# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(1)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
poly[[pentakis-(N,N-dimethylformamide)(μ₁₀-
1,3,5,7-tetrakis(5-tetrazolato)adamantane-tris-(μ-chlorido)-chlorido-
tetracopper(II)] N,N-dimethylformamide solvate]

;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(Cu 2+)4, (Cl -)4, (C14 H12 N16 4-), (C3 H7 N O)6'
_chemical_formula_sum            'C32 H54 Cl4 Cu4 N22 O6'
_chemical_formula_weight         1238.93

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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           orthorhombic
_symmetry_space_group_name_H-M   'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
_symmetry_Int_Tables_number      70


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   19.6939(4)
_cell_length_b                   27.4554(4)
_cell_length_c                   41.4894(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     22433.5(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    4208
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      23.76

_exptl_crystal_description       octahedron
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10112
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7798
_exptl_absorpt_correction_T_max  0.8449
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      113(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 APEX2 area-detector diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            57172
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         5.13
_diffrn_reflns_theta_max         23.73
_reflns_number_total             4217
_reflns_number_gt                3692
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------# 


_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.

 Methylene hydrogen atoms of the adamantane ligand were constrained, 
 with d(C-H) = 0.99 A and with U(iso) = 1.2U(eq)(C).

 The refinement was associated with disorder of coordinated chloride 
 ligands, coordinated DMF ligands and guest DMF molecules. In the structure 
 of Cu4Cl4 cluster, three chlorides are bridging connecting metal ions into 
 the finite chain, while fourth chloride is terminal. This chloride is 
 coordinated to the outer Cd ion (Cu2) of the cluster and it is disordered 
 between two symmetry related outer Cu2 sites. Therefore, the corresponding 
 coordination site at Cu2 was considered as mixed, occupied by 0.5 Cl
 and 0.5 DMF ligands.

 Other DMF ligand at the Cu2 ion is also disordered: it adopts two 
 overlapped orientations and refinement of partial occupancies (at the 
 stage of isotropic refinement) suggested partial occupancies at 0.55 and 
 0.45. A stable and well-refinable model was found while employing a set of 
 restraints for geometry and thermal motion of the disordered fragments,
 and refinement of the disorder components in different PARTs. 
 Due to very close location of Cl3 and O21 atoms (disorder Cl/DMF) and 
 O31 and O31A atoms (two orientations of coordinated DMF), for each pair 
 of these atoms we have assigned equal anisotropic displacement parameters 
 (EADP). Geometry of disordered DMF was constrained at the standard values: 
 C-O 1.23(1); C(O)-N 1.31(1); N-CH3 1.47(1). 
 Atoms of C(O)-NMe2 fragments were restrained to be coplanar within 0.01 A
 (FLAT). Also, a set of similarity restraints was used also for the thermal 
 motion (SADI/DELU) of the disordered DMF. Such an approach led to a 
 well-refinable model and therefore the H atoms were added (constrained) for 
 every of the coordinated DMF ligands, considering partial occupancy 
 factors of the corresponding parent C-atoms (with U(iso)=1.2U(eq)(C) for 
 CHO and U(iso)=1.2U(eq)(C) for methyl groups).

 Non-coordinated DMF molecules reside in the crystal voids. They are badly 
 disordered by symmetry, while adopting several overlapping positions. 
 We were not successful to resolve this disorder and the subsequent 
 refinements led to divirgence. This remaining electron density was 
 successfully modeled using SQUEEZE routine as it is implemented in 
 PLATON. 
;

_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)+(0.1208P)²+496.5938P] 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_number_reflns         4217
_refine_ls_number_parameters     346
_refine_ls_number_restraints     160
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1989
_refine_ls_wR_factor_gt          0.1931
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.002
_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
Cu1 Cu 0.18298(4) 0.46137(3) 1.091899(17) 0.0217(3) Uani 1 1 d . . .
Cu2 Cu 0.14292(4) 0.39080(3) 1.02289(2) 0.0313(3) Uani 1 1 d . . .
Cl1 Cl 0.22981(9) 0.38199(6) 1.05883(4) 0.0368(5) Uani 1 1 d . A .
Cl2 Cl 0.1250 0.53016(13) 1.1250 0.0622(9) Uani 1 2 d S . .
Cl3 Cl 0.1355(4) 0.3114(2) 1.0144(2) 0.0714(15) Uani 0.50 1 d P A 1
N1 N 0.1501(3) 0.49158(18) 0.99683(12) 0.0264(12) Uani 1 1 d . . .
N2 N 0.1581(3) 0.46257(18) 1.02231(12) 0.0244(12) Uani 1 1 d . A .
N3 N 0.1680(2) 0.48935(18) 1.04824(12) 0.0206(11) Uani 1 1 d . . .
N4 N 0.1653(3) 0.53643(17) 1.04057(12) 0.0214(11) Uani 1 1 d . A .
N5 N 0.3096(2) 0.65907(17) 0.93444(11) 0.0187(11) Uani 1 1 d . . .
N6 N 0.3405(3) 0.67851(17) 0.90876(11) 0.0184(11) Uani 1 1 d . . .
N7 N 0.2981(3) 0.68096(18) 0.88483(12) 0.0216(11) Uani 1 1 d . . .
N8 N 0.2376(3) 0.66356(18) 0.89345(12) 0.0220(11) Uani 1 1 d . . .
C1 C 0.1541(3) 0.5366(2) 1.00893(14) 0.0203(13) Uani 1 1 d . A .
C2 C 0.1412(3) 0.5808(2) 0.98832(14) 0.0205(13) Uani 1 1 d . . .
C3 C 0.2027(3) 0.5915(2) 0.96674(14) 0.0195(13) Uani 1 1 d . A .
H3A H 0.2430 0.5983 0.9803 0.023 Uiso 1 1 calc R . .
H3B H 0.2128 0.5628 0.9532 0.023 Uiso 1 1 calc R . .
C4 C 0.1877(3) 0.6355(2) 0.94531(13) 0.0176(12) Uani 1 1 d . . .
C5 C 0.1250 0.6250 0.92407(19) 0.0186(17) Uani 1 2 d S . .
H5A H 0.1342 0.5966 0.9101 0.022 Uiso 0.50 1 calc PR . .
H5B H 0.1158 0.6534 0.9101 0.022 Uiso 0.50 1 calc PR . .
C6 C 0.1250 0.6250 1.01000(19) 0.0213(18) Uani 1 2 d S . .
H6A H 0.0856 0.6175 1.0240 0.026 Uiso 0.50 1 calc PR . .
H6B H 0.1644 0.6325 1.0240 0.026 Uiso 0.50 1 calc PR . .
C7 C 0.0787(3) 0.5698(2) 0.96687(14) 0.0188(12) Uani 1 1 d . . .
H7A H 0.0391 0.5621 0.9806 0.023 Uiso 1 1 calc R . .
H7B H 0.0883 0.5411 0.9531 0.023 Uiso 1 1 calc R . .
C8 C 0.2458(3) 0.6503(2) 0.92433(13) 0.0178(12) Uani 1 1 d . A .
O11 O 0.2712(2) 0.49575(18) 1.09267(11) 0.0371(11) Uani 1 1 d DU . .
N11 N 0.3849(3) 0.4996(3) 1.09058(17) 0.0743(18) Uani 1 1 d DU . .
C11 C 0.3270(3) 0.4768(3) 1.0918(2) 0.0530(16) Uani 1 1 d DU A .
H11 H 0.3285 0.4422 1.0920 0.064 Uiso 1 1 calc R . .
C12 C 0.3878(7) 0.5515(3) 1.0827(4) 0.121(4) Uani 1 1 d DU A .
H12A H 0.3430 0.5625 1.0754 0.182 Uiso 1 1 calc R . .
H12B H 0.4212 0.5569 1.0656 0.182 Uiso 1 1 calc R . .
H12C H 0.4011 0.5700 1.1019 0.182 Uiso 1 1 calc R . .
C13 C 0.4490(4) 0.4749(5) 1.0969(4) 0.101(3) Uani 1 1 d DU A .
H13A H 0.4679 0.4866 1.1173 0.152 Uiso 1 1 calc R . .
H13B H 0.4809 0.4818 1.0794 0.152 Uiso 1 1 calc R . .
H13C H 0.4411 0.4397 1.0983 0.152 Uiso 1 1 calc R . .
O21 O 0.1219(11) 0.3226(5) 1.0223(7) 0.0714(15) Uani 0.50 1 d PDU A 2
N21 N 0.1365(6) 0.2436(4) 1.0082(3) 0.071(3) Uani 0.50 1 d PDU A 2
C21 C 0.1563(8) 0.2881(4) 1.0133(6) 0.073(2) Uani 0.50 1 d PDU A 2
H21 H 0.2031 0.2946 1.0097 0.088 Uiso 0.50 1 calc PR A 2
C22 C 0.0660(7) 0.2290(7) 1.0076(7) 0.082(4) Uani 0.50 1 d PDU A 2
H22A H 0.0395 0.2509 1.0214 0.123 Uiso 0.50 1 calc PR A 2
H22B H 0.0619 0.1956 1.0156 0.123 Uiso 0.50 1 calc PR A 2
H22C H 0.0488 0.2308 0.9855 0.123 Uiso 0.50 1 calc PR A 2
C23 C 0.1873(10) 0.2052(6) 1.0026(7) 0.093(5) Uani 0.50 1 d PDU A 2
H23A H 0.1787 0.1896 0.9818 0.139 Uiso 0.50 1 calc PR A 2
H23B H 0.1844 0.1809 1.0198 0.139 Uiso 0.50 1 calc PR A 2
H23C H 0.2328 0.2197 1.0025 0.139 Uiso 0.50 1 calc PR A 2
O31 O 0.0768(5) 0.4061(3) 0.9866(2) 0.0316(18) Uani 0.55 1 d PDU A 1
N31 N 0.0153(4) 0.4058(3) 0.9407(2) 0.050(2) Uani 0.55 1 d PDU A 1
C31 C 0.0499(7) 0.3843(4) 0.9639(2) 0.046(2) Uani 0.55 1 d PDU A 1
H31 H 0.0544 0.3499 0.9631 0.055 Uiso 0.55 1 calc PR A 1
C32 C -0.0139(9) 0.3776(6) 0.9141(3) 0.061(3) Uani 0.55 1 d PDU A 1
H32A H 0.0196 0.3539 0.9064 0.091 Uiso 0.55 1 calc PR A 1
H32B H -0.0261 0.3997 0.8964 0.091 Uiso 0.55 1 calc PR A 1
H32C H -0.0545 0.3605 0.9216 0.091 Uiso 0.55 1 calc PR A 1
C33 C 0.0057(10) 0.4590(4) 0.9416(5) 0.055(4) Uani 0.55 1 d PDU A 1
H33A H -0.0310 0.4670 0.9566 0.082 Uiso 0.55 1 calc PR A 1
H33B H -0.0062 0.4706 0.9200 0.082 Uiso 0.55 1 calc PR A 1
H33C H 0.0478 0.4746 0.9487 0.082 Uiso 0.55 1 calc PR A 1
O31A O 0.0927(6) 0.3876(4) 0.9781(2) 0.0316(18) Uani 0.45 1 d PDU A 2
N31A N 0.0711(7) 0.4375(4) 0.9357(3) 0.061(3) Uani 0.45 1 d PDU A 2
C31A C 0.1049(8) 0.4194(5) 0.9591(3) 0.052(2) Uani 0.45 1 d PDU A 2
H31A H 0.1482 0.4339 0.9620 0.062 Uiso 0.45 1 calc PR A 2
C32A C 0.1035(12) 0.4493(9) 0.9048(3) 0.076(4) Uani 0.45 1 d PDU A 2
H32D H 0.1530 0.4488 0.9073 0.114 Uiso 0.45 1 calc PR A 2
H32E H 0.0891 0.4818 0.8978 0.114 Uiso 0.45 1 calc PR A 2
H32F H 0.0900 0.4252 0.8885 0.114 Uiso 0.45 1 calc PR A 2
C33A C -0.0013(8) 0.4483(9) 0.9368(7) 0.072(5) Uani 0.45 1 d PDU A 2
H33D H -0.0272 0.4179 0.9352 0.108 Uiso 0.45 1 calc PR A 2
H33E H -0.0132 0.4696 0.9187 0.108 Uiso 0.45 1 calc PR A 2
H33F H -0.0122 0.4647 0.9571 0.108 Uiso 0.45 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O11 1.978(5) . ?
Cu1 N3 1.990(5) . ?
Cu1 N7 2.002(5) 32_556 ?
Cu1 N6 2.033(5) 30_557 ?
Cu1 Cl2 2.599(3) . ?
Cu1 Cl1 2.7354(18) . ?
Cu2 O21 1.919(16) . ?
Cu2 N2 1.993(5) . ?
Cu2 O31 2.033(9) . ?
Cu2 O31A 2.108(9) . ?
Cu2 Cl3 2.213(6) . ?
Cu2 Cl1 2.283(2) . ?
Cu2 N5 2.466(5) 30_557 ?
Cl2 Cu1 2.599(3) 11_456 ?
N1 N2 1.333(7) . ?
N1 C1 1.336(8) . ?
N2 N3 1.318(7) . ?
N3 N4 1.332(7) . ?
N4 C1 1.331(8) . ?
N5 N6 1.338(7) . ?
N5 C8 1.346(8) . ?
N5 Cu2 2.466(5) 18_667 ?
N6 N7 1.298(7) . ?
N6 Cu1 2.033(5) 18_667 ?
N7 N8 1.333(7) . ?
N7 Cu1 2.002(5) 28_565 ?
N8 C8 1.341(8) . ?
C1 C2 1.507(8) . ?
C2 C3 1.534(8) . ?
C2 C6 1.543(7) . ?
C2 C7 1.549(8) . ?
C3 C4 1.527(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C8 1.494(8) . ?
C4 C5 1.544(7) . ?
C4 C7 1.554(8) 14_455 ?
C5 C4 1.544(7) 14_455 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C2 1.543(7) 14_455 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C4 1.554(8) 14_455 ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
O11 C11 1.216(7) . ?
N11 C11 1.300(7) . ?
N11 C13 1.456(8) . ?
N11 C12 1.465(8) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
O21 C21 1.221(10) . ?
N21 C21 1.302(9) . ?
N21 C22 1.444(9) . ?
N21 C23 1.471(9) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O31 C31 1.238(9) . ?
N31 C31 1.316(8) . ?
N31 C32 1.467(9) . ?
N31 C33 1.472(9) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O31A C31A 1.200(9) . ?
N31A C31A 1.277(9) . ?
N31A C33A 1.458(10) . ?
N31A C32A 1.470(10) . ?
C31A H31A 0.9500 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?
C33A H33D 0.9800 . ?
C33A H33E 0.9800 . ?
C33A H33F 0.9800 . ?

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
O11 Cu1 N3 87.7(2) . . ?
O11 Cu1 N7 91.2(2) . 32_556 ?
N3 Cu1 N7 177.0(2) . 32_556 ?
O11 Cu1 N6 177.8(2) . 30_557 ?
N3 Cu1 N6 91.51(19) . 30_557 ?
N7 Cu1 N6 89.6(2) 32_556 30_557 ?
O11 Cu1 Cl2 91.76(15) . . ?
N3 Cu1 Cl2 97.79(15) . . ?
N7 Cu1 Cl2 85.10(15) 32_556 . ?
N6 Cu1 Cl2 86.32(14) 30_557 . ?
O11 Cu1 Cl1 95.28(15) . . ?
N3 Cu1 Cl1 84.31(15) . . ?
N7 Cu1 Cl1 92.94(15) 32_556 . ?
N6 Cu1 Cl1 86.67(14) 30_557 . ?
Cl2 Cu1 Cl1 172.73(7) . . ?
O21 Cu2 N2 175.9(8) . . ?
O21 Cu2 O31 93.1(9) . . ?
N2 Cu2 O31 83.2(3) . . ?
O21 Cu2 O31A 81.2(9) . . ?
N2 Cu2 O31A 95.8(3) . . ?
O31 Cu2 O31A 19.2(4) . . ?
O21 Cu2 Cl3 12.0(7) . . ?
N2 Cu2 Cl3 169.1(2) . . ?
O31 Cu2 Cl3 92.5(3) . . ?
O31A Cu2 Cl3 77.8(4) . . ?
O21 Cu2 Cl1 93.8(8) . . ?
N2 Cu2 Cl1 90.03(16) . . ?
O31 Cu2 Cl1 170.1(3) . . ?
O31A Cu2 Cl1 157.4(4) . . ?
Cl3 Cu2 Cl1 92.8(2) . . ?
O21 Cu2 N5 93.7(6) . 30_557 ?
N2 Cu2 N5 84.67(19) . 30_557 ?
O31 Cu2 N5 93.6(3) . 30_557 ?
O31A Cu2 N5 109.3(4) . 30_557 ?
Cl3 Cu2 N5 105.7(2) . 30_557 ?
Cl1 Cu2 N5 92.95(12) . 30_557 ?
Cu2 Cl1 Cu1 89.46(6) . . ?
Cu1 Cl2 Cu1 86.81(11) . 11_456 ?
N2 N1 C1 104.3(5) . . ?
N3 N2 N1 109.4(5) . . ?
N3 N2 Cu2 124.3(4) . . ?
N1 N2 Cu2 125.6(4) . . ?
N2 N3 N4 109.9(5) . . ?
N2 N3 Cu1 123.4(4) . . ?
N4 N3 Cu1 126.7(4) . . ?
C1 N4 N3 104.2(5) . . ?
N6 N5 C8 104.3(4) . . ?
N6 N5 Cu2 110.5(3) . 18_667 ?
C8 N5 Cu2 144.0(4) . 18_667 ?
N7 N6 N5 109.7(5) . . ?
N7 N6 Cu1 122.8(4) . 18_667 ?
N5 N6 Cu1 126.5(4) . 18_667 ?
N6 N7 N8 110.5(5) . . ?
N6 N7 Cu1 125.7(4) . 28_565 ?
N8 N7 Cu1 123.7(4) . 28_565 ?
N7 N8 C8 104.3(5) . . ?
N4 C1 N1 112.2(5) . . ?
N4 C1 C2 126.1(5) . . ?
N1 C1 C2 121.5(5) . . ?
C1 C2 C3 110.7(5) . . ?
C1 C2 C6 109.7(5) . . ?
C3 C2 C6 110.7(4) . . ?
C1 C2 C7 107.5(5) . . ?
C3 C2 C7 109.2(5) . . ?
C6 C2 C7 108.9(5) . . ?
C4 C3 C2 109.8(5) . . ?
C4 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C8 C4 C3 114.0(5) . . ?
C8 C4 C5 109.3(5) . . ?
C3 C4 C5 109.9(4) . . ?
C8 C4 C7 106.2(4) . 14_455 ?
C3 C4 C7 109.3(5) . 14_455 ?
C5 C4 C7 108.0(4) . 14_455 ?
C4 C5 C4 110.4(6) . 14_455 ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5A 109.6 14_455 . ?
C4 C5 H5B 109.6 . . ?
C4 C5 H5B 109.6 14_455 . ?
H5A C5 H5B 108.1 . . ?
C2 C6 C2 108.7(7) 14_455 . ?
C2 C6 H6A 109.9 14_455 . ?
C2 C6 H6A 109.9 . . ?
C2 C6 H6B 109.9 14_455 . ?
C2 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
C2 C7 C4 110.0(4) . 14_455 ?
C2 C7 H7A 109.7 . . ?
C4 C7 H7A 109.7 14_455 . ?
C2 C7 H7B 109.7 . . ?
C4 C7 H7B 109.7 14_455 . ?
H7A C7 H7B 108.2 . . ?
N8 C8 N5 111.1(5) . . ?
N8 C8 C4 122.6(5) . . ?
N5 C8 C4 125.5(5) . . ?
C11 O11 Cu1 126.1(5) . . ?
C11 N11 C13 121.9(7) . . ?
C11 N11 C12 120.7(7) . . ?
C13 N11 C12 117.4(9) . . ?
O11 C11 N11 126.0(7) . . ?
O11 C11 H11 117.0 . . ?
N11 C11 H11 117.0 . . ?
N11 C12 H12A 109.5 . . ?
N11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C13 H13A 109.5 . . ?
N11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C21 O21 Cu2 129.8(16) . . ?
C21 N21 C22 123.4(9) . . ?
C21 N21 C23 119.6(10) . . ?
C22 N21 C23 117.0(13) . . ?
O21 C21 N21 127.7(13) . . ?
O21 C21 H21 116.2 . . ?
N21 C21 H21 116.2 . . ?
N21 C22 H22A 109.5 . . ?
N21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N21 C23 H23A 109.5 . . ?
N21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C31 O31 Cu2 137.7(8) . . ?
C31 N31 C32 121.0(9) . . ?
C31 N31 C33 119.6(9) . . ?
C32 N31 C33 119.3(11) . . ?
O31 C31 N31 124.1(10) . . ?
O31 C31 H31 117.9 . . ?
N31 C31 H31 117.9 . . ?
N31 C32 H32A 109.5 . . ?
N31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N31 C33 H33A 109.5 . . ?
N31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31A O31A Cu2 117.0(9) . . ?
C31A N31A C33A 124.6(12) . . ?
C31A N31A C32A 121.5(11) . . ?
C33A N31A C32A 113.9(16) . . ?
O31A C31A N31A 132.6(12) . . ?
O31A C31A H31A 113.7 . . ?
N31A C31A H31A 113.7 . . ?
N31A C32A H32D 109.5 . . ?
N31A C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
N31A C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
N31A C33A H33D 109.5 . . ?
N31A C33A H33E 109.5 . . ?
H33D C33A H33E 109.5 . . ?
N31A C33A H33F 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?

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
O21 Cu2 Cl1 Cu1 -135.6(6) . . . . ?
N2 Cu2 Cl1 Cu1 43.00(16) . . . . ?
O31A Cu2 Cl1 Cu1 148.3(7) . . . . ?
Cl3 Cu2 Cl1 Cu1 -147.50(18) . . . . ?
N5 Cu2 Cl1 Cu1 -41.66(12) 30_557 . . . ?
O11 Cu1 Cl1 Cu2 -128.47(14) . . . . ?
N3 Cu1 Cl1 Cu2 -41.28(15) . . . . ?
N7 Cu1 Cl1 Cu2 140.01(15) 32_556 . . . ?
N6 Cu1 Cl1 Cu2 50.57(14) 30_557 . . . ?
O11 Cu1 Cl2 Cu1 -136.67(14) . . . 11_456 ?
N3 Cu1 Cl2 Cu1 135.38(14) . . . 11_456 ?
N7 Cu1 Cl2 Cu1 -45.58(14) 32_556 . . 11_456 ?
N6 Cu1 Cl2 Cu1 44.35(13) 30_557 . . 11_456 ?
C1 N1 N2 N3 -1.5(7) . . . . ?
C1 N1 N2 Cu2 169.5(4) . . . . ?
O31 Cu2 N2 N3 142.5(6) . . . . ?
O31A Cu2 N2 N3 157.1(6) . . . . ?
Cl3 Cu2 N2 N3 -149.9(13) . . . . ?
Cl1 Cu2 N2 N3 -44.8(5) . . . . ?
N5 Cu2 N2 N3 48.2(5) 30_557 . . . ?
O31 Cu2 N2 N1 -27.3(6) . . . . ?
O31A Cu2 N2 N1 -12.7(6) . . . . ?
Cl3 Cu2 N2 N1 40.3(17) . . . . ?
Cl1 Cu2 N2 N1 145.5(5) . . . . ?
N5 Cu2 N2 N1 -121.6(5) 30_557 . . . ?
N1 N2 N3 N4 1.4(7) . . . . ?
Cu2 N2 N3 N4 -169.8(4) . . . . ?
N1 N2 N3 Cu1 -179.6(4) . . . . ?
Cu2 N2 N3 Cu1 9.2(7) . . . . ?
O11 Cu1 N3 N2 121.2(5) . . . . ?
N6 Cu1 N3 N2 -60.9(5) 30_557 . . . ?
Cl2 Cu1 N3 N2 -147.4(4) . . . . ?
Cl1 Cu1 N3 N2 25.6(4) . . . . ?
O11 Cu1 N3 N4 -60.0(5) . . . . ?
N6 Cu1 N3 N4 118.0(5) 30_557 . . . ?
Cl2 Cu1 N3 N4 31.5(5) . . . . ?
Cl1 Cu1 N3 N4 -155.5(5) . . . . ?
N2 N3 N4 C1 -0.6(6) . . . . ?
Cu1 N3 N4 C1 -179.6(4) . . . . ?
C8 N5 N6 N7 -0.4(6) . . . . ?
Cu2 N5 N6 N7 170.2(3) 18_667 . . . ?
C8 N5 N6 Cu1 168.9(4) . . . 18_667 ?
Cu2 N5 N6 Cu1 -20.5(5) 18_667 . . 18_667 ?
N5 N6 N7 N8 0.2(6) . . . . ?
Cu1 N6 N7 N8 -169.5(4) 18_667 . . . ?
N5 N6 N7 Cu1 175.5(4) . . . 28_565 ?
Cu1 N6 N7 Cu1 5.7(6) 18_667 . . 28_565 ?
N6 N7 N8 C8 0.1(6) . . . . ?
Cu1 N7 N8 C8 -175.3(4) 28_565 . . . ?
N3 N4 C1 N1 -0.3(7) . . . . ?
N3 N4 C1 C2 175.0(6) . . . . ?
N2 N1 C1 N4 1.1(7) . . . . ?
N2 N1 C1 C2 -174.4(5) . . . . ?
N4 C1 C2 C3 108.2(7) . . . . ?
N1 C1 C2 C3 -76.9(7) . . . . ?
N4 C1 C2 C6 -14.3(8) . . . . ?
N1 C1 C2 C6 160.6(5) . . . . ?
N4 C1 C2 C7 -132.6(6) . . . . ?
N1 C1 C2 C7 42.3(8) . . . . ?
C1 C2 C3 C4 178.2(5) . . . . ?
C6 C2 C3 C4 -59.9(6) . . . . ?
C7 C2 C3 C4 59.9(6) . . . . ?
C2 C3 C4 C8 177.4(5) . . . . ?
C2 C3 C4 C5 -59.5(6) . . . . ?
C2 C3 C4 C7 58.8(6) . . . 14_455 ?
C8 C4 C5 C4 -174.4(5) . . . 14_455 ?
C3 C4 C5 C4 59.8(4) . . . 14_455 ?
C7 C4 C5 C4 -59.3(3) 14_455 . . 14_455 ?
C1 C2 C6 C2 -177.3(6) . . . 14_455 ?
C3 C2 C6 C2 60.2(4) . . . 14_455 ?
C7 C2 C6 C2 -59.9(3) . . . 14_455 ?
C1 C2 C7 C4 179.2(5) . . . 14_455 ?
C3 C2 C7 C4 -60.6(6) . . . 14_455 ?
C6 C2 C7 C4 60.3(6) . . . 14_455 ?
N7 N8 C8 N5 -0.3(6) . . . . ?
N7 N8 C8 C4 170.8(5) . . . . ?
N6 N5 C8 N8 0.4(6) . . . . ?
Cu2 N5 C8 N8 -164.5(5) 18_667 . . . ?
N6 N5 C8 C4 -170.4(5) . . . . ?
Cu2 N5 C8 C4 24.7(10) 18_667 . . . ?
C3 C4 C8 N8 138.2(6) . . . . ?
C5 C4 C8 N8 14.8(7) . . . . ?
C7 C4 C8 N8 -101.4(6) 14_455 . . . ?
C3 C4 C8 N5 -52.0(8) . . . . ?
C5 C4 C8 N5 -175.3(5) . . . . ?
C7 C4 C8 N5 68.4(7) 14_455 . . . ?
N3 Cu1 O11 C11 -111.4(7) . . . . ?
N7 Cu1 O11 C11 65.7(7) 32_556 . . . ?
Cl2 Cu1 O11 C11 150.8(6) . . . . ?
Cl1 Cu1 O11 C11 -27.4(7) . . . . ?
Cu1 O11 C11 N11 176.1(5) . . . . ?
C13 N11 C11 O11 165.8(10) . . . . ?
C12 N11 C11 O11 -14.1(10) . . . . ?
O31 Cu2 O21 C21 109(3) . . . . ?
O31A Cu2 O21 C21 94(3) . . . . ?
Cl3 Cu2 O21 C21 22(3) . . . . ?
Cl1 Cu2 O21 C21 -63(3) . . . . ?
N5 Cu2 O21 C21 -157(3) 30_557 . . . ?
Cu2 O21 C21 N21 -167.3(16) . . . . ?
C22 N21 C21 O21 10(3) . . . . ?
C23 N21 C21 O21 -170(3) . . . . ?
O21 Cu2 O31 C31 -23.9(15) . . . . ?
N2 Cu2 O31 C31 158.0(14) . . . . ?
O31A Cu2 O31 C31 27.6(13) . . . . ?
Cl3 Cu2 O31 C31 -11.9(14) . . . . ?
N5 Cu2 O31 C31 -117.8(14) 30_557 . . . ?
Cu2 O31 C31 N31 -169.6(8) . . . . ?
C32 N31 C31 O31 178.5(15) . . . . ?
C33 N31 C31 O31 -1.6(15) . . . . ?
O21 Cu2 O31A C31A -157.8(15) . . . . ?
N2 Cu2 O31A C31A 25.0(13) . . . . ?
O31 Cu2 O31A C31A 74.5(17) . . . . ?
Cl3 Cu2 O31A C31A -146.1(13) . . . . ?
Cl1 Cu2 O31A C31A -79.2(15) . . . . ?
N5 Cu2 O31A C31A 111.4(13) 30_557 . . . ?
Cu2 O31A C31A N31A -154.2(15) . . . . ?
C33A N31A C31A O31A 42(2) . . . . ?
C32A N31A C31A O31A -138(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        23.73
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.882
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.143


# SQUEEZE RESULTS (APPEND TO CIF)
# 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 0.125 0.125 0.125 549 113 '2 DMF '
2 0.375 -0.125 0.375 550 113 '2 DMF '
3 0.625 0.125 0.625 549 113 '2 DMF '
4 -0.125 -0.125 0.875 550 113 '2 DMF '
5 0.125 0.125 0.289 7 0 ' '
6 0.125 0.125 0.348 11 0 ' '
7 0.625 0.125 0.402 11 0 ' '
8 0.625 0.125 0.461 7 0 ' '
9 0.625 0.125 0.789 7 0 ' '
10 0.625 0.125 0.848 11 0 ' '
11 0.125 0.125 0.902 11 0 ' '
12 0.125 0.125 0.961 7 0 ' '
13 0.875 0.375 0.375 550 113 '2 DMF '
14 0.375 0.375 0.875 550 113 '2 DMF '
15 0.375 0.375 0.039 7 0 ' '
16 0.375 0.375 0.098 11 0 ' '
17 0.875 0.375 0.152 11 0 ' '
18 0.875 0.375 0.211 7 0 ' '
19 0.875 0.375 0.539 7 0 ' '
20 0.875 0.375 0.598 11 0 ' '
21 0.375 0.375 0.652 11 0 ' '
22 0.375 0.375 0.711 7 0 ' '
23 0.625 0.625 0.125 549 113 '2 DMF '
24 0.125 0.625 0.625 549 113 '2 DMF '
25 0.625 0.625 0.289 7 0 ' '
26 0.625 0.625 0.348 11 0 ' '
27 0.125 0.625 0.402 11 0 ' '
28 0.125 0.625 0.461 7 0 ' '
29 0.125 0.625 0.789 7 0 ' '
30 0.125 0.625 0.848 11 0 ' '
31 0.625 0.625 0.902 11 0 ' '
32 0.625 0.625 0.961 7 0 ' '
33 0.875 0.875 0.039 7 0 ' '
34 0.875 0.875 0.098 11 0 ' '
35 0.375 0.875 0.152 11 0 ' '
36 0.375 0.875 0.211 7 0 ' '
37 0.375 0.875 0.539 7 0 ' '
38 0.375 0.875 0.598 11 0 ' '
39 0.875 0.875 0.652 11 0 ' '
40 0.875 0.875 0.711 7 0 ' '
_platon_squeeze_details          
;
;


_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL IBAA in Fddd
CELL  0.71073  19.6939  27.4554  41.4894   90.000   90.000   90.000
ZERR    16.00   0.0004   0.0004   0.0009    0.000    0.000    0.000
LATT   4
SYMM  3/4 - X, 3/4 - Y,   Z
SYMM  3/4 - X,   Y, 3/4 - Z
SYMM    X, 3/4 - Y, 3/4 - Z
SFAC  C    H    N    CL   CU   O
UNIT  512  864  352  64   64   96
MERG   2
OMIT     3   1   9
OMIT     2  10   0
OMIT     1  11  13
OMIT     0   8   8
SHEL 0.8 4
FLAT 0.01 C11 N11 C12 C13
FLAT 0.01 C21 N21 C22 C23
FLAT 0.01 C31 N31 C32 C33
FLAT 0.01 C31A N31A C32A C33A
DFIX 1.230 0.01 C11 O11
DFIX 1.310 0.01 C11 N11
DFIX 1.470 0.01 N11 C12 N11 C13
DFIX 2.253 0.01 O11 N11
DFIX 2.405 0.01 C11 C12 C11 C13
DFIX 1.230 0.01 C21 O21
DFIX 1.310 0.01 C21 N21
DFIX 1.470 0.01 N21 C22 N21 C23
DFIX 2.253 0.01 O21 N21
DFIX 2.405 0.01 C21 C22 C21 C23
DFIX 1.230 0.01 C31 O31 C31A O31A
DFIX 1.310 0.01 C31 N31
DFIX 1.470 0.01 N31 C32 N31 C33
DFIX 2.253 0.01 O31A N31 O31A N31A
DFIX 2.405 0.01 C31 C32 C31 C33
DFIX 1.310 0.01 C31A N31A
DFIX 1.470 0.01 N31A C32A N31A C33A
DFIX 2.405 0.01 C31A C32A C31A C33A
EADP CL3 O21
EADP O31 O31A
DELU 0.005 O11 C11 N11 C12 C13
DELU 0.005 O21 C21 N21 C22 C23
DELU 0.005 O31 C31 N31 C32 C33
DELU 0.005 O31A C31A N31A C32A C33A
SIMU 0.005 O11 C11 N11 C12 C13
SIMU 0.005 O21 C21 N21 C22 C23
SIMU 0.005 O31 C31 N31 C32 C33
SIMU 0.005 O31A C31A N31A C32A C33A
FMAP   2
PLAN   25
SIZE     0.10   0.10   0.15
ACTA
BOND
BOND   $H
CONF
LIST   4
L.S.   8
TEMP  -160.00
WGHT    0.120800  496.593781
FVAR       0.14950
CU1   5    0.182981    0.461372    1.091899    11.00000    0.02133    0.02817 =
         0.01561    0.00842   -0.00320   -0.00312
CU2   5    0.142923    0.390800    1.022887    11.00000    0.04335    0.01801 =
         0.03239    0.00234   -0.00371   -0.00619
CL1   4    0.229813    0.381992    1.058835    11.00000    0.04177    0.03364 =
         0.03489    0.00350    0.00171    0.01436
CL2   4    0.125000    0.530157    1.125000    10.50000    0.06791    0.06572 =
         0.05288    0.00000   -0.00407    0.00000
PART   1
CL3   4    0.135453    0.311411    1.014445    10.50000    0.07630    0.02911 =
         0.10887   -0.01381    0.01759   -0.00256
PART    0
N1    3    0.150085    0.491576    0.996834    11.00000    0.04738    0.01791 =
         0.01400    0.00475   -0.00091   -0.00607
N2    3    0.158061    0.462574    1.022310    11.00000    0.03343    0.02098 =
         0.01878    0.00333   -0.00391   -0.00395
N3    3    0.168020    0.489350    1.048238    11.00000    0.01972    0.02328 =
         0.01874    0.00123   -0.00106   -0.00279
N4    3    0.165330    0.536427    1.040571    11.00000    0.02864    0.01904 =
         0.01664    0.00298   -0.00172   -0.00240
N5    3    0.309561    0.659071    0.934436    11.00000    0.02482    0.01658 =
         0.01477    0.00234   -0.00080   -0.00313
N6    3    0.340470    0.678510    0.908760    11.00000    0.02570    0.01830 =
         0.01107   -0.00024   -0.00132   -0.00351
N7    3    0.298146    0.680959    0.884827    11.00000    0.02104    0.02358 =
         0.02006    0.00321    0.00242   -0.00404
N8    3    0.237649    0.663559    0.893447    11.00000    0.02443    0.02400 =
         0.01763    0.00223    0.00170   -0.00510
C1    1    0.154051    0.536573    1.008932    11.00000    0.02582    0.02417 =
         0.01096    0.00335    0.00134   -0.00272
C2    1    0.141247    0.580832    0.988322    11.00000    0.03028    0.01812 =
         0.01296   -0.00011    0.00030   -0.00527
C3    1    0.202718    0.591536    0.966741    11.00000    0.02668    0.01753 =
         0.01444   -0.00104    0.00084   -0.00577
AFIX  23
H3A   2    0.243016    0.598306    0.980284    11.00000   -1.20000
H3B   2    0.212780    0.562778    0.953161    11.00000   -1.20000
AFIX   0
C4    1    0.187710    0.635463    0.945314    11.00000    0.02220    0.01606 =
         0.01440   -0.00190   -0.00127   -0.00462
C5    1    0.125000    0.625000    0.924069    10.50000    0.02502    0.02061 =
         0.01010    0.00000    0.00000   -0.00552
AFIX  23
H5A   2    0.134220    0.596566    0.910063    10.50000   -1.20000
H5B   2    0.115780    0.653434    0.910063    10.50000   -1.20000
AFIX   0
C6    1    0.125000    0.625000    1.009998    10.50000    0.03595    0.01791 =
         0.01014    0.00000    0.00000   -0.00345
AFIX  23
H6A   2    0.085593    0.617542    1.023967    10.50000   -1.20000
H6B   2    0.164407    0.632458    1.023967    10.50000   -1.20000
AFIX   0
C7    1    0.078750    0.569783    0.966868    11.00000    0.02734    0.01592 =
         0.01300    0.00301    0.00019   -0.00595
AFIX  23
H7A   2    0.039125    0.562083    0.980638    11.00000   -1.20000
H7B   2    0.088258    0.541113    0.953118    11.00000   -1.20000
AFIX   0
C8    1    0.245767    0.650340    0.924326    11.00000    0.02782    0.01486 =
         0.01082   -0.00041   -0.00186   -0.00760
O11   6    0.271222    0.495748    1.092667    11.00000    0.03199    0.04360 =
         0.03577    0.00988   -0.00319   -0.00727
N11   3    0.384884    0.499578    1.090583    11.00000    0.04274    0.06979 =
         0.11038    0.00288    0.00276   -0.01587
C11   1    0.327030    0.476831    1.091796    11.00000    0.03789    0.05411 =
         0.06704    0.00112    0.00169   -0.00955
AFIX  43
H11   2    0.328490    0.442247    1.092023    11.00000   -1.20000
AFIX   0
C12   1    0.387781    0.551545    1.082736    11.00000    0.09969    0.07965 =
         0.18414    0.02427    0.00384   -0.03316
AFIX  33
H12A  2    0.342998    0.562526    1.075439    11.00000   -1.50000
H12B  2    0.421164    0.556884    1.065579    11.00000   -1.50000
H12C  2    0.401120    0.569996    1.101938    11.00000   -1.50000
AFIX   0
C13   1    0.448951    0.474896    1.096909    11.00000    0.04716    0.11300 =
         0.14380   -0.01302   -0.00021    0.00034
AFIX  33
H13A  2    0.467912    0.486606    1.117327    11.00000   -1.50000
H13B  2    0.480917    0.481767    1.079387    11.00000   -1.50000
H13C  2    0.441146    0.439704    1.098272    11.00000   -1.50000
AFIX   0
PART   2
O21   6    0.121911    0.322563    1.022277    10.50000    0.07630    0.02911 =
         0.10887   -0.01381    0.01759   -0.00256
N21   3    0.136480    0.243567    1.008195    10.50000    0.06755    0.03229 =
         0.11344   -0.02064    0.00164    0.00727
C21   1    0.156312    0.288116    1.013329    10.50000    0.07448    0.03362 =
         0.11066   -0.01729    0.00853    0.00165
AFIX  43
H21   2    0.203070    0.294601    1.009686    10.50000   -1.20000
AFIX   0
C22   1    0.066020    0.229024    1.007633    10.50000    0.06781    0.05207 =
         0.12633   -0.02086   -0.00303    0.00135
AFIX  33
H22A  2    0.039498    0.250889    1.021420    10.50000   -1.50000
H22B  2    0.061902    0.195554    1.015605    10.50000   -1.50000
H22C  2    0.048844    0.230759    0.985494    10.50000   -1.50000
AFIX   0
C23   1    0.187332    0.205246    1.002615    10.50000    0.07922    0.04965 =
         0.14878   -0.02690    0.00637    0.01840
AFIX  33
H23A  2    0.178678    0.189633    0.981775    10.50000   -1.50000
H23B  2    0.184371    0.180871    1.019813    10.50000   -1.50000
H23C  2    0.232830    0.219703    1.002539    10.50000   -1.50000
AFIX   0
PART   1
O31   6    0.076842    0.406115    0.986631    10.55000    0.04018    0.02325 =
         0.03138    0.01296   -0.00922   -0.02227
N31   3    0.015312    0.405801    0.940744    10.55000    0.06775    0.04086 =
         0.04048    0.00339   -0.01068   -0.01751
C31   1    0.049851    0.384303    0.963872    10.55000    0.05923    0.03705 =
         0.04053    0.00270   -0.00572   -0.01909
AFIX  43
H31   2    0.054357    0.349875    0.963053    10.55000   -1.20000
AFIX   0
C32   1   -0.013852    0.377618    0.914077    10.55000    0.08295    0.04193 =
         0.05740   -0.00161   -0.02071   -0.01759
AFIX  33
H32A  2    0.019570    0.353855    0.906398    10.55000   -1.50000
H32B  2   -0.026057    0.399678    0.896435    10.55000   -1.50000
H32C  2   -0.054547    0.360497    0.921588    10.55000   -1.50000
AFIX   0
C33   1    0.005659    0.458953    0.941582    10.55000    0.06653    0.03963 =
         0.05836   -0.00165   -0.01045   -0.01731
AFIX  33
H33A  2   -0.030994    0.466987    0.956648    10.55000   -1.50000
H33B  2   -0.006247    0.470620    0.919986    10.55000   -1.50000
H33C  2    0.047791    0.474637    0.948671    10.55000   -1.50000
AFIX   0
PART   2
O31A  6    0.092723    0.387585    0.978057    10.45000    0.04018    0.02325 =
         0.03138    0.01296   -0.00922   -0.02227
N31A  3    0.071111    0.437463    0.935725    10.45000    0.07289    0.05740 =
         0.05197    0.02268   -0.01138   -0.01739
C31A  1    0.104925    0.419372    0.959086    10.45000    0.06589    0.04223 =
         0.04650    0.01750   -0.00808   -0.02150
AFIX  43
H31A  2    0.148241    0.433938    0.962023    10.45000   -1.20000
AFIX   0
C32A  1    0.103492    0.449319    0.904777    10.45000    0.09514    0.07977 =
         0.05248    0.02476   -0.00619   -0.01954
AFIX  33
H32D  2    0.152955    0.448787    0.907334    10.45000   -1.50000
H32E  2    0.089080    0.481825    0.897818    10.45000   -1.50000
H32F  2    0.090025    0.425248    0.888550    10.45000   -1.50000
AFIX   0
C33A  1   -0.001333    0.448318    0.936763    10.45000    0.06899    0.06840 =
         0.07824   -0.00135   -0.01672   -0.01949
AFIX  33
H33D  2   -0.027234    0.417932    0.935197    10.45000   -1.50000
H33E  2   -0.013226    0.469639    0.918680    10.45000   -1.50000
H33F  2   -0.012228    0.464678    0.957109    10.45000   -1.50000
HKLF    4
 
REM  IBAA in Fddd
REM R1 =  0.0681 for   3692 Fo > 4sig(Fo)  and  0.0747 for all   4217 data
REM    346 parameters refined using    160 restraints
 
END
 
WGHT      0.1208    496.6731
REM Highest difference peak  1.882,  deepest hole -1.144,  1-sigma level  0.143
Q1    1  -0.0417  0.4276  0.9009  11.00000  0.05    1.88
Q2    1   0.1530  0.4597  0.9543  11.00000  0.05    1.57
Q3    1   0.1677  0.4610  0.9268  11.00000  0.05    1.46
Q4    1   0.0886  0.5641  1.1167  11.00000  0.05    1.26
Q5    1   0.1400  0.1732  1.0213  11.00000  0.05    1.07
Q6    1   0.3869  0.5509  1.1070  11.00000  0.05    1.01
Q7    1   0.0826  0.2067  0.9929  11.00000  0.05    0.87
Q8    1   0.1766  0.4507  0.9093  11.00000  0.05    0.84
Q9    1   0.1085  0.2865  1.0110  11.00000  0.05    0.81
Q10   1   0.0820  0.1822  1.0146  11.00000  0.05    0.74

;
_database_code_depnum_ccdc_archive 'CCDC 991447'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(2)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
poly[[heptakis-(N,N-dimethylformamide)(μ₁₀-
1,3,5,7-tetrakis(5-tetrazolato)adamantane-tris-(μ-chlorido)-chlorido-
tetracadmium(II)] N,N-dimethylformamide solvate]
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(Cd 2+)4, (Cl -)4, (C14 H12 N16 4-), 8(C3 H7 N O)'
_chemical_formula_sum            'C38 H68 Cd4 Cl4 N24 O8'
_chemical_formula_weight         1580.56

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'
Cl Cl 0.1484 0.1585 '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   'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
_symmetry_Int_Tables_number      70


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   20.8726(7)
_cell_length_b                   27.5137(9)
_cell_length_c                   43.5530(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     25011.7(14)
_cell_formula_units_Z            16
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    5499
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             12608
_exptl_absorpt_coefficient_mu    1.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7754
_exptl_absorpt_correction_T_max  0.8213
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      113(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 APEX2 area-detector diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            31554
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_theta_min         4.08
_diffrn_reflns_theta_max         27.10
_reflns_number_total             6877
_reflns_number_gt                5066
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------# 


_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.

 Methylene hydrogen atoms of the adamantane ligand were constrained, 
 with d(C-H) = 0.99 A and with U(iso) = 1.2U(eq)(C).

 Most problems with the crystal structure refinement were associated with 
 disorder of coordinated chloride ligands, coordinated DMF ligands and guest 
 DMF molecules. In the structure of Cd4Cl4 cluster, three chlorides are 
 bridging connecting metal ions into the finite chain, while fourth chloride 
 is terminal. This chloride is coordinated to the outer Cd ion (Cd2) of the 
 cluster and it is disordered between two symmetry related outer Cd2 sites. 
 Moreover, examination of the residual electron density and parameters for 
 the thermal motion (at the stage of isotropic refinement) suggested disorder 
 of this 0.50 terminal chloride ligand over two positions of the coordination 
 environment of Cd2 (Cl3a and Cl3b, respectively), which are overlapped with 
 DMF ligands. Refinement of occupancy factors for these position led to 
 partial populations 0.30 for Cl3a and 0.70 for the corresponding DMF ligand 
 referenced by O41; 0.20 for Cl3b and 0.80 the corresponding DMF ligand 
 referenced by O21. 

 One of these DMF ligands (referenced by O41) and other DMF, coordinated to 
 the central Cd1 ions (referenced by O11) adopt disorder of --NMe2 fragments, 
 as was suggested by extremely large thermal parameters for N and C atoms 
 and high anisotropy of thermal motion. Partial occupancies of --NMe2 
 fragments were 0.35/0.35 (in total giving 0.70, as for this partially 
 occupied DMF ligand) for the first molecule and 0.65/0.35 for the DMF 
 molecule referenced by O11.

 The disorder was successfully resolved and refined in the anisotropic 
 approximation (with component of the disorder kept in different PARTs), 
 however, a set of restraints for geometry and thermal motion was applied 
 to improve the refinement stability. First, considering very close location 
 (0.13 and 0.52 A) of Cl ions and O atoms of DMF (constituting the above 
 Cl/DMF disorder), these atoms were assigned with equal anisotropic thermal 
 parameters (EADP). Equal anisotropic theraml parameters were assigned also 
 to carbon atoms of the disordered methyl groups for one of the DMF (C12, 
 C12A, C13 and C13A). Second, for every case of disordered DMF, the C-NMe2 
 fragment was restrained to be planar within 0.01 A (FLAT) and geometry 
 parameters were restrained at the standard values for DMF: C-O 1.230(5); 
 C(O)-N 1.310(5); N-CH3 1.47(5). Third, a set of similarity restrains was 
 used also for the thermal motion (SADI/DELU). Such an approach led to a 
 well-refinable model and therefore the H atoms were added (constrained) 
 for every of the coordinated DMF ligands, considering partial occupancy 
 factors of the corresponding parent C-atoms (with U(iso)=1.2U(eq)(C) for 
 CHO and  U(iso)=1.2U(eq)(C) for methyl groups).
 
 Non-coordinated DMF molecules reside in the crystal void and are disordered 
 by symmetry (two overlapping positions, with the nitrogen atom being common 
 for both of them). Carbonyl group of this molecule adopts two orientation 
 and, therefore, partial occupancy factors for the two contributions for the 
 oxygen atom were 0.25. This molecule was refined anisotropically, with a 
 set of above geometry (DFIX, FLAT) and thermal motion restraints (SADI/DELU). 
 Considering mode of the disorder, and high parameters for thermal motion, 
 the hydrogen atoms were not added in this case. 
;

_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)+(0.0781P)²+282.1452P] 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_number_reflns         6877
_refine_ls_number_parameters     435
_refine_ls_number_restraints     231
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1528
_refine_ls_wR_factor_gt          0.1359
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.035
_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 0.68392(2) 0.293057(15) 0.158649(9) 0.02784(14) Uani 1 1 d . . .
Cd2 Cd 0.62726(2) 0.369469(15) 0.225848(10) 0.03240(14) Uani 1 1 d . . .
Cl1 Cl 0.72369(8) 0.37235(6) 0.18875(4) 0.0430(4) Uani 1 1 d . A .
Cl2 Cl 0.6250 0.22842(7) 0.1250 0.0388(5) Uani 1 2 d S . .
Cl3A Cl 0.6936(9) 0.3949(4) 0.2734(3) 0.097(2) Uani 0.30 1 d PD A 1
Cl3B Cl 0.6173(9) 0.4587(7) 0.2251(7) 0.077(2) Uani 0.20 1 d P A 2
N1 N 0.6332(2) 0.25905(16) 0.25331(10) 0.0283(10) Uani 1 1 d . . .
N2 N 0.6454(2) 0.28718(18) 0.22897(10) 0.0297(11) Uani 1 1 d . A .
N3 N 0.6632(2) 0.25976(17) 0.20586(10) 0.0285(10) Uani 1 1 d . . .
N4 N 0.6636(2) 0.21344(16) 0.21400(10) 0.0281(10) Uani 1 1 d . A .
N5 N 0.8022(2) 0.10193(16) 0.31489(10) 0.0240(9) Uani 1 1 d . . .
N6 N 0.8336(2) 0.08459(16) 0.33970(10) 0.0250(10) Uani 1 1 d . . .
N7 N 0.7931(2) 0.08010(17) 0.36218(10) 0.0276(10) Uani 1 1 d . . .
N8 N 0.7341(2) 0.09376(17) 0.35362(10) 0.0280(10) Uani 1 1 d . . .
C1 C 0.6449(3) 0.21394(19) 0.24342(12) 0.0247(11) Uani 1 1 d . A .
C2 C 0.6354(3) 0.16998(19) 0.26314(11) 0.0223(11) Uani 1 1 d . . .
C3 C 0.6948(3) 0.16247(18) 0.28355(11) 0.0220(10) Uani 1 1 d . A .
H3A H 0.7018 0.1916 0.2965 0.026 Uiso 1 1 calc R . .
H3B H 0.7332 0.1577 0.2705 0.026 Uiso 1 1 calc R . .
C4 C 0.6846(2) 0.11747(18) 0.30408(11) 0.0202(10) Uani 1 1 d . . .
C5 C 0.6250 0.1250 0.32408(16) 0.0219(15) Uani 1 2 d S . .
H5 H 0.6313 0.1537 0.3374 0.026 Uiso 1 1 d R . .
C6 C 0.6250 0.1250 0.24288(15) 0.0227(15) Uani 1 2 d S . .
H6 H 0.5871 0.1299 0.2296 0.027 Uiso 1 1 d R . .
C7 C 0.5764(3) 0.17773(19) 0.28360(11) 0.0221(11) Uani 1 1 d . . .
H7A H 0.5382 0.1834 0.2706 0.027 Uiso 1 1 calc R . .
H7B H 0.5829 0.2067 0.2967 0.027 Uiso 1 1 calc R . .
C8 C 0.7410(3) 0.10647(18) 0.32402(11) 0.0223(11) Uani 1 1 d . A .
C11 C 0.8334(2) 0.2776(3) 0.15308(19) 0.065(2) Uani 1 1 d DU . .
H11 H 0.8301 0.3104 0.1466 0.078 Uiso 1 1 calc R B 1
O11 O 0.7833(2) 0.25685(19) 0.15921(13) 0.0577(14) Uani 1 1 d DU C .
N11 N 0.8911(3) 0.2594(3) 0.1545(3) 0.095(4) Uani 0.65 1 d PDU C 1
C12 C 0.9014(6) 0.2111(4) 0.1683(5) 0.103(4) Uani 0.65 1 d PDU C 1
H12A H 0.9153 0.2149 0.1896 0.154 Uiso 0.65 1 calc PR C 1
H12B H 0.9345 0.1938 0.1567 0.154 Uiso 0.65 1 calc PR C 1
H12C H 0.8614 0.1926 0.1676 0.154 Uiso 0.65 1 calc PR C 1
C13 C 0.9456(5) 0.2872(7) 0.1423(10) 0.103(4) Uani 0.65 1 d PDU C 1
H13A H 0.9371 0.3220 0.1446 0.154 Uiso 0.65 1 calc PR C 1
H13B H 0.9515 0.2794 0.1206 0.154 Uiso 0.65 1 calc PR C 1
H13C H 0.9845 0.2787 0.1537 0.154 Uiso 0.65 1 calc PR C 1
N11A N 0.8874(6) 0.2554(5) 0.1470(7) 0.095(4) Uani 0.35 1 d PD C 2
C12A C 0.8879(13) 0.2027(6) 0.1415(9) 0.103(4) Uani 0.35 1 d PD C 2
H12D H 0.9322 0.1910 0.1409 0.154 Uiso 0.35 1 calc PR C 2
H12E H 0.8669 0.1957 0.1218 0.154 Uiso 0.35 1 calc PR C 2
H12F H 0.8648 0.1862 0.1581 0.154 Uiso 0.35 1 calc PR C 2
C13A C 0.9474(6) 0.2831(11) 0.1457(18) 0.103(4) Uani 0.35 1 d PD C 2
H13D H 0.9383 0.3168 0.1398 0.154 Uiso 0.35 1 calc PR C 2
H13E H 0.9761 0.2684 0.1305 0.154 Uiso 0.35 1 calc PR C 2
H13F H 0.9681 0.2826 0.1659 0.154 Uiso 0.35 1 calc PR C 2
O21 O 0.5994(6) 0.4483(4) 0.2289(4) 0.077(2) Uani 0.80 1 d PU A 1
N21 N 0.6207(4) 0.5209(3) 0.2511(3) 0.079(2) Uani 0.80 1 d PDU A 1
C21 C 0.6375(6) 0.4792(4) 0.2391(3) 0.081(2) Uani 0.80 1 d PU A 1
H21 H 0.6820 0.4719 0.2381 0.097 Uiso 0.80 1 calc PR A 1
C22 C 0.5534(5) 0.5343(5) 0.2539(4) 0.103(3) Uani 0.80 1 d PDU A 1
H22A H 0.5276 0.5139 0.2402 0.154 Uiso 0.80 1 calc PR A 1
H22B H 0.5480 0.5685 0.2482 0.154 Uiso 0.80 1 calc PR A 1
H22C H 0.5392 0.5295 0.2751 0.154 Uiso 0.80 1 calc PR A 1
C23 C 0.6659(7) 0.5552(5) 0.2653(4) 0.105(4) Uani 0.80 1 d PDU A 1
H23A H 0.6487 0.5664 0.2850 0.158 Uiso 0.80 1 calc PR A 1
H23B H 0.6721 0.5832 0.2517 0.158 Uiso 0.80 1 calc PR A 1
H23C H 0.7071 0.5390 0.2687 0.158 Uiso 0.80 1 calc PR A 1
O31 O 0.5534(2) 0.3551(2) 0.26391(11) 0.0499(11) Uani 1 1 d U A .
N31 N 0.5083(3) 0.3481(2) 0.31026(13) 0.0563(14) Uani 1 1 d U A .
C31 C 0.5331(4) 0.3720(3) 0.28676(17) 0.0545(15) Uani 1 1 d U . .
H31 H 0.5347 0.4064 0.2885 0.065 Uiso 1 1 calc R A .
C32 C 0.4780(6) 0.3745(4) 0.3348(2) 0.092(3) Uani 1 1 d U . .
H32A H 0.4622 0.3515 0.3502 0.138 Uiso 1 1 calc R A .
H32B H 0.4420 0.3933 0.3266 0.138 Uiso 1 1 calc R . .
H32C H 0.5091 0.3966 0.3443 0.138 Uiso 1 1 calc R . .
C33 C 0.4999(5) 0.2968(3) 0.3108(2) 0.071(2) Uani 1 1 d U . .
H33A H 0.4807 0.2872 0.3304 0.107 Uiso 1 1 calc R A .
H33B H 0.5416 0.2808 0.3085 0.107 Uiso 1 1 calc R . .
H33C H 0.4716 0.2871 0.2940 0.107 Uiso 1 1 calc R . .
O41 O 0.7034(9) 0.3780(4) 0.2673(3) 0.097(2) Uani 0.70 1 d PDU A 2
C41 C 0.6972(6) 0.3517(6) 0.2896(3) 0.108(3) Uani 0.70 1 d PDU A 2
H41 H 0.6683 0.3262 0.2846 0.130 Uiso 0.70 1 calc PR A 2
N41 N 0.7140(8) 0.3466(6) 0.3151(3) 0.112(3) Uani 0.35 1 d PDU A 2
C42 C 0.6908(17) 0.3118(11) 0.3384(5) 0.119(5) Uani 0.35 1 d PDU A 2
H42A H 0.7148 0.3164 0.3575 0.179 Uiso 0.35 1 calc PR A 2
H42B H 0.6972 0.2785 0.3310 0.179 Uiso 0.35 1 calc PR A 2
H42C H 0.6452 0.3173 0.3422 0.179 Uiso 0.35 1 calc PR A 2
C43 C 0.7635(15) 0.3721(13) 0.3329(6) 0.110(4) Uani 0.35 1 d PDU A 2
H43A H 0.7660 0.3580 0.3536 0.164 Uiso 0.35 1 calc PR A 2
H43B H 0.7524 0.4066 0.3345 0.164 Uiso 0.35 1 calc PR A 2
H43C H 0.8050 0.3687 0.3227 0.164 Uiso 0.35 1 calc PR A 2
N41A N 0.7434(7) 0.3408(6) 0.3090(3) 0.111(3) Uani 0.35 1 d PDU D 3
C42A C 0.7389(15) 0.2961(9) 0.3273(7) 0.114(4) Uani 0.35 1 d PDU D 3
H42D H 0.6992 0.2789 0.3222 0.171 Uiso 0.35 1 calc PR D 3
H42E H 0.7388 0.3044 0.3492 0.171 Uiso 0.35 1 calc PR D 3
H42F H 0.7757 0.2751 0.3228 0.171 Uiso 0.35 1 calc PR D 3
C43A C 0.7986(10) 0.3737(11) 0.3118(7) 0.113(5) Uani 0.35 1 d PDU D 3
H43D H 0.7933 0.4012 0.2978 0.169 Uiso 0.35 1 calc PR D 3
H43E H 0.8380 0.3561 0.3067 0.169 Uiso 0.35 1 calc PR D 3
H43F H 0.8013 0.3858 0.3330 0.169 Uiso 0.35 1 calc PR D 3
O51 O 1.0923(19) 0.0644(6) 0.1204(6) 0.156(6) Uani 0.25 1 d PDU . .
O51A O 1.096(3) 0.0335(12) 0.0832(6) 0.156(6) Uani 0.25 1 d PDU . .
N51 N 1.1250 -0.0132(4) 0.1250 0.152(6) Uani 1 2 d SDU . .
C51 C 1.1154(13) 0.0269(6) 0.1095(3) 0.155(6) Uani 0.50 1 d PDU . .
C52 C 1.1154(14) -0.0136(7) 0.15844(14) 0.154(6) Uani 0.50 1 d PDU . .
C53 C 1.1451(14) -0.0578(6) 0.1094(4) 0.152(6) Uani 0.50 1 d PDU . .


_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 N3 2.292(4) . ?
Cd1 O11 2.301(4) . ?
Cd1 N7 2.316(4) 31_655 ?
Cd1 N6 2.386(5) 22 ?
Cd1 Cl2 2.6120(14) . ?
Cd1 Cl1 2.6771(17) . ?
Cd2 O21 2.250(12) . ?
Cd2 O31 2.298(5) . ?
Cd2 N2 2.300(5) . ?
Cd2 N5 2.416(4) 22 ?
Cd2 O41 2.416(16) . ?
Cd2 Cl3B 2.464(19) . ?
Cd2 Cl1 2.5822(18) . ?
Cd2 Cl3A 2.588(15) . ?
N1 C1 1.336(7) . ?
N1 N2 1.337(6) . ?
N2 N3 1.312(6) . ?
N3 N4 1.323(6) . ?
N4 C1 1.339(7) . ?
N5 C8 1.343(7) . ?
N5 N6 1.351(6) . ?
N6 N7 1.300(6) . ?
N7 N8 1.341(6) . ?
N8 C8 1.344(6) . ?
C1 C2 1.497(7) . ?
C2 C7 1.534(7) . ?
C2 C6 1.535(6) . ?
C2 C3 1.540(7) . ?
C3 C4 1.542(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C8 1.495(7) . ?
C4 C5 1.532(6) . ?
C4 C7 1.547(7) 2_655 ?
C5 H5 0.9900 . ?
C6 H6 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C11 O11 1.221(4) . ?
C11 N11 1.306(4) . ?
C11 N11A 1.309(5) . ?
C11 H11 0.9500 . ?
N11 C13 1.471(5) . ?
N11 C12 1.471(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N11A C13A 1.467(5) . ?
N11A C12A 1.471(5) . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C13A H13D 0.9800 . ?
C13A H13E 0.9800 . ?
C13A H13F 0.9800 . ?
O21 C21 1.246(16) . ?
N21 C21 1.310(14) . ?
N21 C22 1.458(5) . ?
N21 C23 1.472(5) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O31 C31 1.177(9) . ?
N31 C31 1.321(10) . ?
N31 C33 1.422(10) . ?
N31 C32 1.438(11) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O41 C41 1.220(5) . ?
C41 N41 1.170(9) . ?
C41 H41 0.9500 . ?
N41 C43 1.471(5) . ?
N41 C42 1.478(5) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
N41A C42A 1.469(5) . ?
N41A C43A 1.471(5) . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 0.9800 . ?
C43A H43D 0.9800 . ?
C43A H43E 0.9800 . ?
C43A H43F 0.9800 . ?
O51 C51 1.233(5) . ?
O51A C51 1.232(5) . ?
N51 C51 1.309(5) . ?
N51 C53 1.462(5) . ?
N51 C52 1.470(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
N3 Cd1 O11 89.28(17) . . ?
N3 Cd1 N7 177.12(17) . 31_655 ?
O11 Cd1 N7 90.73(17) . 31_655 ?
N3 Cd1 N6 89.95(16) . 22 ?
O11 Cd1 N6 176.22(19) . 22 ?
N7 Cd1 N6 89.86(16) 31_655 22 ?
N3 Cd1 Cl2 98.19(13) . . ?
O11 Cd1 Cl2 97.79(15) . . ?
N7 Cd1 Cl2 84.66(12) 31_655 . ?
N6 Cd1 Cl2 85.98(11) 22 . ?
N3 Cd1 Cl1 86.84(13) . . ?
O11 Cd1 Cl1 93.90(15) . . ?
N7 Cd1 Cl1 90.29(12) 31_655 . ?
N6 Cd1 Cl1 82.36(12) 22 . ?
Cl2 Cd1 Cl1 167.30(5) . . ?
O21 Cd2 O31 87.1(4) . . ?
O21 Cd2 N2 171.2(4) . . ?
O31 Cd2 N2 84.16(18) . . ?
O21 Cd2 N5 93.9(4) . 22 ?
O31 Cd2 N5 93.47(17) . 22 ?
N2 Cd2 N5 87.34(16) . 22 ?
O21 Cd2 O41 91.9(4) . . ?
O31 Cd2 O41 85.4(4) . . ?
N2 Cd2 O41 86.7(3) . . ?
N5 Cd2 O41 174.0(3) 22 . ?
O21 Cd2 Cl3B 11.0(6) . . ?
O31 Cd2 Cl3B 97.2(6) . . ?
N2 Cd2 Cl3B 174.7(6) . . ?
N5 Cd2 Cl3B 97.7(6) 22 . ?
O41 Cd2 Cl3B 88.3(7) . . ?
O21 Cd2 Cl1 102.1(3) . . ?
O31 Cd2 Cl1 168.37(13) . . ?
N2 Cd2 Cl1 86.49(13) . . ?
N5 Cd2 Cl1 92.98(11) 22 . ?
O41 Cd2 Cl1 87.2(4) . . ?
Cl3B Cd2 Cl1 91.5(5) . . ?
O21 Cd2 Cl3A 80.2(5) . . ?
O31 Cd2 Cl3A 80.1(4) . . ?
N2 Cd2 Cl3A 97.5(3) . . ?
N5 Cd2 Cl3A 171.4(3) 22 . ?
O41 Cd2 Cl3A 12.6(2) . . ?
Cl3B Cd2 Cl3A 77.7(7) . . ?
Cl1 Cd2 Cl3A 94.3(4) . . ?
Cd2 Cl1 Cd1 92.28(5) . . ?
Cd1 Cl2 Cd1 94.18(7) 4_655 . ?
C1 N1 N2 104.3(4) . . ?
N3 N2 N1 109.3(4) . . ?
N3 N2 Cd2 124.6(3) . . ?
N1 N2 Cd2 125.8(3) . . ?
N2 N3 N4 110.5(4) . . ?
N2 N3 Cd1 120.8(3) . . ?
N4 N3 Cd1 128.6(3) . . ?
N3 N4 C1 104.2(4) . . ?
C8 N5 N6 104.9(4) . . ?
C8 N5 Cd2 144.6(3) . 26 ?
N6 N5 Cd2 110.1(3) . 26 ?
N7 N6 N5 108.7(4) . . ?
N7 N6 Cd1 120.2(3) . 26 ?
N5 N6 Cd1 128.2(3) . 26 ?
N6 N7 N8 111.2(4) . . ?
N6 N7 Cd1 124.4(3) . 27_655 ?
N8 N7 Cd1 123.8(3) . 27_655 ?
N7 N8 C8 103.9(4) . . ?
N1 C1 N4 111.8(5) . . ?
N1 C1 C2 122.8(5) . . ?
N4 C1 C2 125.4(5) . . ?
C1 C2 C7 109.1(4) . . ?
C1 C2 C6 109.9(4) . . ?
C7 C2 C6 109.4(4) . . ?
C1 C2 C3 109.4(4) . . ?
C7 C2 C3 109.2(4) . . ?
C6 C2 C3 109.7(4) . . ?
C2 C3 C4 109.3(4) . . ?
C2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
C8 C4 C5 109.7(4) . . ?
C8 C4 C3 113.0(4) . . ?
C5 C4 C3 109.5(4) . . ?
C8 C4 C7 106.8(4) . 2_655 ?
C5 C4 C7 108.4(4) . 2_655 ?
C3 C4 C7 109.4(4) . 2_655 ?
C4 C5 C4 110.7(6) 2_655 . ?
C4 C5 H5 109.5 2_655 . ?
C4 C5 H5 109.5 . . ?
C2 C6 C2 109.8(6) . 2_655 ?
C2 C6 H6 109.9 . . ?
C2 C6 H6 109.4 2_655 . ?
C2 C7 C4 110.0(4) . 2_655 ?
C2 C7 H7A 109.7 . . ?
C4 C7 H7A 109.7 2_655 . ?
C2 C7 H7B 109.7 . . ?
C4 C7 H7B 109.7 2_655 . ?
H7A C7 H7B 108.2 . . ?
N5 C8 N8 111.3(4) . . ?
N5 C8 C4 126.6(4) . . ?
N8 C8 C4 121.6(5) . . ?
O11 C11 N11 126.8(5) . . ?
O11 C11 N11A 124.3(9) . . ?
O11 C11 H11 116.6 . . ?
N11 C11 H11 116.6 . . ?
N11A C11 H11 116.5 . . ?
C11 O11 Cd1 124.6(4) . . ?
C11 N11 C13 119.7(6) . . ?
C11 N11 C12 120.1(5) . . ?
C13 N11 C12 120.2(8) . . ?
N11 C12 H12A 109.5 . . ?
N11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C13 H13A 109.5 . . ?
N11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 N11A C13A 120.1(7) . . ?
C11 N11A C12A 119.9(6) . . ?
C13A N11A C12A 120.0(10) . . ?
N11A C12A H12D 109.5 . . ?
N11A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
N11A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
N11A C13A H13D 109.5 . . ?
N11A C13A H13E 109.5 . . ?
H13D C13A H13E 109.5 . . ?
N11A C13A H13F 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
C21 O21 Cd2 120.8(11) . . ?
C21 N21 C22 120.9(9) . . ?
C21 N21 C23 124.0(10) . . ?
C22 N21 C23 114.9(10) . . ?
O21 C21 N21 124.6(13) . . ?
O21 C21 H21 117.7 . . ?
N21 C21 H21 117.7 . . ?
N21 C22 H22A 109.5 . . ?
N21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N21 C23 H23A 109.5 . . ?
N21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C31 O31 Cd2 141.6(6) . . ?
C31 N31 C33 123.7(7) . . ?
C31 N31 C32 119.8(8) . . ?
C33 N31 C32 115.7(8) . . ?
O31 C31 N31 126.8(8) . . ?
O31 C31 H31 116.6 . . ?
N31 C31 H31 116.6 . . ?
N31 C32 H32A 109.5 . . ?
N31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N31 C33 H33A 109.5 . . ?
N31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C41 O41 Cd2 117.9(11) . . ?
N41 C41 O41 142.5(12) . . ?
N41 C41 H41 108.7 . . ?
O41 C41 H41 108.7 . . ?
C41 N41 C43 130.9(9) . . ?
C41 N41 C42 129.0(10) . . ?
C43 N41 C42 100.0(17) . . ?
N41 C42 H42A 109.5 . . ?
N41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N41 C43 H43A 109.5 . . ?
N41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42A N41A C43A 121.3(10) . . ?
N41A C42A H42D 109.5 . . ?
N41A C42A H42E 109.5 . . ?
H42D C42A H42E 109.5 . . ?
N41A C42A H42F 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?
N41A C43A H43D 109.5 . . ?
N41A C43A H43E 109.5 . . ?
H43D C43A H43E 109.5 . . ?
N41A C43A H43F 109.5 . . ?
H43D C43A H43F 109.5 . . ?
H43E C43A H43F 109.5 . . ?
C51 N51 C53 120.8(6) . . ?
C51 N51 C53 120.8(6) 4_755 4_755 ?
C51 N51 C52 119.7(6) 4_755 4_755 ?
C53 N51 C52 119.5(9) 4_755 4_755 ?
C51 N51 C52 119.7(6) . . ?
C53 N51 C52 119.5(9) . . ?
C52 N51 C52 179.1(15) 4_755 . ?
O51A C51 N51 131(2) . . ?
O51 C51 N51 124.5(8) . . ?
C51 C51 C52 116.6(13) 4_755 4_755 ?
O51A C51 O51 126(2) . 4_755 ?
N51 C51 O51 100.1(14) . 4_755 ?
C52 C51 O51 130(2) 4_755 4_755 ?
C51 C52 C53 113.7(6) 4_755 4_755 ?
C53 C52 O51A 153(3) 4_755 4_755 ?

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
O21 Cd2 Cl1 Cd1 -138.0(4) . . . . ?
O31 Cd2 Cl1 Cd1 80.3(7) . . . . ?
N2 Cd2 Cl1 Cd1 43.81(13) . . . . ?
N5 Cd2 Cl1 Cd1 -43.34(11) 22 . . . ?
O41 Cd2 Cl1 Cd1 130.7(3) . . . . ?
Cl3B Cd2 Cl1 Cd1 -141.1(6) . . . . ?
Cl3A Cd2 Cl1 Cd1 141.1(3) . . . . ?
N3 Cd1 Cl1 Cd2 -43.95(13) . . . . ?
O11 Cd1 Cl1 Cd2 -133.01(13) . . . . ?
N7 Cd1 Cl1 Cd2 136.24(12) 31_655 . . . ?
N6 Cd1 Cl1 Cd2 46.42(11) 22 . . . ?
Cl2 Cd1 Cl1 Cd2 69.87(19) . . . . ?
N3 Cd1 Cl2 Cd1 133.25(12) . . . 4_655 ?
O11 Cd1 Cl2 Cd1 -136.36(12) . . . 4_655 ?
N7 Cd1 Cl2 Cd1 -46.36(12) 31_655 . . 4_655 ?
N6 Cd1 Cl2 Cd1 43.88(11) 22 . . 4_655 ?
Cl1 Cd1 Cl2 Cd1 20.58(18) . . . 4_655 ?
C1 N1 N2 N3 0.3(6) . . . . ?
C1 N1 N2 Cd2 173.7(4) . . . . ?
O31 Cd2 N2 N3 149.0(5) . . . . ?
N5 Cd2 N2 N3 55.3(5) 22 . . . ?
O41 Cd2 N2 N3 -125.3(6) . . . . ?
Cl1 Cd2 N2 N3 -37.9(5) . . . . ?
Cl3A Cd2 N2 N3 -131.8(6) . . . . ?
O31 Cd2 N2 N1 -23.4(5) . . . . ?
N5 Cd2 N2 N1 -117.2(5) 22 . . . ?
O41 Cd2 N2 N1 62.3(6) . . . . ?
Cl1 Cd2 N2 N1 149.7(5) . . . . ?
Cl3A Cd2 N2 N1 55.8(6) . . . . ?
N1 N2 N3 N4 -0.2(7) . . . . ?
Cd2 N2 N3 N4 -173.7(4) . . . . ?
N1 N2 N3 Cd1 176.8(4) . . . . ?
Cd2 N2 N3 Cd1 3.3(6) . . . . ?
O11 Cd1 N3 N2 125.8(5) . . . . ?
N6 Cd1 N3 N2 -50.5(4) 22 . . . ?
Cl2 Cd1 N3 N2 -136.4(4) . . . . ?
Cl1 Cd1 N3 N2 31.9(4) . . . . ?
O11 Cd1 N3 N4 -57.7(5) . . . . ?
N6 Cd1 N3 N4 126.0(5) 22 . . . ?
Cl2 Cd1 N3 N4 40.0(5) . . . . ?
Cl1 Cd1 N3 N4 -151.7(5) . . . . ?
N2 N3 N4 C1 0.1(6) . . . . ?
Cd1 N3 N4 C1 -176.7(4) . . . . ?
C8 N5 N6 N7 -1.0(6) . . . . ?
Cd2 N5 N6 N7 173.7(3) 26 . . . ?
C8 N5 N6 Cd1 159.4(4) . . . 26 ?
Cd2 N5 N6 Cd1 -25.9(5) 26 . . 26 ?
N5 N6 N7 N8 0.2(6) . . . . ?
Cd1 N6 N7 N8 -162.1(3) 26 . . . ?
N5 N6 N7 Cd1 172.0(3) . . . 27_655 ?
Cd1 N6 N7 Cd1 9.7(6) 26 . . 27_655 ?
N6 N7 N8 C8 0.7(6) . . . . ?
Cd1 N7 N8 C8 -171.1(3) 27_655 . . . ?
N2 N1 C1 N4 -0.2(6) . . . . ?
N2 N1 C1 C2 -178.1(5) . . . . ?
N3 N4 C1 N1 0.1(6) . . . . ?
N3 N4 C1 C2 177.9(5) . . . . ?
N1 C1 C2 C7 36.3(7) . . . . ?
N4 C1 C2 C7 -141.3(5) . . . . ?
N1 C1 C2 C6 156.3(5) . . . . ?
N4 C1 C2 C6 -21.3(7) . . . . ?
N1 C1 C2 C3 -83.2(6) . . . . ?
N4 C1 C2 C3 99.3(6) . . . . ?
C1 C2 C3 C4 179.4(4) . . . . ?
C7 C2 C3 C4 60.0(5) . . . . ?
C6 C2 C3 C4 -60.0(5) . . . . ?
C2 C3 C4 C8 178.1(4) . . . . ?
C2 C3 C4 C5 -59.3(5) . . . . ?
C2 C3 C4 C7 59.4(5) . . . 2_655 ?
C8 C4 C5 C4 -175.7(5) . . . 2_655 ?
C3 C4 C5 C4 59.8(3) . . . 2_655 ?
C7 C4 C5 C4 -59.5(3) 2_655 . . 2_655 ?
C1 C2 C6 C2 -179.5(5) . . . 2_655 ?
C7 C2 C6 C2 -59.7(3) . . . 2_655 ?
C3 C2 C6 C2 60.2(3) . . . 2_655 ?
C1 C2 C7 C4 179.7(4) . . . 2_655 ?
C6 C2 C7 C4 59.4(5) . . . 2_655 ?
C3 C2 C7 C4 -60.7(5) . . . 2_655 ?
N6 N5 C8 N8 1.5(6) . . . . ?
Cd2 N5 C8 N8 -169.9(4) 26 . . . ?
N6 N5 C8 C4 -170.6(5) . . . . ?
Cd2 N5 C8 C4 18.0(10) 26 . . . ?
N7 N8 C8 N5 -1.4(6) . . . . ?
N7 N8 C8 C4 171.2(5) . . . . ?
C5 C4 C8 N5 -173.8(4) . . . . ?
C3 C4 C8 N5 -51.4(7) . . . . ?
C7 C4 C8 N5 68.9(6) 2_655 . . . ?
C5 C4 C8 N8 14.8(6) . . . . ?
C3 C4 C8 N8 137.3(5) . . . . ?
C7 C4 C8 N8 -102.5(5) 2_655 . . . ?
N11 C11 O11 Cd1 176.4(10) . . . . ?
N11A C11 O11 Cd1 -164.8(16) . . . . ?
N3 Cd1 O11 C11 -132.1(7) . . . . ?
N7 Cd1 O11 C11 45.1(7) 31_655 . . . ?
Cl2 Cd1 O11 C11 129.8(7) . . . . ?
Cl1 Cd1 O11 C11 -45.3(7) . . . . ?
O11 C11 N11 C13 171.7(17) . . . . ?
N11A C11 N11 C13 85(4) . . . . ?
O11 C11 N11 C12 -8.2(17) . . . . ?
N11A C11 N11 C12 -94(4) . . . . ?
O11 C11 N11A C13A -168(3) . . . . ?
N11 C11 N11A C13A -64(4) . . . . ?
O11 C11 N11A C12A 12(3) . . . . ?
N11 C11 N11A C12A 116(4) . . . . ?
O31 Cd2 O21 C21 111.5(14) . . . . ?
N5 Cd2 O21 C21 -155.2(14) 22 . . . ?
O41 Cd2 O21 C21 26.3(14) . . . . ?
Cl3B Cd2 O21 C21 -45(5) . . . . ?
Cl1 Cd2 O21 C21 -61.3(14) . . . . ?
Cl3A Cd2 O21 C21 31.1(14) . . . . ?
Cd2 O21 C21 N21 -156.3(12) . . . . ?
C22 N21 C21 O21 1(2) . . . . ?
C23 N21 C21 O21 174.9(16) . . . . ?
O21 Cd2 O31 C31 -38.7(9) . . . . ?
N2 Cd2 O31 C31 140.6(8) . . . . ?
N5 Cd2 O31 C31 -132.4(8) 22 . . . ?
O41 Cd2 O31 C31 53.4(9) . . . . ?
Cl3B Cd2 O31 C31 -34.2(10) . . . . ?
Cl1 Cd2 O31 C31 104.0(10) . . . . ?
Cl3A Cd2 O31 C31 41.9(8) . . . . ?
Cd2 O31 C31 N31 -151.5(7) . . . . ?
C33 N31 C31 O31 -2.9(14) . . . . ?
C32 N31 C31 O31 -171.9(9) . . . . ?
O21 Cd2 O41 C41 123.0(11) . . . . ?
O31 Cd2 O41 C41 36.1(11) . . . . ?
N2 Cd2 O41 C41 -48.3(11) . . . . ?
Cl3B Cd2 O41 C41 133.4(12) . . . . ?
Cl1 Cd2 O41 C41 -134.9(11) . . . . ?
Cl3A Cd2 O41 C41 101(4) . . . . ?
Cd2 O41 C41 N41 -165.9(18) . . . . ?
O41 C41 N41 C43 -8(3) . . . . ?
O41 C41 N41 C42 172(3) . . . . ?
C53 N51 C51 O51A 32(5) . . . . ?
C52 N51 C51 O51A -147(5) . . . . ?
C53 N51 C51 O51 172(3) . . . . ?
C52 N51 C51 O51 -8(3) . . . . ?


_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.002
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.147


_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL ibd164 in Fddd
CELL  0.71073  20.8726  27.5137  43.5530   90.000   90.000   90.000
ZERR    16.00   0.0007   0.0009   0.0013    0.000    0.000    0.000
LATT   4
SYMM  1/4 - X, 1/4 - Y,   Z
SYMM    X, 1/4 - Y, 1/4 - Z
SYMM  1/4 - X,   Y, 1/4 - Z
SFAC  C    H    N    O    CL   CD
UNIT  608  1088 384  128  64   64
MERG   2
OMIT     1   1   1
OMIT     1   5   3
OMIT     7   1   1
OMIT     4   6   2
SHEL 0.78 5.0
FLAT 0.01 C41 N41 C42 C43
FLAT 0.01 C41 N41A C42A C43A
FLAT 0.01 C51 N51 C52 C53
FLAT 0.01 C11 N11 C12 C13
FLAT 0.01 C11 N11A C12A C13A
DFIX 1.230 0.005 C41 O41
DFIX 1.470 0.005 N41 C42 N41 C43
DFIX 2.405 0.005 C41 C42 C41 C43
DFIX 1.310 0.005 C41 N41A
DFIX 1.470 0.005 N41A C42A N41A C43A
DFIX 2.405 0.005 C41 C42A C41 C43A
DFIX 2.250 0.005 O41 N41 O41 N41A
DFIX 1.230 0.005 C51 O51 C51 O51A
DFIX 1.310 0.005 C51 N51
DFIX 1.470 0.005 N51 C52 N51 C53
DFIX 2.253 0.005 O51 N51
DFIX 2.405 0.005 C51 C52 C51 C53
DFIX 1.230 0.005 C11 O11
DFIX 1.310 0.005 C11 N11 C11 N11A
DFIX 1.470 0.005 N11 C12 N11 C13
DFIX 2.253 0.005 O11 N11
DFIX 0.590 0.005 Cl3A O41
DFIX 2.405 0.005 C11 C12 C11 C13
DFIX 1.470 0.005 N11A C12A N11A C13A N21 C22 N21 C23
DFIX 2.405 0.005 C11 C12A C11 C13A
EADP Cl3A O41
EADP CL3B O21
EADP N11 N11A
EADP C12 C12A C13 C13A
DELU 0.005 O11 C11 N11 C12 C13
DELU 0.005 O41 C41 N41 C42 C43
DELU 0.005 O41 C41 N41A C42A C43A
DELU 0.005 O51 C51 N51 C52 C53
DELU 0.005 O21 C21 N21 C22 C23
DELU 0.005 031 C31 N31 C32 C33
SIMU 0.005 O21 > C23
SIMU 0.005 O31 > C33
SIMU 0.005 O41 > C43A
SIMU 0.005 O51 > C53
FMAP   2
PLAN   10
SIZE     0.13   0.13   0.17
ACTA
BOND   $H
CONF
L.S.   6
TEMP  -160.00
WGHT    0.078100  282.145233
FVAR       0.01143
CD1   6    0.683920    0.293057    0.158649    11.00000    0.02710    0.03449 =
         0.02193    0.00938    0.00758    0.00525
CD2   6    0.627264    0.369469    0.225848    11.00000    0.03867    0.02812 =
         0.03042   -0.00003   -0.00186    0.00404
CL1   5    0.723693    0.372346    0.188751    11.00000    0.04145    0.05054 =
         0.03707    0.00781   -0.00239   -0.01721
CL2   5    0.625000    0.228422    0.125000    10.50000    0.05674    0.02597 =
         0.03363    0.00000    0.01105    0.00000
PART    1
CL3A  5    0.693567    0.394929    0.273403    10.30000    0.09069    0.12480 =
         0.07586    0.00289    0.00222    0.00825
PART    2
CL3B  5    0.617262    0.458702    0.225053    10.20000    0.06607    0.04084 =
         0.12373   -0.01654   -0.01080   -0.00604
PART    0
N1    3    0.633175    0.259048    0.253311    11.00000    0.04309    0.02313 =
         0.01874    0.00120    0.00441    0.00367
N2    3    0.645430    0.287177    0.228973    11.00000    0.03716    0.03264 =
         0.01940    0.00563    0.00420    0.00625
N3    3    0.663229    0.259760    0.205859    11.00000    0.03328    0.03053 =
         0.02163    0.00746    0.00285    0.00494
N4    3    0.663567    0.213436    0.214001    11.00000    0.03656    0.02678 =
         0.02107    0.00429    0.00729    0.00759
N5    3    0.802213    0.101926    0.314892    11.00000    0.02503    0.02721 =
         0.01961   -0.00096   -0.00335    0.00216
N6    3    0.833612    0.084589    0.339701    11.00000    0.02343    0.02976 =
         0.02176    0.00249   -0.00563    0.00309
N7    3    0.793062    0.080096    0.362184    11.00000    0.02347    0.03688 =
         0.02251    0.00280   -0.00526    0.00109
N8    3    0.734054    0.093761    0.353624    11.00000    0.02859    0.03619 =
         0.01917    0.00412   -0.00462    0.00322
C1    1    0.644903    0.213938    0.243424    11.00000    0.02874    0.02780 =
         0.01754    0.00180   -0.00071    0.00902
C2    1    0.635375    0.169975    0.263137    11.00000    0.02842    0.02695 =
         0.01164    0.00020    0.00131    0.00510
C3    1    0.694823    0.162470    0.283548    11.00000    0.02539    0.02250 =
         0.01804    0.00044    0.00078    0.00431
AFIX  23
H3A   2    0.701801    0.191561    0.296501    11.00000   -1.20000
H3B   2    0.733206    0.157750    0.270532    11.00000   -1.20000
AFIX   0
C4    1    0.684573    0.117473    0.304081    11.00000    0.02235    0.02511 =
         0.01327    0.00120   -0.00120    0.00437
C5    1    0.625000    0.125000    0.324084    10.50000    0.02529    0.02635 =
         0.01394    0.00000    0.00000    0.00789
AFIX   3
H5    2    0.631292    0.153720    0.337441    11.00000   -1.20000
AFIX   0
C6    1    0.625000    0.125000    0.242880    10.50000    0.02950    0.02910 =
         0.00945    0.00000    0.00000    0.00535
AFIX   3
H6    2    0.587109    0.129851    0.229555    11.00000   -1.20000
AFIX   0
C7    1    0.576421    0.177726    0.283604    11.00000    0.02584    0.02506 =
         0.01539   -0.00080   -0.00167    0.00396
AFIX  23
H7A   2    0.538206    0.183409    0.270628    11.00000   -1.20000
H7B   2    0.582925    0.206732    0.296688    11.00000   -1.20000
AFIX   0
C8    1    0.741029    0.106471    0.324018    11.00000    0.02747    0.02438 =
         0.01520   -0.00043   -0.00135    0.00764
C11   1    0.833389    0.277589    0.153081    11.00000    0.05006    0.08380 =
         0.06064    0.01120   -0.00091    0.00166
AFIX  43
H11   2    0.830058    0.310450    0.146577    11.00000   -1.20000
AFIX   0
O11   4    0.783301    0.256850    0.159207    11.00000    0.03857    0.06732 =
         0.06711    0.02412    0.01710    0.01705
PART    1
N11   3    0.891079    0.259357    0.154527    10.65000    0.04710    0.08979 =
         0.14740    0.02395    0.01733    0.01303
C12   1    0.901432    0.211147    0.168252    10.65000    0.05520    0.09324 =
         0.15963    0.02992    0.00291    0.00126
AFIX  33
H12A  2    0.915289    0.214936    0.189617    10.65000   -1.50000
H12B  2    0.934528    0.193796    0.156651    10.65000   -1.50000
H12C  2    0.861378    0.192589    0.167632    10.65000   -1.50000
AFIX   0
C13   1    0.945597    0.287181    0.142339    10.65000    0.05520    0.09324 =
         0.15963    0.02992    0.00291    0.00126
AFIX  33
H13A  2    0.937100    0.322032    0.144581    10.65000   -1.50000
H13B  2    0.951541    0.279390    0.120568    10.65000   -1.50000
H13C  2    0.984480    0.278664    0.153746    10.65000   -1.50000
AFIX   0
PART    2
N11A  3    0.887408    0.255410    0.147023    10.35000    0.04710    0.08979 =
         0.14740    0.02395    0.01733    0.01303
C12A  1    0.887864    0.202685    0.141498    10.35000    0.05520    0.09324 =
         0.15963    0.02992    0.00291    0.00126
AFIX  33
H12D  2    0.932213    0.191033    0.140879    10.35000   -1.50000
H12E  2    0.866914    0.195704    0.121850    10.35000   -1.50000
H12F  2    0.864768    0.186180    0.158084    10.35000   -1.50000
AFIX   0
C13A  1    0.947447    0.283084    0.145727    10.35000    0.05520    0.09324 =
         0.15963    0.02992    0.00291    0.00126
AFIX  33
H13D  2    0.938256    0.316752    0.139849    10.35000   -1.50000
H13E  2    0.976123    0.268378    0.130524    10.35000   -1.50000
H13F  2    0.968058    0.282605    0.165942    10.35000   -1.50000
AFIX   0
PART    1
O21   4    0.599362    0.448299    0.228911    10.80000    0.06607    0.04084 =
         0.12373   -0.01654   -0.01080   -0.00604
N21   3    0.620689    0.520875    0.251140    10.80000    0.06619    0.04194 =
         0.12742   -0.01629   -0.00138   -0.01326
C21   1    0.637523    0.479163    0.239110    10.80000    0.06658    0.04422 =
         0.13197   -0.01405   -0.00700   -0.01060
AFIX  43
H21   2    0.681974    0.471921    0.238087    10.80000   -1.20000
AFIX   0
C22   1    0.553356    0.534301    0.253874    10.80000    0.07328    0.08662 =
         0.14788   -0.03900    0.00777    0.00003
AFIX  33
H22A  2    0.527620    0.513877    0.240174    10.80000   -1.50000
H22B  2    0.547964    0.568511    0.248167    10.80000   -1.50000
H22C  2    0.539227    0.529541    0.275121    10.80000   -1.50000
AFIX   0
C23   1    0.665908    0.555236    0.265309    10.80000    0.09323    0.05939 =
         0.16338   -0.02401   -0.02147   -0.02041
AFIX  33
H23A  2    0.648670    0.566413    0.285012    10.80000   -1.50000
H23B  2    0.672061    0.583163    0.251657    10.80000   -1.50000
H23C  2    0.707108    0.539016    0.268694    10.80000   -1.50000
AFIX   0
PART    0
O31   4    0.553409    0.355079    0.263915    11.00000    0.04632    0.07099 =
         0.03237   -0.00294    0.00302    0.01693
N31   3    0.508343    0.348110    0.310263    11.00000    0.06753    0.06786 =
         0.03344    0.00756   -0.00094    0.00702
C31   1    0.533096    0.371984    0.286761    11.00000    0.05823    0.06811 =
         0.03715    0.00518   -0.00390    0.00722
AFIX  43
H31   2    0.534666    0.406384    0.288478    11.00000   -1.20000
AFIX   0
C32   1    0.478002    0.374482    0.334787    11.00000    0.12170    0.09510 =
         0.05854   -0.00366    0.01267    0.03106
AFIX  33
H32A  2    0.462199    0.351539    0.350242    11.00000   -1.50000
H32B  2    0.442023    0.393320    0.326578    11.00000   -1.50000
H32C  2    0.509109    0.396559    0.344251    11.00000   -1.50000
AFIX   0
C33   1    0.499890    0.296816    0.310832    11.00000    0.07159    0.06778 =
         0.07424    0.01765    0.00009    0.01555
AFIX  33
H33A  2    0.480652    0.287218    0.330441    11.00000   -1.50000
H33B  2    0.541564    0.280832    0.308494    11.00000   -1.50000
H33C  2    0.471632    0.287060    0.293952    11.00000   -1.50000
AFIX   0
PART    2
O41   4    0.703412    0.377954    0.267284    10.70000    0.09069    0.12480 =
         0.07586    0.00289    0.00222    0.00825
C41   1    0.697171    0.351656    0.289636    10.70000    0.10290    0.13405 =
         0.08703    0.01296   -0.00351    0.01277
AFIX  43
H41   2    0.668274    0.326195    0.284607    10.70000   -1.20000
AFIX   0
N41   3    0.714047    0.346576    0.315053    10.35000    0.10697    0.13779 =
         0.09151    0.02047   -0.00502    0.01304
C42   1    0.690849    0.311772    0.338405    10.35000    0.11625    0.13986 =
         0.10221    0.02491    0.00018    0.01144
AFIX  33
H42A  2    0.714828    0.316396    0.357529    10.35000   -1.50000
H42B  2    0.697186    0.278502    0.330966    10.35000   -1.50000
H42C  2    0.645158    0.317348    0.342201    10.35000   -1.50000
AFIX   0
C43   1    0.763482    0.372076    0.332942    10.35000    0.10919    0.13150 =
         0.08806    0.00963    0.00037    0.01620
AFIX  33
H43A  2    0.765961    0.357952    0.353565    10.35000   -1.50000
H43B  2    0.752396    0.406600    0.334501    10.35000   -1.50000
H43C  2    0.805022    0.368665    0.322679    10.35000   -1.50000
AFIX   0
PART    3
N41A  3    0.743359    0.340797    0.308981    10.35000    0.10514    0.13577 =
         0.09184    0.01769   -0.00511    0.01393
C42A  1    0.738881    0.296099    0.327306    10.35000    0.11186    0.13724 =
         0.09200    0.01994   -0.00335    0.01181
AFIX  33
H42D  2    0.699163    0.278931    0.322171    10.35000   -1.50000
H42E  2    0.738830    0.304399    0.349188    10.35000   -1.50000
H42F  2    0.775662    0.275150    0.322783    10.35000   -1.50000
AFIX   0
C43A  1    0.798581    0.373701    0.311845    10.35000    0.10737    0.13313 =
         0.09705    0.01342    0.00204    0.01322
AFIX  33
H43D  2    0.793293    0.401175    0.297751    10.35000   -1.50000
H43E  2    0.837957    0.356079    0.306718    10.35000   -1.50000
H43F  2    0.801285    0.385771    0.332976    10.35000   -1.50000
AFIX   0
PART    0
O51   4    1.092342    0.064372    0.120423    10.25000    0.25440    0.07139 =
         0.14165    0.00262   -0.08052    0.00225
O51A  4    1.095658    0.033450    0.083192    10.25000    0.25490    0.07418 =
         0.14039    0.00172   -0.08024   -0.00042
N51   3    1.125000   -0.013223    0.125000    10.50000    0.25054    0.06743 =
         0.13661    0.00000   -0.08273    0.00000
C51   1    1.115376    0.026884    0.109521    10.50000    0.25373    0.07101 =
         0.13958    0.00287   -0.08149    0.00136
C52   1    1.115428   -0.013640    0.158445    10.50000    0.25237    0.07133 =
         0.13732    0.00080   -0.08064    0.00116
C53   1    1.145055   -0.057756    0.109420    10.50000    0.24884    0.06783 =
         0.13960   -0.00296   -0.08462   -0.00117
HKLF    4
 
REM  ibd164 in Fddd
REM R1 =  0.0521 for   5066 Fo > 4sig(Fo)  and  0.0750 for all   6877 data
REM    435 parameters refined using    231 restraints
 
END
 
WGHT      0.0781    281.8112
REM Highest difference peak  2.002,  deepest hole -0.951,  1-sigma level  0.147
Q1    1   0.8290  0.3800  0.3318  11.00000  0.05    2.00
Q2    1   0.7097  0.3657  0.3268  11.00000  0.05    1.55
Q3    1   0.6668  0.3073  0.3135  11.00000  0.05    1.32
Q4    1   0.5473  0.3324  0.2830  11.00000  0.05    1.14
Q5    1   0.8237  0.2605  0.1814  11.00000  0.05    0.96
Q6    1   1.1290 -0.0574  0.1219  11.00000  0.05    0.94
Q7    1   0.8786  0.2788  0.1797  11.00000  0.05    0.94
Q8    1   0.6483  0.4413  0.2501  11.00000  0.05    0.86
Q9    1   0.6592  0.3712  0.2380  11.00000  0.05    0.84
Q10   1   0.5164  0.3907  0.3231  11.00000  0.05    0.75
;
_database_code_depnum_ccdc_archive 'CCDC 991448'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(3)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
poly-[μ₈-(5,5',5'',5'''-(adamantane-1,3,5,7-tetrayl)-
tetrakis-tetrazolato)-dichloro-tetrakis-(N,N-dimethylformamide-\kO)-
trizinc(II)], N,N-dimethylformamide disolvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H40 Cl2 N20 O4 Zn3, 2(C3 H7 N O)'
_chemical_formula_sum            'C32 H54 Cl2 N22 O6 Zn3'
_chemical_formula_weight         1109.98

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'
Cl Cl 0.1484 0.1585 '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/n '
_space_group_name_Hall           '-P 2yn'
_symmetry_Int_Tables_number      14


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

_cell_length_a                   15.7345(5)
_cell_length_b                   20.5801(4)
_cell_length_c                   15.7442(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.1180(10)
_cell_angle_gamma                90.00
_cell_volume                     4723.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    16037
_cell_measurement_theta_min      3.134
_cell_measurement_theta_max      27.485

_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2288
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
multi-scan absorption correction did not improve the results,
uncorrected data used, mu*r = 0.084
;

_diffrn_ambient_temperature      123(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 APEX2 area-detector diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            31850
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.52
_reflns_number_total             10695
_reflns_number_gt                9210
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------# 


_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.

 merohedral twinning, plane set up by [101] and [010] used as twin element
 SHELX TWIN instruction TWIN  0 0 1 0 1 0 1 0 0
 volume ratio (BASF) 0.44/0.56
;

_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)+(0.0630P)²+5.8761P] 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_number_reflns         10695
_refine_ls_number_parameters     599
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1156
_refine_ls_wR_factor_gt          0.1071
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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 0.35371(4) 0.09174(2) 0.71213(4) 0.01707(11) Uani 1 1 d . . .
Zn2 Zn 0.20349(4) 0.08950(2) 0.85605(3) 0.01622(11) Uani 1 1 d . . .
Zn3 Zn 0.62763(3) 0.25519(2) 0.63653(3) 0.01996(11) Uani 1 1 d . . .
Cl1 Cl 0.33995(10) 0.02717(5) 0.59744(9) 0.0331(3) Uani 1 1 d . . .
Cl2 Cl 0.08897(9) 0.02506(5) 0.85109(10) 0.0306(2) Uani 1 1 d . . .
O1 O 0.7420(2) 0.19672(15) 0.7070(2) 0.0286(7) Uani 1 1 d . . .
O2 O 0.5773(2) 0.18118(16) 0.5420(2) 0.0323(8) Uani 1 1 d . . .
O3 O 0.5108(3) 0.31068(17) 0.5682(3) 0.0380(9) Uani 1 1 d . . .
O4 O 0.6793(2) 0.32585(16) 0.7366(2) 0.0314(8) Uani 1 1 d . . .
O5 O 0.7365(4) 0.1874(2) 0.3482(4) 0.0713(14) Uani 1 1 d . . .
O6 O 0.2299(4) 0.4901(2) 0.1613(4) 0.0657(14) Uani 1 1 d . . .
N1 N 0.4555(3) 0.15764(17) 0.7488(2) 0.0192(7) Uani 1 1 d . . .
N2 N 0.4827(3) 0.17388(18) 0.6797(3) 0.0200(8) Uani 1 1 d . . .
N3 N 0.5505(3) 0.21437(16) 0.7120(3) 0.0191(7) Uani 1 1 d . . .
N4 N 0.5714(3) 0.22649(16) 0.8016(3) 0.0190(7) Uani 1 1 d . . .
N5 N 0.2432(2) 0.15257(16) 0.9604(2) 0.0177(7) Uani 1 1 d . . .
N6 N 0.1734(3) 0.16609(18) 0.9889(3) 0.0207(8) Uani 1 1 d . . .
N7 N 0.2068(3) 0.20518(16) 1.0587(3) 0.0193(7) Uani 1 1 d . . .
N8 N 0.2968(3) 0.21847(17) 1.0776(3) 0.0200(8) Uani 1 1 d . . .
N9 N 0.5808(3) 0.02101(15) 1.1623(3) 0.0177(7) Uani 1 1 d . . .
N10 N 0.6388(3) -0.02945(16) 1.1843(3) 0.0177(8) Uani 1 1 d . . .
N11 N 0.6916(3) -0.02743(16) 1.1370(3) 0.0174(8) Uani 1 1 d . . .
N12 N 0.6709(3) 0.02415(16) 1.0825(3) 0.0178(7) Uani 1 1 d . . .
N13 N 0.7041(3) 0.31501(17) 1.1257(3) 0.0212(8) Uani 1 1 d . . .
N14 N 0.7362(3) 0.35746(16) 1.1933(3) 0.0193(7) Uani 1 1 d . . .
N15 N 0.6818(3) 0.35951(16) 1.2397(3) 0.0183(7) Uani 1 1 d . . .
N16 N 0.6120(3) 0.31828(17) 1.2029(3) 0.0211(8) Uani 1 1 d . . .
N17 N 0.8635(3) 0.1398(2) 0.7001(3) 0.0340(10) Uani 1 1 d . . .
N18 N 0.5209(3) 0.13155(19) 0.4054(3) 0.0343(9) Uani 1 1 d . . .
N19 N 0.4118(3) 0.3899(2) 0.4911(3) 0.0363(10) Uani 1 1 d . . .
N20 N 0.7474(3) 0.3381(2) 0.8905(3) 0.0352(10) Uani 1 1 d . . .
N21 N 0.8374(4) 0.1075(3) 0.3424(5) 0.0706(15) Uani 1 1 d . . .
N22 N 0.1839(3) 0.5001(2) 0.2800(3) 0.0368(11) Uani 1 1 d . . .
C1 C 0.5100(3) 0.19142(19) 0.8222(3) 0.0163(8) Uani 1 1 d . . .
C2 C 0.5101(3) 0.18704(19) 0.9168(3) 0.0143(8) Uani 1 1 d . . .
C3 C 0.4109(2) 0.18979(15) 0.9156(2) 0.0148(6) Uani 1 1 d . . .
H3A H 0.3816 0.2313 0.8882 0.018 Uiso 1 1 calc R . .
H3B H 0.3741 0.1538 0.8777 0.018 Uiso 1 1 calc R . .
C4 C 0.4131(3) 0.18408(19) 1.0131(3) 0.0156(9) Uani 1 1 d . . .
C5 C 0.4591(3) 0.11950(17) 1.0553(3) 0.0133(8) Uani 1 1 d . . .
H5A H 0.4228 0.0828 1.0189 0.016 Uiso 1 1 calc R . .
H5B H 0.4606 0.1156 1.1185 0.016 Uiso 1 1 calc R . .
C6 C 0.5584(2) 0.11597(14) 1.0573(2) 0.0141(6) Uani 1 1 d . . .
C7 C 0.6143(2) 0.17293(14) 1.1146(2) 0.0142(6) Uani 1 1 d . . .
H7A H 0.6776 0.1714 1.1158 0.017 Uiso 1 1 calc R . .
H7B H 0.6175 0.1691 1.1785 0.017 Uiso 1 1 calc R . .
C8 C 0.5692(2) 0.23825(14) 1.0733(2) 0.0150(6) Uani 1 1 d . . .
C9 C 0.5660(3) 0.24361(19) 0.9751(3) 0.0155(8) Uani 1 1 d . . .
H9A H 0.6291 0.2426 0.9757 0.019 Uiso 1 1 calc R . .
H9B H 0.5375 0.2854 0.9479 0.019 Uiso 1 1 calc R . .
C10 C 0.4704(3) 0.24034(18) 1.0714(3) 0.0146(8) Uani 1 1 d . . .
H10A H 0.4719 0.2370 1.1347 0.017 Uiso 1 1 calc R . .
H10B H 0.4415 0.2823 1.0454 0.017 Uiso 1 1 calc R . .
C11 C 0.5555(3) 0.12213(18) 0.9597(3) 0.0158(8) Uani 1 1 d . . .
H11A H 0.5202 0.0854 0.9222 0.019 Uiso 1 1 calc R . .
H11B H 0.6186 0.1202 0.9604 0.019 Uiso 1 1 calc R . .
C12 C 0.3168(3) 0.18576(19) 1.0152(3) 0.0151(8) Uani 1 1 d . . .
C13 C 0.6026(2) 0.05343(15) 1.0995(2) 0.0156(6) Uani 1 1 d . . .
C14 C 0.6269(3) 0.29159(15) 1.1321(3) 0.0162(6) Uani 1 1 d . . .
C15 C 0.7759(4) 0.1554(2) 0.6689(3) 0.0320(11) Uani 1 1 d . . .
H15 H 0.7359 0.1346 0.6147 0.038 Uiso 1 1 calc R . .
C16 C 0.9288(4) 0.1716(3) 0.7790(4) 0.0445(14) Uani 1 1 d . . .
H16A H 0.9411 0.2153 0.7621 0.067 Uiso 1 1 calc R . .
H16B H 0.9859 0.1465 0.8015 0.067 Uiso 1 1 calc R . .
H16C H 0.9038 0.1745 0.8273 0.067 Uiso 1 1 calc R . .
C17 C 0.8980(4) 0.0922(3) 0.6525(4) 0.0420(13) Uani 1 1 d . . .
H17A H 0.8464 0.0724 0.6027 0.063 Uiso 1 1 calc R . .
H17B H 0.9321 0.0583 0.6957 0.063 Uiso 1 1 calc R . .
H17C H 0.9388 0.1137 0.6271 0.063 Uiso 1 1 calc R . .
C18 C 0.5642(3) 0.1792(2) 0.4602(3) 0.0313(11) Uani 1 1 d . . .
H18 H 0.5866 0.2141 0.4349 0.038 Uiso 1 1 calc R . .
C19 C 0.4879(5) 0.0753(3) 0.4399(4) 0.0485(14) Uani 1 1 d . . .
H19A H 0.5008 0.0811 0.5053 0.073 Uiso 1 1 calc R . .
H19B H 0.5191 0.0362 0.4311 0.073 Uiso 1 1 calc R . .
H19C H 0.4216 0.0707 0.4064 0.073 Uiso 1 1 calc R . .
C20 C 0.5103(5) 0.1320(3) 0.3110(4) 0.0544(17) Uani 1 1 d . . .
H20A H 0.5410 0.1703 0.2990 0.082 Uiso 1 1 calc R . .
H20B H 0.4449 0.1335 0.2722 0.082 Uiso 1 1 calc R . .
H20C H 0.5377 0.0926 0.2974 0.082 Uiso 1 1 calc R . .
C21 C 0.4939(4) 0.3611(2) 0.5242(3) 0.0349(11) Uani 1 1 d . . .
H21 H 0.5427 0.3815 0.5128 0.042 Uiso 1 1 calc R . .
C22 C 0.3316(5) 0.3651(3) 0.5070(6) 0.0547(17) Uani 1 1 d . . .
H22A H 0.2861 0.3489 0.4492 0.082 Uiso 1 1 calc R . .
H22B H 0.3045 0.4001 0.5307 0.082 Uiso 1 1 calc R . .
H22C H 0.3505 0.3296 0.5517 0.082 Uiso 1 1 calc R . .
C23 C 0.3966(5) 0.4474(3) 0.4343(5) 0.0545(16) Uani 1 1 d . . .
H23A H 0.3756 0.4830 0.4628 0.082 Uiso 1 1 calc R . .
H23B H 0.3499 0.4382 0.3735 0.082 Uiso 1 1 calc R . .
H23C H 0.4540 0.4600 0.4280 0.082 Uiso 1 1 calc R . .
C24 C 0.7400(4) 0.3122(2) 0.8113(4) 0.0357(11) Uani 1 1 d . . .
H24 H 0.7845 0.2809 0.8117 0.043 Uiso 1 1 calc R . .
C25 C 0.6766(4) 0.3829(3) 0.8933(4) 0.0417(13) Uani 1 1 d . . .
H25A H 0.7019 0.4270 0.9059 0.062 Uiso 1 1 calc R . .
H25B H 0.6555 0.3696 0.9419 0.062 Uiso 1 1 calc R . .
H25C H 0.6248 0.3823 0.8342 0.062 Uiso 1 1 calc R . .
C26 C 0.8211(4) 0.3209(3) 0.9745(4) 0.0419(13) Uani 1 1 d . . .
H26A H 0.8616 0.2896 0.9616 0.063 Uiso 1 1 calc R . .
H26B H 0.7959 0.3015 1.0168 0.063 Uiso 1 1 calc R . .
H26C H 0.8560 0.3600 1.0024 0.063 Uiso 1 1 calc R . .
C27 C 0.7733(6) 0.1345(4) 0.3701(5) 0.065(2) Uani 1 1 d . . .
H27 H 0.7552 0.1094 0.4111 0.079 Uiso 1 1 calc R . .
C28 C 0.8663(6) 0.1409(4) 0.2781(6) 0.079(3) Uani 1 1 d . . .
H28A H 0.8543 0.1136 0.2238 0.118 Uiso 1 1 calc R . .
H28B H 0.9321 0.1502 0.3065 0.118 Uiso 1 1 calc R . .
H28C H 0.8322 0.1818 0.2599 0.118 Uiso 1 1 calc R . .
C29 C 0.8787(7) 0.0444(4) 0.3753(7) 0.104(3) Uani 1 1 d . . .
H29A H 0.8404 0.0206 0.4016 0.156 Uiso 1 1 calc R . .
H29B H 0.9401 0.0507 0.4225 0.156 Uiso 1 1 calc R . .
H29C H 0.8833 0.0196 0.3242 0.156 Uiso 1 1 calc R . .
C30 C 0.2357(4) 0.5164(2) 0.2336(4) 0.0468(14) Uani 1 1 d . . .
H30 H 0.2797 0.5501 0.2574 0.056 Uiso 1 1 calc R . .
C31 C 0.1170(5) 0.4486(4) 0.2498(6) 0.071(2) Uani 1 1 d . . .
H31A H 0.0576 0.4645 0.2481 0.106 Uiso 1 1 calc R . .
H31B H 0.1371 0.4119 0.2925 0.106 Uiso 1 1 calc R . .
H31C H 0.1108 0.4344 0.1884 0.106 Uiso 1 1 calc R . .
C32 C 0.1934(7) 0.5338(4) 0.3628(5) 0.088(3) Uani 1 1 d . . .
H32A H 0.2024 0.5022 0.4120 0.132 Uiso 1 1 calc R . .
H32B H 0.1379 0.5592 0.3531 0.132 Uiso 1 1 calc R . .
H32C H 0.2465 0.5629 0.3800 0.132 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
Zn1 N1 2.010(4) . ?
Zn1 N10 2.042(3) 3_657 ?
Zn1 N14 2.045(4) 4_565 ?
Zn1 Cl1 2.1861(12) . ?
Zn2 N5 2.000(4) . ?
Zn2 N15 2.025(3) 4_565 ?
Zn2 N11 2.057(3) 3_657 ?
Zn2 Cl2 2.2149(12) . ?
Zn3 O2 2.067(3) . ?
Zn3 O4 2.072(3) . ?
Zn3 O3 2.086(4) . ?
Zn3 O1 2.101(3) . ?
Zn3 N3 2.163(3) . ?
Zn3 N7 2.206(3) 4_665 ?
O1 C15 1.270(6) . ?
O2 C18 1.227(6) . ?
O3 C21 1.220(6) . ?
O4 C24 1.235(6) . ?
O5 C27 1.222(9) . ?
O6 C30 1.232(8) . ?
N1 C1 1.345(6) . ?
N1 N2 1.352(5) . ?
N2 N3 1.296(5) . ?
N3 N4 1.346(5) . ?
N4 C1 1.340(5) . ?
N5 C12 1.340(5) . ?
N5 N6 1.362(5) . ?
N6 N7 1.303(5) . ?
N7 N8 1.361(5) . ?
N7 Zn3 2.206(3) 4_566 ?
N8 C12 1.323(5) . ?
N9 N10 1.339(5) . ?
N9 C13 1.340(5) . ?
N10 N11 1.309(4) . ?
N10 Zn1 2.042(3) 3_657 ?
N11 N12 1.327(5) . ?
N11 Zn2 2.057(3) 3_657 ?
N12 C13 1.345(5) . ?
N13 N14 1.321(5) . ?
N13 C14 1.345(5) . ?
N14 N15 1.320(4) . ?
N14 Zn1 2.045(4) 4_666 ?
N15 N16 1.335(5) . ?
N15 Zn2 2.025(3) 4_666 ?
N16 C14 1.340(5) . ?
N17 C15 1.316(6) . ?
N17 C16 1.436(8) . ?
N17 C17 1.459(7) . ?
N18 C18 1.314(6) . ?
N18 C20 1.431(7) . ?
N18 C19 1.455(6) . ?
N19 C21 1.335(6) . ?
N19 C23 1.449(7) . ?
N19 C22 1.468(7) . ?
N20 C24 1.320(7) . ?
N20 C26 1.437(8) . ?
N20 C25 1.461(7) . ?
N21 C27 1.359(10) . ?
N21 C28 1.432(10) . ?
N21 C29 1.456(10) . ?
N22 C30 1.327(7) . ?
N22 C32 1.434(8) . ?
N22 C31 1.443(8) . ?
C1 C2 1.492(5) . ?
C2 C9 1.537(6) . ?
C2 C11 1.545(6) . ?
C2 C3 1.555(5) . ?
C3 C4 1.526(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C12 1.529(6) . ?
C4 C5 1.540(5) . ?
C4 C10 1.540(6) . ?
C5 C6 1.552(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C13 1.495(4) . ?
C6 C11 1.525(5) . ?
C6 C7 1.538(4) . ?
C7 C8 1.545(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C14 1.501(4) . ?
C8 C9 1.533(5) . ?
C8 C10 1.544(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

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
N1 Zn1 N10 113.22(15) . 3_657 ?
N1 Zn1 N14 105.99(14) . 4_565 ?
N10 Zn1 N14 102.37(13) 3_657 4_565 ?
N1 Zn1 Cl1 117.87(11) . . ?
N10 Zn1 Cl1 103.63(11) 3_657 . ?
N14 Zn1 Cl1 112.81(12) 4_565 . ?
N5 Zn2 N15 107.51(14) . 4_565 ?
N5 Zn2 N11 111.29(15) . 3_657 ?
N15 Zn2 N11 103.21(14) 4_565 3_657 ?
N5 Zn2 Cl2 114.58(10) . . ?
N15 Zn2 Cl2 114.85(12) 4_565 . ?
N11 Zn2 Cl2 104.82(10) 3_657 . ?
O2 Zn3 O4 177.03(13) . . ?
O2 Zn3 O3 90.44(15) . . ?
O4 Zn3 O3 91.45(15) . . ?
O2 Zn3 O1 88.74(14) . . ?
O4 Zn3 O1 89.27(15) . . ?
O3 Zn3 O1 177.68(13) . . ?
O2 Zn3 N3 88.11(13) . . ?
O4 Zn3 N3 89.75(13) . . ?
O3 Zn3 N3 85.88(14) . . ?
O1 Zn3 N3 91.93(13) . . ?
O2 Zn3 N7 90.92(13) . 4_665 ?
O4 Zn3 N7 91.20(13) . 4_665 ?
O3 Zn3 N7 94.77(14) . 4_665 ?
O1 Zn3 N7 87.41(13) . 4_665 ?
N3 Zn3 N7 178.84(14) . 4_665 ?
C15 O1 Zn3 124.2(3) . . ?
C18 O2 Zn3 130.4(3) . . ?
C21 O3 Zn3 136.1(4) . . ?
C24 O4 Zn3 120.4(3) . . ?
C1 N1 N2 105.7(3) . . ?
C1 N1 Zn1 141.0(3) . . ?
N2 N1 Zn1 113.3(3) . . ?
N3 N2 N1 107.8(3) . . ?
N2 N3 N4 111.8(3) . . ?
N2 N3 Zn3 125.7(3) . . ?
N4 N3 Zn3 122.5(3) . . ?
C1 N4 N3 103.8(4) . . ?
C12 N5 N6 107.0(3) . . ?
C12 N5 Zn2 141.8(3) . . ?
N6 N5 Zn2 111.2(3) . . ?
N7 N6 N5 106.6(3) . . ?
N6 N7 N8 111.3(3) . . ?
N6 N7 Zn3 124.4(3) . 4_566 ?
N8 N7 Zn3 124.3(3) . 4_566 ?
C12 N8 N7 104.7(4) . . ?
N10 N9 C13 103.8(3) . . ?
N11 N10 N9 110.2(3) . . ?
N11 N10 Zn1 128.0(3) . 3_657 ?
N9 N10 Zn1 121.5(2) . 3_657 ?
N10 N11 N12 109.9(4) . . ?
N10 N11 Zn2 128.2(3) . 3_657 ?
N12 N11 Zn2 121.9(3) . 3_657 ?
N11 N12 C13 104.4(3) . . ?
N14 N13 C14 105.0(3) . . ?
N15 N14 N13 109.6(4) . . ?
N15 N14 Zn1 130.0(3) . 4_666 ?
N13 N14 Zn1 120.4(3) . 4_666 ?
N14 N15 N16 109.8(4) . . ?
N14 N15 Zn2 126.4(3) . 4_666 ?
N16 N15 Zn2 123.6(3) . 4_666 ?
N15 N16 C14 104.4(3) . . ?
C15 N17 C16 121.3(4) . . ?
C15 N17 C17 120.8(5) . . ?
C16 N17 C17 117.8(4) . . ?
C18 N18 C20 120.3(5) . . ?
C18 N18 C19 121.3(4) . . ?
C20 N18 C19 118.3(5) . . ?
C21 N19 C23 120.9(5) . . ?
C21 N19 C22 123.1(5) . . ?
C23 N19 C22 115.9(5) . . ?
C24 N20 C26 121.6(5) . . ?
C24 N20 C25 119.1(5) . . ?
C26 N20 C25 119.2(5) . . ?
C27 N21 C28 120.1(6) . . ?
C27 N21 C29 122.3(8) . . ?
C28 N21 C29 117.6(8) . . ?
C30 N22 C32 120.2(6) . . ?
C30 N22 C31 121.9(6) . . ?
C32 N22 C31 117.9(7) . . ?
N4 C1 N1 110.8(4) . . ?
N4 C1 C2 123.0(4) . . ?
N1 C1 C2 126.0(3) . . ?
C1 C2 C9 109.6(3) . . ?
C1 C2 C11 108.4(3) . . ?
C9 C2 C11 109.1(3) . . ?
C1 C2 C3 111.3(3) . . ?
C9 C2 C3 109.0(3) . . ?
C11 C2 C3 109.5(3) . . ?
C4 C3 C2 110.0(3) . . ?
C4 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C3 C4 C12 111.8(3) . . ?
C3 C4 C5 109.2(3) . . ?
C12 C4 C5 108.6(3) . . ?
C3 C4 C10 109.1(3) . . ?
C12 C4 C10 109.4(3) . . ?
C5 C4 C10 108.5(3) . . ?
C4 C5 C6 110.8(3) . . ?
C4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C13 C6 C11 110.6(3) . . ?
C13 C6 C7 109.1(3) . . ?
C11 C6 C7 108.8(3) . . ?
C13 C6 C5 110.2(3) . . ?
C11 C6 C5 109.1(3) . . ?
C7 C6 C5 108.9(3) . . ?
C6 C7 C8 110.2(3) . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C14 C8 C9 110.6(3) . . ?
C14 C8 C10 111.3(3) . . ?
C9 C8 C10 109.1(3) . . ?
C14 C8 C7 107.5(3) . . ?
C9 C8 C7 108.8(3) . . ?
C10 C8 C7 109.4(3) . . ?
C8 C9 C2 110.0(3) . . ?
C8 C9 H9A 109.7 . . ?
C2 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 . . ?
C2 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C4 C10 C8 110.5(3) . . ?
C4 C10 H10A 109.6 . . ?
C8 C10 H10A 109.6 . . ?
C4 C10 H10B 109.6 . . ?
C8 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C6 C11 C2 110.2(3) . . ?
C6 C11 H11A 109.6 . . ?
C2 C11 H11A 109.6 . . ?
C6 C11 H11B 109.6 . . ?
C2 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N8 C12 N5 110.4(4) . . ?
N8 C12 C4 122.8(4) . . ?
N5 C12 C4 126.7(4) . . ?
N9 C13 N12 111.7(3) . . ?
N9 C13 C6 123.5(4) . . ?
N12 C13 C6 124.8(4) . . ?
N16 C14 N13 111.2(3) . . ?
N16 C14 C8 123.9(4) . . ?
N13 C14 C8 124.7(4) . . ?
O1 C15 N17 123.6(5) . . ?
O1 C15 H15 118.2 . . ?
N17 C15 H15 118.2 . . ?
N17 C16 H16A 109.5 . . ?
N17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N17 C17 H17A 109.5 . . ?
N17 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N17 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C18 N18 123.7(4) . . ?
O2 C18 H18 118.2 . . ?
N18 C18 H18 118.2 . . ?
N18 C19 H19A 109.5 . . ?
N18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N18 C20 H20A 109.5 . . ?
N18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 N19 124.8(5) . . ?
O3 C21 H21 117.6 . . ?
N19 C21 H21 117.6 . . ?
N19 C22 H22A 109.5 . . ?
N19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N19 C23 H23A 109.5 . . ?
N19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O4 C24 N20 124.7(5) . . ?
O4 C24 H24 117.7 . . ?
N20 C24 H24 117.7 . . ?
N20 C25 H25A 109.5 . . ?
N20 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N20 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N20 C26 H26A 109.5 . . ?
N20 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N20 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O5 C27 N21 127.2(8) . . ?
O5 C27 H27 116.4 . . ?
N21 C27 H27 116.4 . . ?
N21 C28 H28A 109.5 . . ?
N21 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N21 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N21 C29 H29A 109.5 . . ?
N21 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N21 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O6 C30 N22 123.4(6) . . ?
O6 C30 H30 118.3 . . ?
N22 C30 H30 118.3 . . ?
N22 C31 H31A 109.5 . . ?
N22 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N22 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N22 C32 H32A 109.5 . . ?
N22 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N22 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

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
O2 Zn3 O1 C15 31.2(4) . . . . ?
O4 Zn3 O1 C15 -151.0(4) . . . . ?
N3 Zn3 O1 C15 119.3(4) . . . . ?
N7 Zn3 O1 C15 -59.7(4) 4_665 . . . ?
O3 Zn3 O2 C18 67.2(4) . . . . ?
O1 Zn3 O2 C18 -115.0(4) . . . . ?
N3 Zn3 O2 C18 153.0(4) . . . . ?
N7 Zn3 O2 C18 -27.6(4) 4_665 . . . ?
O2 Zn3 O3 C21 -113.0(5) . . . . ?
O4 Zn3 O3 C21 69.3(5) . . . . ?
N3 Zn3 O3 C21 159.0(5) . . . . ?
N7 Zn3 O3 C21 -22.0(5) 4_665 . . . ?
O3 Zn3 O4 C24 161.4(4) . . . . ?
O1 Zn3 O4 C24 -16.4(4) . . . . ?
N3 Zn3 O4 C24 75.5(4) . . . . ?
N7 Zn3 O4 C24 -103.8(4) 4_665 . . . ?
N10 Zn1 N1 C1 -31.4(5) 3_657 . . . ?
N14 Zn1 N1 C1 80.1(5) 4_565 . . . ?
Cl1 Zn1 N1 C1 -152.5(4) . . . . ?
N10 Zn1 N1 N2 146.1(3) 3_657 . . . ?
N14 Zn1 N1 N2 -102.5(3) 4_565 . . . ?
Cl1 Zn1 N1 N2 25.0(3) . . . . ?
C1 N1 N2 N3 0.8(4) . . . . ?
Zn1 N1 N2 N3 -177.5(3) . . . . ?
N1 N2 N3 N4 0.3(5) . . . . ?
N1 N2 N3 Zn3 177.3(3) . . . . ?
O2 Zn3 N3 N2 -18.0(4) . . . . ?
O4 Zn3 N3 N2 164.0(4) . . . . ?
O3 Zn3 N3 N2 72.5(4) . . . . ?
O1 Zn3 N3 N2 -106.7(4) . . . . ?
O2 Zn3 N3 N4 158.6(3) . . . . ?
O4 Zn3 N3 N4 -19.3(3) . . . . ?
O3 Zn3 N3 N4 -110.8(3) . . . . ?
O1 Zn3 N3 N4 70.0(3) . . . . ?
N2 N3 N4 C1 -1.3(5) . . . . ?
Zn3 N3 N4 C1 -178.4(3) . . . . ?
N15 Zn2 N5 C12 -79.5(5) 4_565 . . . ?
N11 Zn2 N5 C12 32.9(5) 3_657 . . . ?
Cl2 Zn2 N5 C12 151.6(4) . . . . ?
N15 Zn2 N5 N6 103.0(3) 4_565 . . . ?
N11 Zn2 N5 N6 -144.6(3) 3_657 . . . ?
Cl2 Zn2 N5 N6 -25.9(3) . . . . ?
C12 N5 N6 N7 -0.8(4) . . . . ?
Zn2 N5 N6 N7 177.5(3) . . . . ?
N5 N6 N7 N8 0.3(5) . . . . ?
N5 N6 N7 Zn3 -179.7(3) . . . 4_566 ?
N6 N7 N8 C12 0.4(5) . . . . ?
Zn3 N7 N8 C12 -179.6(3) 4_566 . . . ?
C13 N9 N10 N11 -0.4(5) . . . . ?
C13 N9 N10 Zn1 173.7(3) . . . 3_657 ?
N9 N10 N11 N12 0.2(6) . . . . ?
Zn1 N10 N11 N12 -173.5(3) 3_657 . . . ?
N9 N10 N11 Zn2 177.7(3) . . . 3_657 ?
Zn1 N10 N11 Zn2 4.1(7) 3_657 . . 3_657 ?
N10 N11 N12 C13 0.2(5) . . . . ?
Zn2 N11 N12 C13 -177.6(3) 3_657 . . . ?
C14 N13 N14 N15 0.6(5) . . . . ?
C14 N13 N14 Zn1 -179.1(3) . . . 4_666 ?
N13 N14 N15 N16 -0.3(6) . . . . ?
Zn1 N14 N15 N16 179.4(3) 4_666 . . . ?
N13 N14 N15 Zn2 174.7(3) . . . 4_666 ?
Zn1 N14 N15 Zn2 -5.6(6) 4_666 . . 4_666 ?
N14 N15 N16 C14 -0.2(5) . . . . ?
Zn2 N15 N16 C14 -175.3(3) 4_666 . . . ?
N3 N4 C1 N1 1.8(5) . . . . ?
N3 N4 C1 C2 176.6(4) . . . . ?
N2 N1 C1 N4 -1.7(5) . . . . ?
Zn1 N1 C1 N4 175.9(3) . . . . ?
N2 N1 C1 C2 -176.3(4) . . . . ?
Zn1 N1 C1 C2 1.3(7) . . . . ?
N4 C1 C2 C9 18.6(5) . . . . ?
N1 C1 C2 C9 -167.4(4) . . . . ?
N4 C1 C2 C11 -100.3(4) . . . . ?
N1 C1 C2 C11 73.7(5) . . . . ?
N4 C1 C2 C3 139.3(4) . . . . ?
N1 C1 C2 C3 -46.7(5) . . . . ?
C1 C2 C3 C4 179.1(3) . . . . ?
C9 C2 C3 C4 -59.9(4) . . . . ?
C11 C2 C3 C4 59.3(4) . . . . ?
C2 C3 C4 C12 -179.3(3) . . . . ?
C2 C3 C4 C5 -59.0(4) . . . . ?
C2 C3 C4 C10 59.4(4) . . . . ?
C3 C4 C5 C6 59.2(4) . . . . ?
C12 C4 C5 C6 -178.5(3) . . . . ?
C10 C4 C5 C6 -59.6(4) . . . . ?
C4 C5 C6 C13 179.3(3) . . . . ?
C4 C5 C6 C11 -59.1(4) . . . . ?
C4 C5 C6 C7 59.6(4) . . . . ?
C13 C6 C7 C8 -179.1(3) . . . . ?
C11 C6 C7 C8 60.1(4) . . . . ?
C5 C6 C7 C8 -58.7(4) . . . . ?
C6 C7 C8 C14 -179.9(3) . . . . ?
C6 C7 C8 C9 -60.0(4) . . . . ?
C6 C7 C8 C10 59.1(4) . . . . ?
C14 C8 C9 C2 177.6(3) . . . . ?
C10 C8 C9 C2 -59.7(4) . . . . ?
C7 C8 C9 C2 59.7(4) . . . . ?
C1 C2 C9 C8 -178.1(3) . . . . ?
C11 C2 C9 C8 -59.6(4) . . . . ?
C3 C2 C9 C8 59.9(4) . . . . ?
C3 C4 C10 C8 -59.4(4) . . . . ?
C12 C4 C10 C8 177.9(3) . . . . ?
C5 C4 C10 C8 59.5(4) . . . . ?
C14 C8 C10 C4 -178.3(3) . . . . ?
C9 C8 C10 C4 59.3(4) . . . . ?
C7 C8 C10 C4 -59.6(4) . . . . ?
C13 C6 C11 C2 -179.7(3) . . . . ?
C7 C6 C11 C2 -59.9(4) . . . . ?
C5 C6 C11 C2 58.8(4) . . . . ?
C1 C2 C11 C6 179.1(3) . . . . ?
C9 C2 C11 C6 59.9(4) . . . . ?
C3 C2 C11 C6 -59.3(4) . . . . ?
N7 N8 C12 N5 -0.9(4) . . . . ?
N7 N8 C12 C4 -177.1(4) . . . . ?
N6 N5 C12 N8 1.1(4) . . . . ?
Zn2 N5 C12 N8 -176.4(3) . . . . ?
N6 N5 C12 C4 177.1(4) . . . . ?
Zn2 N5 C12 C4 -0.5(7) . . . . ?
C3 C4 C12 N8 -138.5(4) . . . . ?
C5 C4 C12 N8 100.9(4) . . . . ?
C10 C4 C12 N8 -17.4(5) . . . . ?
C3 C4 C12 N5 46.0(5) . . . . ?
C5 C4 C12 N5 -74.6(5) . . . . ?
C10 C4 C12 N5 167.1(4) . . . . ?
N10 N9 C13 N12 0.5(4) . . . . ?
N10 N9 C13 C6 -177.1(3) . . . . ?
N11 N12 C13 N9 -0.4(4) . . . . ?
N11 N12 C13 C6 177.1(3) . . . . ?
C11 C6 C13 N9 -149.3(4) . . . . ?
C7 C6 C13 N9 91.1(4) . . . . ?
C5 C6 C13 N9 -28.5(5) . . . . ?
C11 C6 C13 N12 33.4(5) . . . . ?
C7 C6 C13 N12 -86.2(4) . . . . ?
C5 C6 C13 N12 154.2(4) . . . . ?
N15 N16 C14 N13 0.6(4) . . . . ?
N15 N16 C14 C8 175.6(3) . . . . ?
N14 N13 C14 N16 -0.7(4) . . . . ?
N14 N13 C14 C8 -175.7(3) . . . . ?
C9 C8 C14 N16 148.7(4) . . . . ?
C10 C8 C14 N16 27.2(5) . . . . ?
C7 C8 C14 N16 -92.6(4) . . . . ?
C9 C8 C14 N13 -37.0(5) . . . . ?
C10 C8 C14 N13 -158.5(4) . . . . ?
C7 C8 C14 N13 81.7(4) . . . . ?
Zn3 O1 C15 N17 149.5(4) . . . . ?
C16 N17 C15 O1 -3.0(7) . . . . ?
C17 N17 C15 O1 -179.7(5) . . . . ?
Zn3 O2 C18 N18 -171.1(4) . . . . ?
C20 N18 C18 O2 -178.5(5) . . . . ?
C19 N18 C18 O2 -2.4(8) . . . . ?
Zn3 O3 C21 N19 -175.4(4) . . . . ?
C23 N19 C21 O3 -175.7(5) . . . . ?
C22 N19 C21 O3 2.5(9) . . . . ?
Zn3 O4 C24 N20 -145.3(4) . . . . ?
C26 N20 C24 O4 -178.6(5) . . . . ?
C25 N20 C24 O4 4.3(7) . . . . ?
C28 N21 C27 O5 -2.2(11) . . . . ?
C29 N21 C27 O5 178.2(8) . . . . ?
C32 N22 C30 O6 -178.8(6) . . . . ?
C31 N22 C30 O6 1.4(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.102


_iucr_refine_instruction_details 
;
#---------------------------------------------------------
 


TITL pn041 in P21/n (14) sir97
CELL  0.71073   15.7345   20.5801   15.7442    90.000   112.118    90.000
ZERR  4          0.0005    0.0004    0.0004     0.000     0.001     0.000
LATT   1
SYMM     0.50000 - X ,    0.50000 + Y ,    0.50000 - Z
SFAC  C  H Cl  N  O Zn
UNIT   128  216   8  88  24  12
OMIT   3   6   0
OMIT  -6   6   9
OMIT   0   6   3
OMIT  -2   1   3
OMIT   3  12   6
OMIT   6  12   3
OMIT  -2   5   1
 
TWIN  0 0 1 0 1 0 1 0 0
L.S.     10
FMAP 2
PLAN -20
ACTA
BOND $H
CONF
TEMP  -150
WGHT    0.063000    5.876101
BASF   0.43774
FVAR       0.20594
ZN1   6    0.353710    0.091742    0.712135    11.00000    0.01894    0.01425 =
         0.02043    0.00212    0.01016    0.00099
ZN2   6    0.203492    0.089499    0.856047    11.00000    0.01822    0.01388 =
         0.01880    0.00102    0.00953    0.00194
ZN3   6    0.627628    0.255193    0.636531    11.00000    0.02219    0.02068 =
         0.02091    0.00225    0.01258   -0.00153
CL1   3    0.339950    0.027172    0.597441    11.00000    0.04939    0.02479 =
         0.02654   -0.00450    0.01582    0.00380
CL2   3    0.088970    0.025061    0.851091    11.00000    0.02743    0.02662 =
         0.04289    0.00128    0.01895   -0.00545
O1    5    0.741991    0.196723    0.707043    11.00000    0.02921    0.02899 =
         0.03417    0.00787    0.01934    0.00476
O2    5    0.577304    0.181184    0.542032    11.00000    0.03987    0.03371 =
         0.03070   -0.00905    0.02165   -0.00847
O3    5    0.510821    0.310679    0.568187    11.00000    0.04066    0.03998 =
         0.03802    0.01633    0.02007    0.01290
O4    5    0.679303    0.325850    0.736618    11.00000    0.04064    0.02447 =
         0.03345   -0.00760    0.01908   -0.01238
O5    5    0.736467    0.187444    0.348223    11.00000    0.07516    0.06052 =
         0.06926   -0.00946    0.01687   -0.01130
O6    5    0.229913    0.490137    0.161314    11.00000    0.10107    0.04904 =
         0.07573    0.01031    0.06592    0.01852
N1    4    0.455490    0.157639    0.748766    11.00000    0.01863    0.02135 =
         0.01971    0.00222    0.00972   -0.00010
N2    4    0.482723    0.173882    0.679687    11.00000    0.02208    0.02319 =
         0.01948    0.00384    0.01339   -0.00074
N3    4    0.550458    0.214374    0.711970    11.00000    0.02112    0.02009 =
         0.02024   -0.00108    0.01253   -0.00349
N4    4    0.571417    0.226495    0.801628    11.00000    0.02398    0.01631 =
         0.01984    0.00166    0.01197   -0.00295
N5    4    0.243240    0.152565    0.960415    11.00000    0.01768    0.01653 =
         0.02243   -0.00096    0.01165   -0.00092
N6    4    0.173424    0.166089    0.988887    11.00000    0.02118    0.01945 =
         0.02519   -0.00337    0.01302    0.00156
N7    4    0.206784    0.205178    1.058724    11.00000    0.01696    0.02179 =
         0.02310   -0.00332    0.01192    0.00172
N8    4    0.296792    0.218474    1.077607    11.00000    0.01586    0.02515 =
         0.02376   -0.00482    0.01275   -0.00098
N9    4    0.580797    0.021007    1.162308    11.00000    0.02154    0.01272 =
         0.02312    0.00349    0.01331    0.00312
N10   4    0.638806   -0.029452    1.184346    11.00000    0.01941    0.01436 =
         0.02255    0.00429    0.01171    0.00372
N11   4    0.691650   -0.027426    1.137038    11.00000    0.02066    0.00935 =
         0.02320    0.00135    0.00934    0.00190
N12   4    0.670922    0.024155    1.082464    11.00000    0.02050    0.01354 =
         0.02038    0.00454    0.00902    0.00425
N13   4    0.704058    0.315013    1.125681    11.00000    0.02717    0.01770 =
         0.02329   -0.00744    0.01465   -0.00724
N14   4    0.736246    0.357460    1.193260    11.00000    0.02082    0.01835 =
         0.02059   -0.00408    0.00991   -0.00448
N15   4    0.681759    0.359513    1.239686    11.00000    0.02136    0.01439 =
         0.02111   -0.00336    0.01034   -0.00389
N16   4    0.611954    0.318283    1.202859    11.00000    0.02371    0.02071 =
         0.02263   -0.00539    0.01287   -0.00666
N17   4    0.863497    0.139838    0.700117    11.00000    0.03115    0.03179 =
         0.04184    0.00435    0.01693    0.00518
N18   4    0.520934    0.131547    0.405424    11.00000    0.04400    0.03315 =
         0.02870   -0.00764    0.01695   -0.00220
N19   4    0.411824    0.389885    0.491091    11.00000    0.03286    0.04368 =
         0.03473    0.00315    0.01550    0.01321
N20   4    0.747380    0.338067    0.890471    11.00000    0.03600    0.03309 =
         0.04096   -0.00685    0.01952   -0.00863
N21   4    0.837402    0.107481    0.342368    11.00000    0.06158    0.06729 =
         0.08106   -0.01454    0.02480   -0.00612
N22   4    0.183870    0.500149    0.279975    11.00000    0.04635    0.02710 =
         0.04747    0.00239    0.02957    0.00214
C1    1    0.509988    0.191420    0.822168    11.00000    0.01641    0.01547 =
         0.02023    0.00185    0.01056   -0.00049
C2    1    0.510065    0.187044    0.916779    11.00000    0.01490    0.01481 =
         0.01538    0.00039    0.00815    0.00007
C3    1    0.410870    0.189786    0.915646    11.00000    0.01455    0.01368 =
         0.01939    0.00164    0.01015    0.00162
AFIX  23
H3A   2    0.381593    0.231329    0.888186    11.00000   -1.20000
H3B   2    0.374054    0.153820    0.877671    11.00000   -1.20000
AFIX   0
C4    1    0.413093    0.184077    1.013104    11.00000    0.01741    0.01179 =
         0.02173   -0.00285    0.01220   -0.00110
C5    1    0.459147    0.119497    1.055307    11.00000    0.01152    0.00949 =
         0.01848   -0.00008    0.00508   -0.00032
AFIX  23
H5A   2    0.422793    0.082783    1.018871    11.00000   -1.20000
H5B   2    0.460626    0.115571    1.118518    11.00000   -1.20000
AFIX   0
C6    1    0.558403    0.115965    1.057287    11.00000    0.01737    0.00962 =
         0.01580    0.00100    0.00695    0.00118
C7    1    0.614289    0.172930    1.114641    11.00000    0.01751    0.01055 =
         0.01640   -0.00026    0.00849    0.00287
AFIX  23
H7A   2    0.677620    0.171383    1.115849    11.00000   -1.20000
H7B   2    0.617526    0.169149    1.178473    11.00000   -1.20000
AFIX   0
C8    1    0.569185    0.238245    1.073337    11.00000    0.01792    0.01168 =
         0.01826   -0.00031    0.00999   -0.00110
C9    1    0.565961    0.243613    0.975072    11.00000    0.01440    0.01542 =
         0.01961    0.00006    0.00976   -0.00060
AFIX  23
H9A   2    0.629107    0.242594    0.975717    11.00000   -1.20000
H9B   2    0.537504    0.285437    0.947904    11.00000   -1.20000
AFIX   0
C10   1    0.470355    0.240338    1.071380    11.00000    0.01519    0.01028 =
         0.02008   -0.00100    0.00872   -0.00003
AFIX  23
H10A  2    0.471923    0.236994    1.134682    11.00000   -1.20000
H10B  2    0.441456    0.282299    1.045357    11.00000   -1.20000
AFIX   0
C11   1    0.555471    0.122125    0.959700    11.00000    0.01972    0.01241 =
         0.01998   -0.00167    0.01281   -0.00031
AFIX  23
H11A  2    0.520227    0.085434    0.922171    11.00000   -1.20000
H11B  2    0.618612    0.120243    0.960427    11.00000   -1.20000
AFIX   0
C12   1    0.316750    0.185759    1.015175    11.00000    0.01440    0.01473 =
         0.01806    0.00421    0.00824    0.00312
C13   1    0.602614    0.053433    1.099524    11.00000    0.01892    0.01260 =
         0.01712   -0.00202    0.00873   -0.00027
C14   1    0.626921    0.291590    1.132118    11.00000    0.01821    0.01017 =
         0.02171    0.00162    0.00906    0.00038
C15   1    0.775927    0.155401    0.668851    11.00000    0.03508    0.02700 =
         0.03587    0.00781    0.01554    0.00489
AFIX  43
H15   2    0.735917    0.134562    0.614723    11.00000   -1.20000
AFIX   0
C16   1    0.928757    0.171552    0.779007    11.00000    0.04274    0.04268 =
         0.05452    0.00703    0.02569    0.00616
AFIX 137
H16A  2    0.941146    0.215342    0.762074    11.00000   -1.50000
H16B  2    0.985899    0.146474    0.801524    11.00000   -1.50000
H16C  2    0.903756    0.174479    0.827254    11.00000   -1.50000
AFIX   0
C17   1    0.898025    0.092150    0.652487    11.00000    0.03971    0.03304 =
         0.05759    0.00260    0.02342    0.01080
AFIX 137
H17A  2    0.846390    0.072418    0.602663    11.00000   -1.50000
H17B  2    0.932099    0.058322    0.695705    11.00000   -1.50000
H17C  2    0.938784    0.113670    0.627091    11.00000   -1.50000
AFIX   0
C18   1    0.564206    0.179212    0.460160    11.00000    0.03655    0.02547 =
         0.03477   -0.00370    0.01665   -0.00521
AFIX  43
H18   2    0.586600    0.214092    0.434938    11.00000   -1.20000
AFIX   0
C19   1    0.487907    0.075310    0.439885    11.00000    0.07054    0.03157 =
         0.05895   -0.01508    0.04206   -0.01336
AFIX 137
H19A  2    0.500777    0.081145    0.505344    11.00000   -1.50000
H19B  2    0.519079    0.036154    0.431076    11.00000   -1.50000
H19C  2    0.421617    0.070745    0.406450    11.00000   -1.50000
AFIX   0
C20   1    0.510305    0.132035    0.311048    11.00000    0.08180    0.04896 =
         0.03631   -0.00893    0.02669   -0.00243
AFIX 137
H20A  2    0.541048    0.170335    0.298999    11.00000   -1.50000
H20B  2    0.444896    0.133491    0.272171    11.00000   -1.50000
H20C  2    0.537695    0.092611    0.297359    11.00000   -1.50000
AFIX   0
C21   1    0.493892    0.361141    0.524241    11.00000    0.03713    0.03567 =
         0.03929    0.00294    0.02288    0.00303
AFIX  43
H21   2    0.542725    0.381472    0.512775    11.00000   -1.20000
AFIX   0
C22   1    0.331579    0.365062    0.506992    11.00000    0.04692    0.04533 =
         0.08339    0.01063    0.03776    0.00692
AFIX 137
H22A  2    0.286106    0.348938    0.449166    11.00000   -1.50000
H22B  2    0.304541    0.400117    0.530702    11.00000   -1.50000
H22C  2    0.350532    0.329565    0.551720    11.00000   -1.50000
AFIX   0
C23   1    0.396604    0.447433    0.434254    11.00000    0.06432    0.05270 =
         0.05765    0.01658    0.03583    0.02835
AFIX 137
H23A  2    0.375553    0.483020    0.462813    11.00000   -1.50000
H23B  2    0.349925    0.438230    0.373538    11.00000   -1.50000
H23C  2    0.454038    0.459973    0.427970    11.00000   -1.50000
AFIX   0
C24   1    0.739988    0.312215    0.811252    11.00000    0.03875    0.03306 =
         0.03765   -0.00527    0.01703   -0.01006
AFIX  43
H24   2    0.784499    0.280898    0.811668    11.00000   -1.20000
AFIX   0
C25   1    0.676557    0.382925    0.893344    11.00000    0.04994    0.03686 =
         0.04682    0.00077    0.02809   -0.00586
AFIX 137
H25A  2    0.701911    0.426969    0.905884    11.00000   -1.50000
H25B  2    0.655486    0.369597    0.941899    11.00000   -1.50000
H25C  2    0.624764    0.382303    0.834177    11.00000   -1.50000
AFIX   0
C26   1    0.821071    0.320937    0.974498    11.00000    0.04148    0.04728 =
         0.04189   -0.00878    0.02148   -0.00647
AFIX 137
H26A  2    0.861607    0.289631    0.961622    11.00000   -1.50000
H26B  2    0.795862    0.301471    1.016803    11.00000   -1.50000
H26C  2    0.856013    0.360024    1.002391    11.00000   -1.50000
AFIX   0
C27   1    0.773333    0.134480    0.370144    11.00000    0.06725    0.06179 =
         0.05632   -0.00629    0.01080   -0.00898
AFIX  43
H27   2    0.755223    0.109394    0.411127    11.00000   -1.20000
AFIX   0
C28   1    0.866255    0.140914    0.278063    11.00000    0.07934    0.09269 =
         0.06526   -0.03134    0.02900   -0.02857
AFIX 137
H28A  2    0.854283    0.113623    0.223769    11.00000   -1.50000
H28B  2    0.932067    0.150243    0.306464    11.00000   -1.50000
H28C  2    0.832162    0.181756    0.259949    11.00000   -1.50000
AFIX   0
C29   1    0.878671    0.044428    0.375332    11.00000    0.09821    0.07278 =
         0.14381   -0.00357    0.04975    0.01502
AFIX 137
H29A  2    0.840402    0.020623    0.401564    11.00000   -1.50000
H29B  2    0.940068    0.050659    0.422455    11.00000   -1.50000
H29C  2    0.883313    0.019572    0.324160    11.00000   -1.50000
AFIX   0
C30   1    0.235736    0.516407    0.233603    11.00000    0.04684    0.03020 =
         0.07043    0.01426    0.03005    0.00372
AFIX  43
H30   2    0.279655    0.550059    0.257377    11.00000   -1.20000
AFIX   0
C31   1    0.116990    0.448606    0.249802    11.00000    0.04674    0.06560 =
         0.08830    0.03565    0.01291   -0.00926
AFIX 137
H31A  2    0.057645    0.464473    0.248097    11.00000   -1.50000
H31B  2    0.137074    0.411946    0.292464    11.00000   -1.50000
H31C  2    0.110825    0.434390    0.188350    11.00000   -1.50000
AFIX   0
C32   1    0.193411    0.533773    0.362825    11.00000    0.12599    0.09125 =
         0.04352   -0.00289    0.02779    0.06615
AFIX 137
H32A  2    0.202396    0.502172    0.412021    11.00000   -1.50000
H32B  2    0.137863    0.559212    0.353053    11.00000   -1.50000
H32C  2    0.246495    0.562918    0.380035    11.00000   -1.50000
HKLF 4
 
REM  pn041 in P21/n (14) sir97
REM R1 =  0.0445 for   9210 Fo > 4sig(Fo)  and  0.0578 for all  10695 data
REM    599 parameters refined using      0 restraints
 
END
 
WGHT      0.0630      5.8626
REM Highest difference peak  0.839,  deepest hole -0.755,  1-sigma level  0.102
Q1    1   0.3107  0.0584  0.6617  11.00000  0.05    0.84
Q2    1   0.1593  0.0615  0.8058  11.00000  0.05    0.81
Q3    1   0.3033  0.0940  0.6582  11.00000  0.05    0.80
Q4    1   0.5758  0.2530  0.5819  11.00000  0.05    0.79
Q5    1   0.2593  0.0920  0.9134  11.00000  0.05    0.71
Q6    1   0.6848  0.2566  0.6927  11.00000  0.05    0.68
Q7    1   0.4020  0.0917  0.7672  11.00000  0.05    0.64
Q8    1   0.3612  0.0676  0.8018  11.00000  0.05    0.47
Q9    1   0.4785  0.2499  0.7806  11.00000  0.05    0.47
Q10   1   0.5572  0.4084  0.5023  11.00000  0.05    0.46
;
_database_code_depnum_ccdc_archive 'CCDC 991449'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(4)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
poly[[bis-(N,N-dimethylformamide)-tetrakis(methanol)-(μ₆-
1,3,5,7-tetrakis(5-tetrazolato)adamantane-dimanganese(II)] 
N,N-dimethylformamide, bis-methanol, di-water solvate]
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C24 H42 Mn2 N18 O6, (C3 H7 N O), 2(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C29 H61 Mn2 N19 O11'
_chemical_formula_weight         961.85

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
_symmetry_Int_Tables_number      29


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

_cell_length_a                   21.439(4)
_cell_length_b                   12.674(3)
_cell_length_c                   18.917(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5140.0(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    15470
_cell_measurement_theta_min      3.134
_cell_measurement_theta_max      25.350

_exptl_crystal_description       'thin platelet'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2024
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.9018
_exptl_absorpt_correction_T_max  0.9835
_exptl_absorpt_process_details   SADABS


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(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  'Kappa CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            29031
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         5.10
_diffrn_reflns_theta_max         25.32
_reflns_number_total             9208
_reflns_number_gt                6199
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------# 


_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.

 Methylene hydrogen atoms of the adamantane ligand were constrained, with 
 d(C-H) = 0.99 A and with U(iso) = 1.2U(eq)(C).

 Inspection of the residual electron density revealed several types of the 
 disorder. Non-coordinated tetrazolate group of the adamantane ligand is 
 equally disordered in such a way that two contributions adopt nearly 
 orthogonal orientations. The disorder was modelled with a set of soft 
 restraints (DFIX) for the standard ring geometry (i.e. C-N = 1.365(10) A; 
 N1-N2 and N3-N4 = 1.320(10) A; N2-N3 = 1.332(10) A) and keeping the ring 
 atoms coplanar within 0.01 A (FLAT). Similarity restraints (SIMU) were 
 also applied for the thermal motion of all ring atoms constituting two 
 components of the disorder. Two components of the disorder were refined 
 in two different PARTs.

 Atoms of the coordinated DMF and methanol ligand possess high parameters 
 for the thermal motion, which was suggestive of the disorder. In one case, 
 disorder of the coordinated DMF ligand (at Mn2 ion) was successfully 
 resolved. The refined scheme considers common O-atom (coordinated to Mn2) 
 and two 0.5 populated CH-NMe2 fragments, which were kept in two different 
 PARTs. Attempts to resolve possible disorder for second coordinated DMF 
 (at Mn1) and four methanol ligands did not afford stable model and the 
 subsequent refinement led to divirgence. In order to improve the 
 refinement stability, both DMF molecules were refined with restrained 
 (DFIX) standard geometry as follows: C-O = 1.230(10) A; 
 C(O)-N = 1.310(10) A; N-C(Me) 1.470(10) A and FLAT 0.01 restraints for 
 the planarity of C-NMe2 fragment. As well, similarity restraints 
 (SIMU, DELU) were used for the anisotropic thermal parameters. In the 
 case of coordinated methanol ligands, the C-O bond lengths were 
 restrained at 1.42(2) A, and similarity restraints for anisotropic 
 thermal values were used separately for every oxygen and corresponding 
 carbon atoms. The hydrogen atoms were added geometrically (and 
 considering 0.5 occupancy factors for the disordered DMF molecule). 
 OH-hydrogen of the coordinated methanol were not added. We note that for 
 two of the methanol ligands the positions of OH-hydrogens are evident 
 from the analysis of intermolecular O...N separations suggesting 
 convenient OH...N hydrogen bonding between these MeOH molecules and 
 non-coordinated tetrazolate groups (0.5+x, -y, z) (O...N = 2.62-2.84 A).

 Solvate DMF and methanol molecules, which populate voids of the 
 framework (total solvent accessible area is 1731 A³ per unit cell), 
 are badly disordered. We were not successful in the refinement of the 
 disorder in the solvent region of the structure. Therefore, this 
 disordered residual electron density was modelled using SQUEEZE routine 
 as it is implemented in PLATON. Four voids of 436-437 A³ were found 
 (474 e/cell) corresponding to 1 DMF,  2MeOH and 2 H2O guest molecules per 
 formula unit.  
;

_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)+(0.1197P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.32(3)
_refine_ls_number_reflns         9208
_refine_ls_number_parameters     533
_refine_ls_number_restraints     317
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0654
_refine_ls_wR_factor_ref         0.1813
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_restrained_S_all      0.979
_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
Mn1 Mn 0.31444(4) 0.55788(7) 0.19882(6) 0.0570(2) Uani 1 1 d . . .
Mn2 Mn 0.39804(3) 0.30078(6) 0.27461(6) 0.0500(2) Uani 1 1 d . . .
N1 N 0.20821(18) 0.4216(4) 0.2771(3) 0.0615(11) Uani 1 1 d . . .
N2 N 0.26858(19) 0.4245(4) 0.2579(2) 0.0582(12) Uani 1 1 d . . .
N3 N 0.29663(18) 0.3404(4) 0.2842(3) 0.0619(12) Uani 1 1 d . . .
N4 N 0.25617(19) 0.2834(4) 0.3187(2) 0.0624(13) Uani 1 1 d . . .
N5 N -0.0290(2) 0.5035(4) 0.3378(2) 0.0585(11) Uani 1 1 d . . .
N6 N -0.0808(2) 0.5317(4) 0.3014(2) 0.0530(11) Uani 1 1 d . . .
N7 N -0.10530(19) 0.4430(4) 0.2768(3) 0.0570(11) Uani 1 1 d . . .
N8 N -0.0730(2) 0.3593(4) 0.2961(2) 0.0559(11) Uani 1 1 d . . .
N9 N 0.1337(2) 0.4348(4) 0.5644(2) 0.0620(12) Uani 1 1 d . . .
N10 N 0.1350(2) 0.4334(4) 0.6365(2) 0.0591(12) Uani 1 1 d . . .
N11 N 0.1065(2) 0.3473(4) 0.6599(2) 0.0605(12) Uani 1 1 d . . .
N12 N 0.0850(2) 0.2908(4) 0.6067(2) 0.0636(13) Uani 1 1 d . . .
C4 C 0.0668(3) 0.0396(7) 0.3898(4) 0.098(2) Uani 0.50 1 d PDU A 1
N13 N 0.0310(5) -0.0151(7) 0.3433(6) 0.103(2) Uani 0.50 1 d PDU A 1
N14 N 0.0395(6) -0.1161(8) 0.3621(7) 0.110(3) Uani 0.50 1 d PDU A 1
N15 N 0.0782(5) -0.1230(7) 0.4172(6) 0.108(3) Uani 0.50 1 d PDU A 1
N16 N 0.0958(5) -0.0264(6) 0.4348(6) 0.097(3) Uani 0.50 1 d PDU A 1
C4A C 0.0516(4) 0.0441(6) 0.3795(5) 0.099(2) Uani 0.50 1 d PDU A 2
N13A N 0.0118(5) -0.0099(7) 0.4200(5) 0.103(2) Uani 0.50 1 d PDU A 2
N14A N 0.0069(5) -0.1047(7) 0.3936(7) 0.104(2) Uani 0.50 1 d PDU A 2
N15A N 0.0433(5) -0.1096(8) 0.3347(7) 0.107(3) Uani 0.50 1 d PDU A 2
N16A N 0.0723(5) -0.0175(7) 0.3245(5) 0.105(2) Uani 0.50 1 d PDU A 2
C1 C 0.2020(2) 0.3359(5) 0.3135(3) 0.0547(13) Uani 1 1 d . . .
C2 C -0.0265(2) 0.3991(5) 0.3334(3) 0.0496(12) Uani 1 1 d . . .
C3 C 0.1036(2) 0.3410(5) 0.5485(3) 0.0499(12) Uani 1 1 d . . .
C5 C 0.1421(2) 0.3079(4) 0.3537(3) 0.0507(12) Uani 1 1 d . . .
C6 C 0.0870(2) 0.3638(5) 0.3223(3) 0.0467(12) Uani 1 1 d . . .
H6A H 0.0819 0.3424 0.2723 0.056 Uiso 1 1 calc R . .
H6B H 0.0940 0.4410 0.3237 0.056 Uiso 1 1 calc R . .
C7 C 0.0267(2) 0.3354(5) 0.3649(3) 0.0558(13) Uani 1 1 d . . .
C8 C 0.0380(2) 0.3643(5) 0.4414(3) 0.0548(14) Uani 1 1 d . . .
H8A H 0.0441 0.4416 0.4447 0.066 Uiso 1 1 calc R . .
H8B H 0.0004 0.3462 0.4692 0.066 Uiso 1 1 calc R . .
C9 C 0.0927(2) 0.3110(4) 0.4733(3) 0.0524(13) Uani 1 1 d . . .
C10 C 0.1525(2) 0.3341(5) 0.4313(2) 0.0520(13) Uani 1 1 d . . .
H10A H 0.1637 0.4095 0.4363 0.062 Uiso 1 1 calc R . .
H10B H 0.1873 0.2912 0.4502 0.062 Uiso 1 1 calc R . .
C11 C 0.1300(2) 0.1876(5) 0.3471(3) 0.0582(14) Uani 1 1 d . A .
H11A H 0.1239 0.1690 0.2967 0.070 Uiso 1 1 calc R . .
H11B H 0.1667 0.1483 0.3648 0.070 Uiso 1 1 calc R . .
C12 C 0.0723(2) 0.1565(4) 0.3895(3) 0.0584(14) Uani 1 1 d D . .
C13 C 0.0147(2) 0.2197(5) 0.3614(3) 0.0613(14) Uani 1 1 d . A .
H13A H 0.0060 0.1992 0.3118 0.074 Uiso 1 1 calc R . .
H13B H -0.0225 0.2023 0.3901 0.074 Uiso 1 1 calc R . .
C14 C 0.0830(3) 0.1909(5) 0.4687(3) 0.0590(14) Uani 1 1 d . A .
H14A H 0.0464 0.1704 0.4975 0.071 Uiso 1 1 calc R . .
H14B H 0.1201 0.1543 0.4879 0.071 Uiso 1 1 calc R . .
O1 O 0.2379(2) 0.5604(5) 0.1227(3) 0.1088(18) Uani 1 1 d DU . .
N17 N 0.1886(4) 0.5529(8) 0.0175(4) 0.160(3) Uani 1 1 d DU . .
C15 C 0.2361(4) 0.5367(9) 0.0591(4) 0.136(3) Uani 1 1 d DU . .
H15 H 0.2720 0.5042 0.0392 0.163 Uiso 1 1 calc R . .
C16 C 0.1463(8) 0.6425(14) 0.0372(8) 0.228(6) Uani 1 1 d DU . .
H16A H 0.1139 0.6504 0.0011 0.341 Uiso 1 1 calc R . .
H16B H 0.1706 0.7078 0.0403 0.341 Uiso 1 1 calc R . .
H16C H 0.1268 0.6278 0.0830 0.341 Uiso 1 1 calc R . .
C17 C 0.1862(6) 0.5220(14) -0.0570(5) 0.200(5) Uani 1 1 d DU . .
H17A H 0.1438 0.5324 -0.0751 0.300 Uiso 1 1 calc R . .
H17B H 0.1978 0.4476 -0.0615 0.300 Uiso 1 1 calc R . .
H17C H 0.2154 0.5655 -0.0842 0.300 Uiso 1 1 calc R . .
O2 O 0.3573(4) 0.6794(5) 0.1352(3) 0.123(2) Uani 1 1 d DU . .
C20 C 0.4122(8) 0.6744(14) 0.0908(9) 0.198(5) Uani 1 1 d DU . .
H20A H 0.4254 0.6017 0.0814 0.297 Uiso 1 1 d R . .
H20B H 0.4460 0.7122 0.1146 0.297 Uiso 1 1 d R . .
H20C H 0.4025 0.7096 0.0460 0.297 Uiso 1 1 d R . .
O3 O 0.2665(3) 0.6745(5) 0.2619(5) 0.152(3) Uani 1 1 d DU . .
C30 C 0.2244(8) 0.7387(15) 0.2254(11) 0.240(6) Uani 1 1 d DU . .
H30A H 0.2049 0.7881 0.2584 0.360 Uiso 1 1 calc R . .
H30B H 0.1922 0.6947 0.2034 0.360 Uiso 1 1 calc R . .
H30C H 0.2467 0.7782 0.1887 0.360 Uiso 1 1 calc R . .
O4 O 0.3760(3) 0.1404(5) 0.2508(3) 0.1137(18) Uani 1 1 d DU . .
N19A N 0.3991(5) -0.0088(10) 0.1876(7) 0.150(4) Uani 0.50 1 d PDU B 1
C21A C 0.3956(10) 0.0928(10) 0.1998(8) 0.136(3) Uani 0.50 1 d PDU B 1
H21A H 0.4110 0.1362 0.1628 0.163 Uiso 0.50 1 calc PR B 1
C22A C 0.3978(13) -0.0822(16) 0.2482(13) 0.172(7) Uani 0.50 1 d PDU B 1
H22A H 0.3971 -0.1551 0.2308 0.258 Uiso 0.50 1 calc PR B 1
H22B H 0.3605 -0.0689 0.2767 0.258 Uiso 0.50 1 calc PR B 1
H22C H 0.4351 -0.0714 0.2773 0.258 Uiso 0.50 1 calc PR B 1
C23A C 0.4043(13) -0.0435(17) 0.1128(9) 0.162(6) Uani 0.50 1 d PDU B 1
H23A H 0.4021 -0.1206 0.1106 0.244 Uiso 0.50 1 calc PR B 1
H23B H 0.4442 -0.0196 0.0933 0.244 Uiso 0.50 1 calc PR B 1
H23C H 0.3700 -0.0130 0.0853 0.244 Uiso 0.50 1 calc PR B 1
N19B N 0.3293(7) -0.0067(9) 0.2914(7) 0.157(4) Uani 0.50 1 d PDU B 2
C21B C 0.3677(9) 0.0746(12) 0.2990(8) 0.141(4) Uani 0.50 1 d PDU B 2
H21B H 0.3895 0.0831 0.3424 0.169 Uiso 0.50 1 calc PR B 2
C22B C 0.2774(10) 0.008(2) 0.2403(14) 0.190(7) Uani 0.50 1 d PDU B 2
H22D H 0.2494 -0.0526 0.2421 0.286 Uiso 0.50 1 calc PR B 2
H22E H 0.2945 0.0155 0.1925 0.286 Uiso 0.50 1 calc PR B 2
H22F H 0.2542 0.0724 0.2526 0.286 Uiso 0.50 1 calc PR B 2
C23B C 0.3402(13) -0.1032(12) 0.3327(13) 0.175(7) Uani 0.50 1 d PDU B 2
H23D H 0.3044 -0.1506 0.3277 0.262 Uiso 0.50 1 calc PR B 2
H23E H 0.3457 -0.0848 0.3827 0.262 Uiso 0.50 1 calc PR B 2
H23F H 0.3779 -0.1385 0.3154 0.262 Uiso 0.50 1 calc PR B 2
O5 O 0.4071(2) 0.2481(5) 0.3836(2) 0.0896(15) Uani 1 1 d DU . .
C50 C 0.3844(7) 0.2891(14) 0.4421(7) 0.181(5) Uani 1 1 d DU B .
H50A H 0.3982 0.2472 0.4827 0.272 Uiso 1 1 calc R . .
H50B H 0.3387 0.2889 0.4399 0.272 Uiso 1 1 calc R . .
H50C H 0.3994 0.3618 0.4472 0.272 Uiso 1 1 calc R . .
O6 O 0.49658(18) 0.2656(4) 0.2613(3) 0.0876(14) Uani 1 1 d DU . .
C60 C 0.5487(5) 0.3255(11) 0.2317(7) 0.150(4) Uani 1 1 d DU B .
H60A H 0.5870 0.2836 0.2352 0.224 Uiso 1 1 calc R . .
H60B H 0.5539 0.3915 0.2581 0.224 Uiso 1 1 calc R . .
H60C H 0.5403 0.3416 0.1819 0.224 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
Mn1 O3 2.159(6) . ?
Mn1 O2 2.161(6) . ?
Mn1 O1 2.183(4) . ?
Mn1 N10 2.248(5) 3_554 ?
Mn1 N2 2.252(5) . ?
Mn1 N7 2.267(4) 4_565 ?
Mn2 O4 2.135(6) . ?
Mn2 O6 2.174(4) . ?
Mn2 O5 2.176(4) . ?
Mn2 N6 2.230(5) 4_565 ?
Mn2 N3 2.239(4) . ?
Mn2 N11 2.251(5) 3_554 ?
N1 C1 1.293(7) . ?
N1 N2 1.345(6) . ?
N2 N3 1.321(7) . ?
N3 N4 1.304(7) . ?
N4 C1 1.342(7) . ?
N5 C2 1.327(8) . ?
N5 N6 1.355(6) . ?
N6 N7 1.324(6) . ?
N6 Mn2 2.230(5) 4_465 ?
N7 N8 1.319(6) . ?
N7 Mn1 2.267(4) 4_465 ?
N8 C2 1.320(6) . ?
N9 N10 1.364(6) . ?
N9 C3 1.386(7) . ?
N10 N11 1.326(7) . ?
N10 Mn1 2.248(5) 3 ?
N11 N12 1.317(7) . ?
N11 Mn2 2.251(5) 3 ?
N12 C3 1.333(7) . ?
C4 N16 1.347(8) . ?
C4 N13 1.358(8) . ?
C4 C12 1.486(9) . ?
N13 N14 1.341(9) . ?
N14 N15 1.335(9) . ?
N15 N16 1.323(8) . ?
C4A N13A 1.335(8) . ?
C4A N16A 1.375(9) . ?
C4A C12 1.504(9) . ?
N13A N14A 1.306(9) . ?
N14A N15A 1.360(10) . ?
N15A N16A 1.336(9) . ?
C1 C5 1.534(7) . ?
C2 C7 1.520(8) . ?
C3 C9 1.491(8) . ?
C5 C6 1.499(7) . ?
C5 C10 1.521(7) . ?
C5 C11 1.552(8) . ?
C6 C7 1.566(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C13 1.491(8) . ?
C7 C8 1.512(7) . ?
C8 C9 1.482(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.536(7) . ?
C9 C14 1.538(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.526(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.567(8) . ?
C12 C14 1.577(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
O1 C15 1.241(7) . ?
N17 C15 1.302(7) . ?
N17 C17 1.463(8) . ?
N17 C16 1.500(8) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O2 C20 1.446(14) . ?
C20 H20A 0.9803 . ?
C20 H20B 0.9788 . ?
C20 H20C 0.9802 . ?
O3 C30 1.398(13) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O4 C21A 1.212(9) . ?
O4 C21B 1.248(9) . ?
N19A C21A 1.310(9) . ?
N19A C22A 1.477(10) . ?
N19A C23A 1.485(10) . ?
C21A H21A 0.9500 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
N19B C21B 1.327(9) . ?
N19B C23B 1.471(10) . ?
N19B C22B 1.486(10) . ?
C21B H21B 0.9500 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
O5 C50 1.316(12) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
O6 C60 1.463(10) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?

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
O3 Mn1 O2 91.3(3) . . ?
O3 Mn1 O1 89.8(2) . . ?
O2 Mn1 O1 86.7(2) . . ?
O3 Mn1 N10 178.1(3) . 3_554 ?
O2 Mn1 N10 90.2(3) . 3_554 ?
O1 Mn1 N10 91.54(19) . 3_554 ?
O3 Mn1 N2 91.8(3) . . ?
O2 Mn1 N2 175.8(2) . . ?
O1 Mn1 N2 90.6(2) . . ?
N10 Mn1 N2 86.81(17) 3_554 . ?
O3 Mn1 N7 90.3(2) . 4_565 ?
O2 Mn1 N7 92.5(2) . 4_565 ?
O1 Mn1 N7 179.1(2) . 4_565 ?
N10 Mn1 N7 88.37(17) 3_554 4_565 ?
N2 Mn1 N7 90.26(16) . 4_565 ?
O4 Mn2 O6 89.7(2) . . ?
O4 Mn2 O5 85.8(2) . . ?
O6 Mn2 O5 87.73(18) . . ?
O4 Mn2 N6 178.6(2) . 4_565 ?
O6 Mn2 N6 91.39(18) . 4_565 ?
O5 Mn2 N6 93.4(2) . 4_565 ?
O4 Mn2 N3 90.9(2) . . ?
O6 Mn2 N3 177.7(2) . . ?
O5 Mn2 N3 94.51(19) . . ?
N6 Mn2 N3 88.00(17) 4_565 . ?
O4 Mn2 N11 92.1(2) . 3_554 ?
O6 Mn2 N11 89.07(18) . 3_554 ?
O5 Mn2 N11 176.2(2) . 3_554 ?
N6 Mn2 N11 88.75(18) 4_565 3_554 ?
N3 Mn2 N11 88.71(18) . 3_554 ?
C1 N1 N2 105.5(4) . . ?
N3 N2 N1 108.3(4) . . ?
N3 N2 Mn1 126.4(3) . . ?
N1 N2 Mn1 125.1(4) . . ?
N4 N3 N2 109.4(4) . . ?
N4 N3 Mn2 124.2(4) . . ?
N2 N3 Mn2 126.3(3) . . ?
N3 N4 C1 105.4(5) . . ?
C2 N5 N6 105.2(4) . . ?
N7 N6 N5 106.3(4) . . ?
N7 N6 Mn2 130.4(3) . 4_465 ?
N5 N6 Mn2 122.2(3) . 4_465 ?
N8 N7 N6 112.2(4) . . ?
N8 N7 Mn1 125.1(3) . 4_465 ?
N6 N7 Mn1 122.3(3) . 4_465 ?
N7 N8 C2 103.7(5) . . ?
N10 N9 C3 102.4(4) . . ?
N11 N10 N9 109.6(5) . . ?
N11 N10 Mn1 128.6(3) . 3 ?
N9 N10 Mn1 121.6(4) . 3 ?
N12 N11 N10 110.7(4) . . ?
N12 N11 Mn2 125.3(4) . 3 ?
N10 N11 Mn2 123.9(4) . 3 ?
N11 N12 C3 105.5(5) . . ?
N16 C4 N13 110.7(6) . . ?
N16 C4 C12 125.8(7) . . ?
N13 C4 C12 123.5(7) . . ?
N14 N13 C4 103.8(7) . . ?
N15 N14 N13 110.8(8) . . ?
N16 N15 N14 108.2(7) . . ?
N15 N16 C4 106.5(7) . . ?
N13A C4A N16A 110.5(6) . . ?
N13A C4A C12 127.1(8) . . ?
N16A C4A C12 122.5(8) . . ?
N14A N13A C4A 107.6(8) . . ?
N13A N14A N15A 108.0(8) . . ?
N16A N15A N14A 110.2(8) . . ?
N15A N16A C4A 103.7(7) . . ?
N1 C1 N4 111.4(5) . . ?
N1 C1 C5 123.0(5) . . ?
N4 C1 C5 125.1(5) . . ?
N8 C2 N5 112.6(5) . . ?
N8 C2 C7 125.0(5) . . ?
N5 C2 C7 122.3(4) . . ?
N12 C3 N9 111.6(5) . . ?
N12 C3 C9 128.3(5) . . ?
N9 C3 C9 120.0(5) . . ?
C6 C5 C10 113.3(4) . . ?
C6 C5 C1 110.7(4) . . ?
C10 C5 C1 107.8(4) . . ?
C6 C5 C11 107.5(4) . . ?
C10 C5 C11 108.5(5) . . ?
C1 C5 C11 109.0(4) . . ?
C5 C6 C7 109.8(4) . . ?
C5 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C13 C7 C8 108.0(5) . . ?
C13 C7 C2 112.0(4) . . ?
C8 C7 C2 111.6(4) . . ?
C13 C7 C6 110.2(4) . . ?
C8 C7 C6 107.7(4) . . ?
C2 C7 C6 107.2(4) . . ?
C9 C8 C7 113.9(5) . . ?
C9 C8 H8A 108.8 . . ?
C7 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
C7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C8 C9 C3 113.3(5) . . ?
C8 C9 C10 111.2(4) . . ?
C3 C9 C10 108.3(4) . . ?
C8 C9 C14 108.8(4) . . ?
C3 C9 C14 109.1(5) . . ?
C10 C9 C14 105.8(5) . . ?
C5 C10 C9 109.6(4) . . ?
C5 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
C5 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C12 C11 C5 110.3(4) . . ?
C12 C11 H11A 109.6 . . ?
C5 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
C5 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C4 C12 C11 109.0(4) . . ?
C4A C12 C11 114.8(6) . . ?
C4 C12 C13 116.6(5) . . ?
C4A C12 C13 102.0(3) . . ?
C11 C12 C13 109.2(4) . . ?
C4 C12 C14 106.5(5) . . ?
C4A C12 C14 115.1(5) . . ?
C11 C12 C14 108.0(4) . . ?
C13 C12 C14 107.2(4) . . ?
C7 C13 C12 110.5(4) . . ?
C7 C13 H13A 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C7 C13 H13B 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C9 C14 C12 110.3(4) . . ?
C9 C14 H14A 109.6 . . ?
C12 C14 H14A 109.6 . . ?
C9 C14 H14B 109.6 . . ?
C12 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C15 O1 Mn1 131.3(5) . . ?
C15 N17 C17 124.5(7) . . ?
C15 N17 C16 116.2(7) . . ?
C17 N17 C16 114.8(7) . . ?
O1 C15 N17 124.9(7) . . ?
O1 C15 H15 117.5 . . ?
N17 C15 H15 117.5 . . ?
N17 C16 H16A 109.5 . . ?
N17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N17 C17 H17A 109.5 . . ?
N17 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N17 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C20 O2 Mn1 129.6(8) . . ?
O2 C20 H20A 112.4 . . ?
O2 C20 H20B 108.3 . . ?
H20A C20 H20B 109.3 . . ?
O2 C20 H20C 108.0 . . ?
H20A C20 H20C 109.3 . . ?
H20B C20 H20C 109.4 . . ?
C30 O3 Mn1 115.6(10) . . ?
O3 C30 H30A 109.5 . . ?
O3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C21A O4 C21B 107.4(13) . . ?
C21A O4 Mn2 124.4(8) . . ?
C21B O4 Mn2 120.8(9) . . ?
C21A N19A C22A 118.7(10) . . ?
C21A N19A C23A 117.6(10) . . ?
C22A N19A C23A 123.7(15) . . ?
O4 C21A N19A 130.5(12) . . ?
O4 C21A H21A 114.8 . . ?
N19A C21A H21A 114.8 . . ?
N19A C22A H22A 109.5 . . ?
N19A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
N19A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
N19A C23A H23A 109.5 . . ?
N19A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
N19A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C21B N19B C23B 119.3(11) . . ?
C21B N19B C22B 115.8(10) . . ?
C23B N19B C22B 124.9(15) . . ?
O4 C21B N19B 121.8(11) . . ?
O4 C21B H21B 119.1 . . ?
N19B C21B H21B 119.1 . . ?
N19B C22B H22D 109.5 . . ?
N19B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
N19B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
N19B C23B H23D 109.5 . . ?
N19B C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
N19B C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C50 O5 Mn2 130.0(8) . . ?
O5 C50 H50A 109.5 . . ?
O5 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
O5 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C60 O6 Mn2 132.9(6) . . ?
O6 C60 H60A 109.5 . . ?
O6 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
O6 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

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
C1 N1 N2 N3 -0.6(6) . . . . ?
C1 N1 N2 Mn1 -175.9(3) . . . . ?
O3 Mn1 N2 N3 -132.3(5) . . . . ?
O1 Mn1 N2 N3 137.8(5) . . . . ?
N10 Mn1 N2 N3 46.3(4) 3_554 . . . ?
N7 Mn1 N2 N3 -42.0(4) 4_565 . . . ?
O3 Mn1 N2 N1 42.1(4) . . . . ?
O1 Mn1 N2 N1 -47.7(4) . . . . ?
N10 Mn1 N2 N1 -139.2(4) 3_554 . . . ?
N7 Mn1 N2 N1 132.4(4) 4_565 . . . ?
N1 N2 N3 N4 0.9(6) . . . . ?
Mn1 N2 N3 N4 176.1(3) . . . . ?
N1 N2 N3 Mn2 -177.9(3) . . . . ?
Mn1 N2 N3 Mn2 -2.6(7) . . . . ?
O4 Mn2 N3 N4 45.6(5) . . . . ?
O5 Mn2 N3 N4 -40.3(5) . . . . ?
N6 Mn2 N3 N4 -133.6(4) 4_565 . . . ?
N11 Mn2 N3 N4 137.6(4) 3_554 . . . ?
O4 Mn2 N3 N2 -135.9(5) . . . . ?
O5 Mn2 N3 N2 138.2(5) . . . . ?
N6 Mn2 N3 N2 45.0(5) 4_565 . . . ?
N11 Mn2 N3 N2 -43.8(5) 3_554 . . . ?
N2 N3 N4 C1 -0.8(6) . . . . ?
Mn2 N3 N4 C1 178.0(4) . . . . ?
C2 N5 N6 N7 -0.9(5) . . . . ?
C2 N5 N6 Mn2 -169.7(3) . . . 4_465 ?
N5 N6 N7 N8 1.0(6) . . . . ?
Mn2 N6 N7 N8 168.5(3) 4_465 . . . ?
N5 N6 N7 Mn1 -171.3(3) . . . 4_465 ?
Mn2 N6 N7 Mn1 -3.8(6) 4_465 . . 4_465 ?
N6 N7 N8 C2 -0.6(6) . . . . ?
Mn1 N7 N8 C2 171.4(3) 4_465 . . . ?
C3 N9 N10 N11 -1.5(5) . . . . ?
C3 N9 N10 Mn1 174.5(3) . . . 3 ?
N9 N10 N11 N12 -1.0(6) . . . . ?
Mn1 N10 N11 N12 -176.7(4) 3 . . . ?
N9 N10 N11 Mn2 175.2(4) . . . 3 ?
Mn1 N10 N11 Mn2 -0.5(7) 3 . . 3 ?
N10 N11 N12 C3 3.1(6) . . . . ?
Mn2 N11 N12 C3 -173.0(4) 3 . . . ?
N16 C4 N13 N14 0.1(4) . . . . ?
C12 C4 N13 N14 179.9(3) . . . . ?
C4 N13 N14 N15 0.2(5) . . . . ?
N13 N14 N15 N16 -0.5(7) . . . . ?
N14 N15 N16 C4 0.5(7) . . . . ?
N13 C4 N16 N15 -0.4(5) . . . . ?
C12 C4 N16 N15 179.8(3) . . . . ?
N16A C4A N13A N14A 0.8(4) . . . . ?
C12 C4A N13A N14A -179.4(3) . . . . ?
C4A N13A N14A N15A -1.1(5) . . . . ?
N13A N14A N15A N16A 1.0(7) . . . . ?
N14A N15A N16A C4A -0.4(7) . . . . ?
N13A C4A N16A N15A -0.2(5) . . . . ?
C12 C4A N16A N15A 180.0(3) . . . . ?
N2 N1 C1 N4 0.1(6) . . . . ?
N2 N1 C1 C5 172.2(5) . . . . ?
N3 N4 C1 N1 0.4(6) . . . . ?
N3 N4 C1 C5 -171.5(5) . . . . ?
N7 N8 C2 N5 0.0(6) . . . . ?
N7 N8 C2 C7 -176.7(5) . . . . ?
N6 N5 C2 N8 0.6(5) . . . . ?
N6 N5 C2 C7 177.3(4) . . . . ?
N11 N12 C3 N9 -4.2(6) . . . . ?
N11 N12 C3 C9 179.3(5) . . . . ?
N10 N9 C3 N12 3.5(6) . . . . ?
N10 N9 C3 C9 -179.7(5) . . . . ?
N1 C1 C5 C6 23.6(7) . . . . ?
N4 C1 C5 C6 -165.4(5) . . . . ?
N1 C1 C5 C10 -100.8(6) . . . . ?
N4 C1 C5 C10 70.2(7) . . . . ?
N1 C1 C5 C11 141.6(5) . . . . ?
N4 C1 C5 C11 -47.4(7) . . . . ?
C10 C5 C6 C7 -57.9(6) . . . . ?
C1 C5 C6 C7 -179.1(4) . . . . ?
C11 C5 C6 C7 61.9(5) . . . . ?
N8 C2 C7 C13 -11.2(7) . . . . ?
N5 C2 C7 C13 172.4(5) . . . . ?
N8 C2 C7 C8 -132.4(5) . . . . ?
N5 C2 C7 C8 51.2(7) . . . . ?
N8 C2 C7 C6 109.8(5) . . . . ?
N5 C2 C7 C6 -66.6(6) . . . . ?
C5 C6 C7 C13 -61.1(5) . . . . ?
C5 C6 C7 C8 56.5(6) . . . . ?
C5 C6 C7 C2 176.8(4) . . . . ?
C13 C7 C8 C9 61.2(6) . . . . ?
C2 C7 C8 C9 -175.4(4) . . . . ?
C6 C7 C8 C9 -57.9(6) . . . . ?
C7 C8 C9 C3 179.5(5) . . . . ?
C7 C8 C9 C10 57.2(6) . . . . ?
C7 C8 C9 C14 -59.0(6) . . . . ?
N12 C3 C9 C8 95.8(7) . . . . ?
N9 C3 C9 C8 -80.4(6) . . . . ?
N12 C3 C9 C10 -140.3(5) . . . . ?
N9 C3 C9 C10 43.5(7) . . . . ?
N12 C3 C9 C14 -25.6(7) . . . . ?
N9 C3 C9 C14 158.2(5) . . . . ?
C6 C5 C10 C9 55.2(6) . . . . ?
C1 C5 C10 C9 178.0(5) . . . . ?
C11 C5 C10 C9 -64.0(5) . . . . ?
C8 C9 C10 C5 -52.9(6) . . . . ?
C3 C9 C10 C5 -178.0(5) . . . . ?
C14 C9 C10 C5 65.1(6) . . . . ?
C6 C5 C11 C12 -62.6(5) . . . . ?
C10 C5 C11 C12 60.2(5) . . . . ?
C1 C5 C11 C12 177.3(4) . . . . ?
N16 C4 C12 C4A -160(2) . . . . ?
N13 C4 C12 C4A 21(2) . . . . ?
N16 C4 C12 C11 84.6(7) . . . . ?
N13 C4 C12 C11 -95.1(7) . . . . ?
N16 C4 C12 C13 -151.2(7) . . . . ?
N13 C4 C12 C13 29.0(7) . . . . ?
N16 C4 C12 C14 -31.7(7) . . . . ?
N13 C4 C12 C14 148.6(7) . . . . ?
N13A C4A C12 C4 95(2) . . . . ?
N16A C4A C12 C4 -85(2) . . . . ?
N13A C4A C12 C11 164.7(6) . . . . ?
N16A C4A C12 C11 -15.5(6) . . . . ?
N13A C4A C12 C13 -77.3(6) . . . . ?
N16A C4A C12 C13 102.4(6) . . . . ?
N13A C4A C12 C14 38.4(6) . . . . ?
N16A C4A C12 C14 -141.9(6) . . . . ?
C5 C11 C12 C4 -172.7(5) . . . . ?
C5 C11 C12 C4A 172.7(4) . . . . ?
C5 C11 C12 C13 58.9(5) . . . . ?
C5 C11 C12 C14 -57.4(5) . . . . ?
C8 C7 C13 C12 -60.7(5) . . . . ?
C2 C7 C13 C12 176.1(4) . . . . ?
C6 C7 C13 C12 56.8(6) . . . . ?
C4 C12 C13 C7 179.4(4) . . . . ?
C4A C12 C13 C7 -178.5(6) . . . . ?
C11 C12 C13 C7 -56.6(6) . . . . ?
C14 C12 C13 C7 60.2(5) . . . . ?
C8 C9 C14 C12 56.7(6) . . . . ?
C3 C9 C14 C12 -179.2(4) . . . . ?
C10 C9 C14 C12 -62.9(5) . . . . ?
C4 C12 C14 C9 177.1(4) . . . . ?
C4A C12 C14 C9 -170.0(5) . . . . ?
C11 C12 C14 C9 60.2(5) . . . . ?
C13 C12 C14 C9 -57.4(5) . . . . ?
O3 Mn1 O1 C15 156.4(10) . . . . ?
O2 Mn1 O1 C15 65.1(10) . . . . ?
N10 Mn1 O1 C15 -24.9(9) 3_554 . . . ?
N2 Mn1 O1 C15 -111.8(9) . . . . ?
Mn1 O1 C15 N17 -172.0(9) . . . . ?
C17 N17 C15 O1 -178.3(13) . . . . ?
C16 N17 C15 O1 27(2) . . . . ?
O3 Mn1 O2 C20 160.0(10) . . . . ?
O1 Mn1 O2 C20 -110.3(10) . . . . ?
N10 Mn1 O2 C20 -18.7(10) 3_554 . . . ?
N7 Mn1 O2 C20 69.6(10) 4_565 . . . ?
O2 Mn1 O3 C30 61.9(11) . . . . ?
O1 Mn1 O3 C30 -24.8(11) . . . . ?
N2 Mn1 O3 C30 -115.4(11) . . . . ?
N7 Mn1 O3 C30 154.4(11) 4_565 . . . ?
O6 Mn2 O4 C21A -50.1(14) . . . . ?
O5 Mn2 O4 C21A -137.9(14) . . . . ?
N3 Mn2 O4 C21A 127.7(14) . . . . ?
N11 Mn2 O4 C21A 38.9(14) 3_554 . . . ?
O6 Mn2 O4 C21B 95.9(12) . . . . ?
O5 Mn2 O4 C21B 8.2(12) . . . . ?
N3 Mn2 O4 C21B -86.3(12) . . . . ?
N11 Mn2 O4 C21B -175.0(12) 3_554 . . . ?
C21B O4 C21A N19A 11(2) . . . . ?
Mn2 O4 C21A N19A 161.1(14) . . . . ?
C22A N19A C21A O4 -21(2) . . . . ?
C23A N19A C21A O4 159(2) . . . . ?
C21A O4 C21B N19B -59(2) . . . . ?
Mn2 O4 C21B N19B 149.6(12) . . . . ?
C23B N19B C21B O4 153(2) . . . . ?
C22B N19B C21B O4 -27(2) . . . . ?
O4 Mn2 O5 C50 -132.7(11) . . . . ?
O6 Mn2 O5 C50 137.4(11) . . . . ?
N6 Mn2 O5 C50 46.1(10) 4_565 . . . ?
N3 Mn2 O5 C50 -42.1(11) . . . . ?
O4 Mn2 O6 C60 143.2(9) . . . . ?
O5 Mn2 O6 C60 -131.0(9) . . . . ?
N6 Mn2 O6 C60 -37.7(9) 4_565 . . . ?
N11 Mn2 O6 C60 51.1(9) 3_554 . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.32
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.061


# SQUEEZE RESULTS (APPEND TO CIF)
# 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 0.181 0.042 0.053 437 119 '1 DMF + 2 methanol + 2 water'
2 0.680 -0.042 0.053 436 118 '1 DMF + 2 methanol + 2 water'
3 0.319 0.042 0.553 437 119 '1 DMF + 2 methanol + 2 water'
4 0.820 -0.042 0.553 436 118 '1 DMF + 2 methanol + 2 water'
_platon_squeeze_details          
;
;



_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL pca21 in Pca2(1)  
CELL  0.71073  21.4394  12.6738  18.9165   90.000   90.000   90.000
ZERR     4.00   0.0043   0.0025   0.0038    0.000    0.000    0.000
LATT  -1
SYMM  - X, - Y, 1/2 + Z
SYMM  1/2 - X,   Y, 1/2 + Z
SYMM  1/2 + X, - Y,   Z
SFAC  C    H    N    O    MN
UNIT  132  272  80   44   8
MERG   2
OMIT     1   3  -2
OMIT     0   0  -8
OMIT     0   0   8
OMIT     3   5   0
OMIT     8   7   0
OMIT     0   2   4
OMIT     1   3   2
TWIN
SHEL 0.80 4.0
FLAT 0.01 C12 C4 N13 N14 N15 N16
FLAT 0.01 C12 C4A N13A N14A N15A N16A
DFIX 1.365 0.01 C4 N13 C4 N16 C4A N13A C4A N16A
DFIX 1.320 0.01 N13 N14 N15 N16 N13A N14A N15A N16A
DFIX 1.332 0.01 N14 N15 N14A N15A
DFIX 2.230 0.01 N13 N16 N13A N16A
DFIX 2.130 0.01 C4 N14 C4 N15 C4A N14A C4A N15A
DFIX 2.520 0.01 C12 N13 C12 N16 C12 N13A C12 N16A
SIMU 0.008 C4 > N16A
DFIX  1.230 0.01 O1 C15
DFIX  1.310 0.01 C15 N17
DFIX  1.470 0.01 N17 C16 N17 C17
DFIX  2.405 0.01 C15 C16 C15 C17
DFIX  2.253 0.01 O1 N17
DFIX 2.500 0.01 C16 C17
SIMU  0.008 O1 > C17
DELU  0.008 O1 > C17
DFIX  1.230 0.01 O4 C21A
DFIX  1.310 0.01 C21A N19A
DFIX  1.470 0.01 N19A C22A N19A C23A
DFIX  2.405 0.01 C21A C22A C21A C23A
DFIX  2.253 0.01 O4 N19A
SIMU  0.008 O4 > C23B
DELU  0.008 O4 > C23B
DFIX  1.230 0.01 O4 C21B
DFIX  1.310 0.01 C21B N19B
DFIX  1.470 0.01 N19B C22B N19B C23B
DFIX  2.405 0.01 C21B C22B C21B C23B
DFIX  2.253 0.01 O4 N19B
FLAT  0.01 N19B C21B C22B C23B
FLAT  0.01 N19A C21A C22A C23A
DFIX  1.420 0.02 O2 C20 O3 C30 O5 C50 O6 C60
SIMU  0.008 O2 C20
DELU  0.008 O2 C20
SIMU 0.008 O3 C30
DELU 0.008 O3 C30
SIMU 0.008 O5 C50
DELU 0.008 O5 C50
SIMU 0.008 O6 C60
DELU 0.008 O6 C60
FMAP   2
PLAN   10
SIZE     0.03   0.16   0.19
ACTA
BOND   $H
CONF
LIST   4
L.S.   4
TEMP  -100.00
WGHT    0.119700
BASF   0.31601
FVAR       1.76306
MN1   5    0.314442    0.557879    0.198817    11.00000    0.04905    0.06279 =
         0.05904    0.00126   -0.01694    0.00993
MN2   5    0.398036    0.300780    0.274609    11.00000    0.04201    0.06392 =
         0.04420    0.00823   -0.00222    0.00685
N1    3    0.208211    0.421574    0.277130    11.00000    0.03707    0.08942 =
         0.05814   -0.00184   -0.00976   -0.00376
N2    3    0.268581    0.424509    0.257916    11.00000    0.03768    0.08256 =
         0.05437   -0.00063   -0.00435    0.00004
N3    3    0.296634    0.340436    0.284227    11.00000    0.03261    0.07537 =
         0.07784   -0.00235    0.01155    0.00165
N4    3    0.256172    0.283401    0.318657    11.00000    0.04071    0.09203 =
         0.05446   -0.00369   -0.00095    0.01656
N5    3   -0.029022    0.503539    0.337820    11.00000    0.05188    0.06029 =
         0.06344   -0.00152   -0.01140   -0.00633
N6    3   -0.080831    0.531657    0.301388    11.00000    0.04762    0.06815 =
         0.04321   -0.00632   -0.00825   -0.00688
N7    3   -0.105305    0.443026    0.276812    11.00000    0.04773    0.07352 =
         0.04961    0.01144   -0.01029   -0.00499
N8    3   -0.072970    0.359309    0.296061    11.00000    0.04994    0.06260 =
         0.05504    0.00137   -0.00692   -0.00812
N9    3    0.133696    0.434831    0.564411    11.00000    0.05689    0.07969 =
         0.04949   -0.00091    0.00038   -0.00269
N10   3    0.134964    0.433415    0.636490    11.00000    0.05712    0.07466 =
         0.04554    0.00660   -0.00269   -0.00224
N11   3    0.106508    0.347322    0.659891    11.00000    0.06469    0.07071 =
         0.04623    0.00860   -0.01017   -0.01005
N12   3    0.085038    0.290820    0.606736    11.00000    0.05120    0.08660 =
         0.05291    0.01572   -0.00492   -0.00534
PART 1
C4    1    0.066782    0.039648    0.389780    10.50000    0.10678    0.05091 =
         0.13667   -0.01167   -0.04447   -0.01362
N13   3    0.030976   -0.015072    0.343257    10.50000    0.10854    0.05380 =
         0.14799   -0.00782   -0.04048   -0.01614
N14   3    0.039529   -0.116054    0.362098    10.50000    0.11157    0.06221 =
         0.15515   -0.00866   -0.04215   -0.01739
N15   3    0.078192   -0.122964    0.417248    10.50000    0.11293    0.06115 =
         0.15021   -0.00159   -0.05071   -0.00151
N16   3    0.095832   -0.026386    0.434807    10.50000    0.10152    0.05088 =
         0.14008   -0.00645   -0.05341   -0.00396
PART   2
C4A   1    0.051551    0.044139    0.379496    10.50000    0.10508    0.05112 =
         0.14158   -0.01047   -0.03813   -0.01326
N13A  3    0.011832   -0.009920    0.420045    10.50000    0.11610    0.04933 =
         0.14418   -0.01301   -0.03140   -0.01989
N14A  3    0.006939   -0.104714    0.393563    10.50000    0.10695    0.05686 =
         0.14765   -0.01391   -0.03610   -0.02200
N15A  3    0.043327   -0.109566    0.334734    10.50000    0.11013    0.06110 =
         0.14964   -0.00736   -0.03912   -0.01904
N16A  3    0.072288   -0.017474    0.324504    10.50000    0.11257    0.05460 =
         0.14682   -0.01066   -0.04232   -0.02067
PART    0
C1    1    0.201986    0.335880    0.313550    11.00000    0.04095    0.07083 =
         0.05238   -0.00217   -0.00279    0.00218
C2    1   -0.026541    0.399109    0.333366    11.00000    0.03474    0.06385 =
         0.05035   -0.00985    0.00473    0.00080
C3    1    0.103596    0.341014    0.548472    11.00000    0.04272    0.06407 =
         0.04305   -0.00041    0.00053   -0.00666
C5    1    0.142079    0.307944    0.353750    11.00000    0.04154    0.06010 =
         0.05047   -0.00358    0.00306   -0.00112
C6    1    0.087034    0.363755    0.322318    11.00000    0.03732    0.05833 =
         0.04457   -0.00901    0.00313    0.00158
AFIX  23
H6A   2    0.081899    0.342375    0.272318    11.00000   -1.20000
H6B   2    0.093989    0.440951    0.323691    11.00000   -1.20000
AFIX   0
C7    1    0.026715    0.335449    0.364932    11.00000    0.04657    0.06687 =
         0.05402   -0.01207    0.00089   -0.00738
C8    1    0.038022    0.364346    0.441392    11.00000    0.04785    0.07237 =
         0.04411    0.01197   -0.00397   -0.00477
AFIX  23
H8A   2    0.044101    0.441620    0.444723    11.00000   -1.20000
H8B   2    0.000412    0.346191    0.469212    11.00000   -1.20000
AFIX   0
C9    1    0.092693    0.310954    0.473284    11.00000    0.04983    0.05342 =
         0.05386    0.00742   -0.00475    0.00109
C10   1    0.152456    0.334135    0.431331    11.00000    0.04843    0.07876 =
         0.02889   -0.00023   -0.01152   -0.00331
AFIX  23
H10A  2    0.163664    0.409547    0.436314    11.00000   -1.20000
H10B  2    0.187280    0.291245    0.450184    11.00000   -1.20000
AFIX   0
C11   1    0.130032    0.187639    0.347060    11.00000    0.04635    0.06193 =
         0.06618    0.00793   -0.01741    0.00776
AFIX  23
H11A  2    0.123869    0.168970    0.296724    11.00000   -1.20000
H11B  2    0.166718    0.148260    0.364781    11.00000   -1.20000
AFIX   0
C12   1    0.072330    0.156487    0.389470    11.00000    0.05650    0.06239 =
         0.05616    0.00270   -0.00926    0.00912
C13   1    0.014651    0.219737    0.361353    11.00000    0.05240    0.07050 =
         0.06086   -0.00946    0.00026   -0.00557
AFIX  23
H13A  2    0.006000    0.199175    0.311825    11.00000   -1.20000
H13B  2   -0.022520    0.202289    0.390120    11.00000   -1.20000
AFIX   0
C14   1    0.083029    0.190918    0.468680    11.00000    0.05205    0.07027 =
         0.05460    0.00077   -0.00145   -0.01292
AFIX  23
H14A  2    0.046445    0.170404    0.497506    11.00000   -1.20000
H14B  2    0.120120    0.154253    0.487874    11.00000   -1.20000
AFIX   0
O1    4    0.237949    0.560397    0.122698    11.00000    0.09238    0.14469 =
         0.08927   -0.01452   -0.04720    0.04385
N17   3    0.188622    0.552903    0.017495    11.00000    0.13979    0.21809 =
         0.12260   -0.04187   -0.07564    0.05823
C15   1    0.236068    0.536658    0.059061    11.00000    0.12092    0.18212 =
         0.10462   -0.02955   -0.06045    0.04374
AFIX  43
H15   2    0.271954    0.504189    0.039193    11.00000   -1.20000
AFIX   0
C16   1    0.146323    0.642512    0.037189    11.00000    0.20448    0.27955 =
         0.19892   -0.02630   -0.02315    0.11164
AFIX  33
H16A  2    0.113877    0.650411    0.001082    11.00000   -1.50000
H16B  2    0.170619    0.707840    0.040337    11.00000   -1.50000
H16C  2    0.126843    0.627815    0.083009    11.00000   -1.50000
AFIX   0
C17   1    0.186223    0.522049   -0.056960    11.00000    0.19301    0.28056 =
         0.12712   -0.06669   -0.08588    0.06098
AFIX  33
H17A  2    0.143833    0.532394   -0.075063    11.00000   -1.50000
H17B  2    0.197816    0.447562   -0.061517    11.00000   -1.50000
H17C  2    0.215413    0.565517   -0.084187    11.00000   -1.50000
AFIX   0
O2    4    0.357323    0.679423    0.135154    11.00000    0.18749    0.09189 =
         0.08888    0.05143   -0.06065   -0.04565
C20   1    0.412178    0.674388    0.090823    11.00000    0.25370    0.15463 =
         0.18479    0.03159   -0.00558   -0.05631
AFIX   3
H20A  2    0.425358    0.601676    0.081371    11.00000   -1.50000
H20B  2    0.445983    0.712216    0.114638    11.00000   -1.50000
H20C  2    0.402488    0.709581    0.046006    11.00000   -1.50000
AFIX   0
O3    4    0.266544    0.674502    0.261892    11.00000    0.09592    0.12545 =
         0.23566   -0.08056   -0.04656    0.05037
C30   1    0.224435    0.738672    0.225363    11.00000    0.20939    0.21104 =
         0.29913   -0.01389   -0.04146    0.08883
AFIX  33
H30A  2    0.204857    0.788138    0.258427    11.00000   -1.50000
H30B  2    0.192246    0.694652    0.203383    11.00000   -1.50000
H30C  2    0.246681    0.778214    0.188670    11.00000   -1.50000
AFIX   0
O4    4    0.375994    0.140362    0.250805    11.00000    0.12973    0.08740 =
         0.12391   -0.00578   -0.00807   -0.01497
PART   1
N19A  3    0.399080   -0.008793    0.187566    10.50000    0.19218    0.10394 =
         0.15297   -0.01589   -0.00437   -0.00245
C21A  1    0.395614    0.092785    0.199846    10.50000    0.17125    0.10068 =
         0.13636   -0.01143   -0.00198   -0.01122
AFIX  43
H21A  2    0.410971    0.136208    0.162795    10.50000   -1.20000
AFIX   0
C22A  1    0.397811   -0.082223    0.248213    10.50000    0.19953    0.12089 =
         0.19617    0.01493   -0.01771    0.00191
AFIX  33
H22A  2    0.397055   -0.155062    0.230845    10.50000   -1.50000
H22B  2    0.360454   -0.068883    0.276700    10.50000   -1.50000
H22C  2    0.435081   -0.071430    0.277321    10.50000   -1.50000
AFIX   0
C23A  1    0.404288   -0.043471    0.112832    10.50000    0.18907    0.12462 =
         0.17352   -0.04271    0.00227    0.00659
AFIX  33
H23A  2    0.402075   -0.120631    0.110571    10.50000   -1.50000
H23B  2    0.444216   -0.019643    0.093308    10.50000   -1.50000
H23C  2    0.370010   -0.013029    0.085288    10.50000   -1.50000
AFIX   0
PART   2
N19B  3    0.329306   -0.006660    0.291403    10.50000    0.16738    0.11351 =
         0.18972    0.00504    0.01079   -0.02975
C21B  1    0.367712    0.074636    0.299044    10.50000    0.15802    0.10307 =
         0.16225    0.00546    0.00345   -0.02215
AFIX  43
H21B  2    0.389501    0.083051    0.342409    10.50000   -1.20000
AFIX   0
C22B  1    0.277428    0.008454    0.240290    10.50000    0.18858    0.15702 =
         0.22558   -0.03869   -0.02447   -0.01494
AFIX  33
H22D  2    0.249435   -0.052613    0.242137    10.50000   -1.50000
H22E  2    0.294477    0.015503    0.192454    10.50000   -1.50000
H22F  2    0.254162    0.072438    0.252573    10.50000   -1.50000
AFIX   0
C23B  1    0.340231   -0.103216    0.332746    10.50000    0.21938    0.09764 =
         0.20773    0.00085    0.04802   -0.00446
AFIX  33
H23D  2    0.304398   -0.150628    0.327687    10.50000   -1.50000
H23E  2    0.345665   -0.084805    0.382685    10.50000   -1.50000
H23F  2    0.377906   -0.138539    0.315410    10.50000   -1.50000
AFIX   0
PART    0
O5    4    0.407090    0.248069    0.383583    11.00000    0.07944    0.12436 =
         0.06507    0.02716   -0.00998   -0.00485
C50   1    0.384407    0.289102    0.442065    11.00000    0.18072    0.23908 =
         0.12376    0.00163   -0.00916    0.01363
AFIX  33
H50A  2    0.398204    0.247164    0.482684    11.00000   -1.50000
H50B  2    0.338736    0.288949    0.439896    11.00000   -1.50000
H50C  2    0.399382    0.361759    0.447180    11.00000   -1.50000
AFIX   0
O6    4    0.496577    0.265601    0.261253    11.00000    0.05306    0.11793 =
         0.09171    0.02575    0.01341    0.00618
C60   1    0.548736    0.325526    0.231700    11.00000    0.11218    0.17944 =
         0.15720    0.02506    0.01605   -0.02236
AFIX  33
H60A  2    0.587033    0.283639    0.235209    11.00000   -1.50000
H60B  2    0.553861    0.391454    0.258141    11.00000   -1.50000
H60C  2    0.540255    0.341633    0.181949    11.00000   -1.50000
HKLF    4
 
REM  pca21 in Pca2(1)   2DMF 3MeOH guest
REM R1 =  0.0654 for   6199 Fo > 4sig(Fo)  and  0.0884 for all   9208 data
REM    533 parameters refined using    317 restraints
 
END
 
WGHT      0.1197      0.0000
REM Highest difference peak  0.379,  deepest hole -0.348,  1-sigma level  0.061
Q1    1   0.4668  0.6588  0.0779  11.00000  0.05    0.38
Q2    1   0.2217  0.8455  0.2742  11.00000  0.05    0.38
Q3    1   0.3743 -0.1434  0.1117  11.00000  0.05    0.33
Q4    1   0.3125  0.0991  0.1990  11.00000  0.05    0.32
Q5    1   0.6034  0.2985  0.2730  11.00000  0.05    0.31
Q6    1   0.2837  0.7610  0.2806  11.00000  0.05    0.30
Q7    1   0.2610 -0.0880  0.2772  11.00000  0.05    0.27
Q8    1   0.2688 -0.1331  0.2946  11.00000  0.05    0.27
Q9    1   0.0237 -0.1817  0.4549  11.00000  0.05    0.26
Q10   1   0.3884  0.7777  0.1541  11.00000  0.05    0.25

;



# start Validation Reply Form
_vrf_CHEMW03_1                   
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: The discrepancy is hence SQUEEZE was applied. 
;
_vrf_THETM01_1                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The quality of the crystal did not allowed to measure at
higher angles.
;
_vrf_PLAT220_1                   
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) Range 7.0 Ratio
RESPONSE: The disordered solvent molecules with large 
thermal displacement parameters expectedly give such a
large ratio.
;
_vrf_PLAT222_1                   
;
PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 8.3 Ratio
RESPONSE: The disordered solvent molecules with large 
thermal displacement parameters expectedly give such a
large ratio.
;
_vrf_PLAT232_1                   
;
PROBLEM: Hirshfeld Test Diff (M-X) Cu2 -- N5_* .. 12.0 su
RESPONSE: Checked and no specific problem were found. 
It was decided not to use restraints in this case. 
;
_vrf_PLAT220_2                   
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) Range 7.9 Ratio
RESPONSE: The disordered solvent molecules with large 
thermal displacement parameters expectedly give such a
large ratio.
;
_vrf_PLAT222_2                   
;
PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 9.2 Ratio
RESPONSE: The disordered solvent molecules with large 
thermal displacement parameters expectedly give such a
large ratio.
;
_vrf_PLAT250_2                   
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.2 Note
RESPONSE: A possible effect of excessive use of similarity restraints. 
;
_vrf_CHEMW03_4                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: SQUEEZE was used. The actual guest molecule content
was determined by TGA and elemental analysis.
;
_vrf_PLAT242_4                   
;
PROBLEM: Low Ueq as Compared to Neighbors for ..... Mn1 Check
RESPONSE: Checked. 
Low crystallinity of the sample, due to ongoing structural collapse might 
create a situation when the effective displacement parameters of the metal 
atoms would be significantly less compared to the atoms of the 
coordinated neighbours, especially if they are belonging to coordinated
solvent molecules.
 
;
# end Validation Reply Form

#   -------------  END of CIF  -----------------#
_database_code_depnum_ccdc_archive 'CCDC 991450'
