5) 0.0536(5) 0.1846(3) 0.0239(15) Uani 1 1 d . . . . .
C2B C 0.1283(6) 0.0119(6) 0.2305(4) 0.0271(18) Uani 1 1 d . . . . .
H2B H 0.158372 0.039987 0.263648 0.033 Uiso 1 1 calc R U . . .
C3B C 0.1237(7) -0.0764(6) 0.2293(5) 0.030(2) Uani 1 1 d . . . . .
H3B H 0.150660 -0.106554 0.262713 0.036 Uiso 1 1 calc R U . . .
C4B C 0.0811(6) -0.1207(6) 0.1809(4) 0.0255(18) Uani 1 1 d . . . . .
C5B C 0.0385(7) -0.0686(7) 0.1325(5) 0.033(2) Uani 1 1 d . U . . .
H5B H 0.005835 -0.093292 0.098977 0.039 Uiso 1 1 calc R U . . .
C6B C 0.0465(9) 0.0174(7) 0.1365(4) 0.039(3) Uani 1 1 d . . . . .
H6B H 0.020849 0.050932 0.104524 0.047 Uiso 1 1 calc R U . . .
C7B C 0.0750(7) -0.2134(6) 0.1798(5) 0.0308(19) Uani 1 1 d . U . . .
N8B N 0.1053(7) -0.2501(6) 0.2318(5) 0.041(2) Uani 1 1 d . U . . .
N9B N 0.1122(9) -0.3365(8) 0.2321(6) 0.057(3) Uani 1 1 d . U . . .
C10B C 0.0794(9) -0.3790(7) 0.1825(6) 0.047(3) Uani 1 1 d D . . . .
N11B N 0.0422(11) -0.3356(10) 0.1331(6) 0.075(4) Uani 1 1 d . . . . .
N12B N 0.0339(7) -0.2465(6) 0.1305(5) 0.038(2) Uani 1 1 d . U . . .
C13B C 0.0847(10) -0.4732(6) 0.1826(6) 0.046(3) Uani 1 1 d D . . . .
C14B C 0.1297(10) -0.5092(9) 0.2320(6) 0.056(3) Uani 1 1 d . . . . .
H14B H 0.158247 -0.477532 0.263944 0.068 Uiso 1 1 calc R U . . .
C15B C 0.1304(14) -0.5997(8) 0.2318(8) 0.072(5) Uani 1 1 d . . . . .
H15B H 0.155808 -0.625565 0.267662 0.087 Uiso 1 1 calc R U . . .
N16B N 0.0989(6) -0.6521(4) 0.1861(4) 0.0281(16) Uani 1 1 d . . . . .
C17B C 0.0541(13) -0.6063(12) 0.1414(9) 0.075(5) Uani 1 1 d . U . . .
H17B H 0.022137 -0.637084 0.110464 0.090 Uiso 1 1 calc R U . . .
C18B C 0.0496(16) -0.5158(10) 0.1355(8) 0.093(7) Uani 1 1 d . . . . .
H18B H 0.023177 -0.489454 0.100208 0.111 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
Cd1 N16B 2.238(7) 1_565 ?
Cd1 O4A 2.275(6) 7_656 ?
Cd1 O2A 2.326(6) . ?
Cd1 O3A 2.332(7) 6 ?
Cd1 O1A 2.416(7) . ?
Cd1 N1B 2.418(8) . ?
Cd1 C11A 2.711(8) . ?
O1A C11A 1.251(10) . ?
O2A C11A 1.253(10) . ?
C11A C1A 1.496(10) . ?
C1A C2A 1.388(12) . ?
C1A C6A 1.406(11) . ?
C2A C3A 1.402(12) . ?
C3A C4A 1.401(12) . ?
C4A C5A 1.375(12) . ?
C4A C41A 1.511(10) . ?
C41A O3A 1.242(10) . ?
C41A O4A 1.261(10) . ?
C5A C6A 1.390(11) . ?
N1B C2B 1.291(11) . ?
N1B C6B 1.313(11) . ?
C2B C3B 1.395(13) . ?
C3B C4B 1.375(12) . ?
C4B C5B 1.441(14) . ?
C4B C7B 1.467(13) . ?
C5B C6B 1.364(14) . ?
C7B N12B 1.298(13) . ?
C7B N8B 1.309(13) . ?
N8B N9B 1.367(15) . ?
N9B C10B 1.325(16) . ?
C10B N11B 1.352(17) . ?
C10B C13B 1.488(9) . ?
N11B N12B 1.413(17) . ?
C13B C18B 1.296(18) . ?
C13B C14B 1.345(18) . ?
C14B C15B 1.429(19) . ?
C15B N16B 1.343(15) . ?
N16B C17B 1.345(19) . ?
C17B C18B 1.43(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N16B Cd1 O4A 93.4(3) 1_565 7_656 ?
N16B Cd1 O2A 90.2(3) 1_565 . ?
O4A Cd1 O2A 143.2(2) 7_656 . ?
N16B Cd1 O3A 86.7(3) 1_565 6 ?
O4A Cd1 O3A 126.2(2) 7_656 6 ?
O2A Cd1 O3A 90.6(2) . 6 ?
N16B Cd1 O1A 90.0(3) 1_565 . ?
O4A Cd1 O1A 88.4(2) 7_656 . ?
O2A Cd1 O1A 54.9(2) . . ?
O3A Cd1 O1A 145.4(2) 6 . ?
N16B Cd1 N1B 173.2(3) 1_565 . ?
O4A Cd1 N1B 91.2(3) 7_656 . ?
O2A Cd1 N1B 89.1(3) . . ?
O3A Cd1 N1B 86.6(3) 6 . ?
O1A Cd1 N1B 95.1(3) . . ?
N16B Cd1 C11A 90.1(3) 1_565 . ?
O4A Cd1 C11A 115.8(2) 7_656 . ?
O2A Cd1 C11A 27.5(2) . . ?
O3A Cd1 C11A 118.0(2) 6 . ?
O1A Cd1 C11A 27.5(2) . . ?
N1B Cd1 C11A 92.3(3) . . ?
C11A O1A Cd1 89.5(5) . . ?
C11A O2A Cd1 93.6(5) . . ?
O1A C11A O2A 121.9(7) . . ?
O1A C11A C1A 119.4(7) . . ?
O2A C11A C1A 118.7(7) . . ?
O1A C11A Cd1 63.0(4) . . ?
O2A C11A Cd1 58.9(4) . . ?
C1A C11A Cd1 176.5(7) . . ?
C2A C1A C6A 119.0(7) . . ?
C2A C1A C11A 121.2(7) . . ?
C6A C1A C11A 119.6(7) . . ?
C1A C2A C3A 121.7(8) . . ?
C4A C3A C2A 117.7(8) . . ?
C5A C4A C3A 121.2(7) . . ?
C5A C4A C41A 119.8(8) . . ?
C3A C4A C41A 119.0(7) . . ?
O3A C41A O4A 121.6(8) . . ?
O3A C41A C4A 120.6(8) . . ?
O4A C41A C4A 117.6(7) . . ?
C41A O3A Cd1 170.9(6) . 6_655 ?
C41A O4A Cd1 103.4(5) . 7_655 ?
C4A C5A C6A 120.6(8) . . ?
C5A C6A C1A 119.6(8) . . ?
C2B N1B C6B 123.5(9) . . ?
C2B N1B Cd1 117.6(6) . . ?
C6B N1B Cd1 118.9(7) . . ?
N1B C2B C3B 118.5(9) . . ?
C4B C3B C2B 122.8(9) . . ?
C3B C4B C5B 114.6(9) . . ?
C3B C4B C7B 123.1(9) . . ?
C5B C4B C7B 122.2(8) . . ?
C6B C5B C4B 119.3(9) . . ?
N1B C6B C5B 121.3(10) . . ?
N12B C7B N8B 129.5(10) . . ?
N12B C7B C4B 116.1(9) . . ?
N8B C7B C4B 114.1(9) . . ?
C7B N8B N9B 118.0(10) . . ?
C10B N9B N8B 118.4(11) . . ?
N9B C10B N11B 119.0(11) . . ?
N9B C10B C13B 119.2(11) . . ?
N11B C10B C13B 121.8(12) . . ?
C10B N11B N12B 124.6(12) . . ?
C7B N12B N11B 109.4(10) . . ?
C18B C13B C14B 123.6(12) . . ?
C18B C13B C10B 119.9(13) . . ?
C14B C13B C10B 116.5(11) . . ?
C13B C14B C15B 115.0(12) . . ?
N16B C15B C14B 128.0(14) . . ?
C15B N16B C17B 109.0(12) . . ?
C15B N16B Cd1 127.2(8) . 1_545 ?
C17B N16B Cd1 123.5(9) . 1_545 ?
N16B C17B C18B 128.0(16) . . ?
C13B C18B C17B 115.7(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O1A C11A O2A 0.1(11) . . . . ?
Cd1 O1A C11A C1A -177.1(9) . . . . ?
Cd1 O2A C11A O1A -0.1(12) . . . . ?
Cd1 O2A C11A C1A 177.1(8) . . . . ?
O1A C11A C1A C2A 0.9(16) . . . . ?
O2A C11A C1A C2A -176.4(10) . . . . ?
O1A C11A C1A C6A -174.6(11) . . . . ?
O2A C11A C1A C6A 8.1(15) . . . . ?
C6A C1A C2A C3A -0.7(18) . . . . ?
C11A C1A C2A C3A -176.2(11) . . . . ?
C1A C2A C3A C4A -3.1(19) . . . . ?
C2A C3A C4A C5A 3.7(19) . . . . ?
C2A C3A C4A C41A -179.8(11) . . . . ?
C5A C4A C41A O3A 176.1(11) . . . . ?
C3A C4A C41A O3A -0.5(16) . . . . ?
C5A C4A C41A O4A -9.3(15) . . . . ?
C3A C4A C41A O4A 174.0(11) . . . . ?
O3A C41A O4A Cd1 -5.0(12) . . . 7_655 ?
C4A C41A O4A Cd1 -179.5(7) . . . 7_655 ?
C3A C4A C5A C6A -0.4(18) . . . . ?
C41A C4A C5A C6A -177.0(10) . . . . ?
C4A C5A C6A C1A -3.5(18) . . . . ?
C2A C1A C6A C5A 4.0(17) . . . . ?
C11A C1A C6A C5A 179.6(10) . . . . ?
C6B N1B C2B C3B -0.2(15) . . . . ?
Cd1 N1B C2B C3B -177.7(7) . . . . ?
N1B C2B C3B C4B 0.9(15) . . . . ?
C2B C3B C4B C5B -2.1(14) . . . . ?
C2B C3B C4B C7B -179.1(9) . . . . ?
C3B C4B C5B C6B 2.7(14) . . . . ?
C7B C4B C5B C6B 179.8(10) . . . . ?
C2B N1B C6B C5B 0.9(17) . . . . ?
Cd1 N1B C6B C5B 178.3(9) . . . . ?
C4B C5B C6B N1B -2.2(17) . . . . ?
C3B C4B C7B N12B -179.0(9) . . . . ?
C5B C4B C7B N12B 4.2(14) . . . . ?
C3B C4B C7B N8B 6.3(14) . . . . ?
C5B C4B C7B N8B -170.5(9) . . . . ?
N12B C7B N8B N9B 13.5(18) . . . . ?
C4B C7B N8B N9B -172.7(10) . . . . ?
C7B N8B N9B C10B -6.6(18) . . . . ?
N8B N9B C10B N11B 1.3(19) . . . . ?
N8B N9B C10B C13B -178.8(11) . . . . ?
N9B C10B N11B N12B -1(2) . . . . ?
C13B C10B N11B N12B 179.1(12) . . . . ?
N8B C7B N12B N11B -12.3(17) . . . . ?
C4B C7B N12B N11B 174.0(10) . . . . ?
C10B N11B N12B C7B 5.7(19) . . . . ?
N9B C10B C13B C18B 177.4(16) . . . . ?
N11B C10B C13B C18B -3(2) . . . . ?
N9B C10B C13B C14B -4.8(19) . . . . ?
N11B C10B C13B C14B 175.0(13) . . . . ?
C18B C13B C14B C15B -5(3) . . . . ?
C10B C13B C14B C15B 177.8(14) . . . . ?
C13B C14B C15B N16B 6(3) . . . . ?
C14B C15B N16B C17B -8(2) . . . . ?
C14B C15B N16B Cd1 178.4(13) . . . 1_545 ?
C15B N16B C17B C18B 8(3) . . . . ?
Cd1 N16B C17B C18B -177.3(16) 1_545 . . . ?
C14B C13B C18B C17B 5(3) . . . . ?
C10B C13B C18B C17B -177.1(15) . . . . ?
N16B C17B C18B C13B -8(3) . . . . ?

_refine_diff_density_max         4.382
_refine_diff_density_min         -2.381
_refine_diff_density_rms         0.238




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dimethylformamide'
_exptl_crystal_preparation       Luminescent
