# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

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

data_akara13
_database_code_depnum_ccdc_archive 'CCDC 764558'
_audit_update_record             
;
2010-02-02 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;
#TrackingRef '400_web_deposit_cif_file_0_OmerANDAC_1265122864.cif'




_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Bis(2,2'-(ethylenedioxy)bis-(ethylamine))Cadmium(II) tetracyano palladate (II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H32 Cd N4 O4, C4 N4 Pd'
_chemical_formula_sum            'C16 H32 Cd N8 O4 Pd'
_chemical_formula_weight         619.30

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'
Pd Pd -0.9988 1.0072 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   18.5700(14)
_cell_length_b                   10.3191(7)
_cell_length_c                   17.2851(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 133.390(5)
_cell_angle_gamma                90.00
_cell_volume                     2407.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    82387
_cell_measurement_theta_min      1.62
_cell_measurement_theta_max      28.11

_exptl_crystal_description       prism
_exptl_crystal_colour            gray
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.463
_exptl_crystal_size_min          0.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    1.667
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.2215
_exptl_absorpt_correction_T_max  0.3948
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 24 -17 0.1650
19 -19 -10 0.1997
28 -27 -30 0.2312
0 10 17 0.2140
13 -8 -26 0.2685
-1 0 1 0.2383
28 -8 -17 0.2761
21 -5 -7 0.2743
-30 -9 -8 0.3440
-15 -8 20 0.1940
1 1 -2 0.1462
4 -4 -7 0.2440
27 5 -16 0.3135
-28 -4 9 0.3480
-30 14 13 0.3235
19 0 -9 0.3101
-2 -19 13 0.2440
-20 -15 16 0.3265
11 0 2 0.2346
-4 -2 5 0.2040
-18 4 19 0.2482

_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_measurement_details      
;
450 frames, detector distance = 100 mm
;
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_voltage           50
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_reflns_number            17480
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         27.77
_reflns_number_total             2784
_reflns_number_gt                2584
_reflns_threshold_expression     I>2σ(I)
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0520P)²+2.8955P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2784
_refine_ls_number_parameters     138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0993
_refine_ls_wR_factor_gt          0.0970
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_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
C1 C 0.3602(3) 0.4982(3) 0.4987(3) 0.0600(9) Uani 1 1 d . . .
H1A H 0.4170 0.4991 0.5062 0.072 Uiso 1 1 calc R . .
H1B H 0.3010 0.5105 0.4240 0.072 Uiso 1 1 calc R . .
C2 C 0.3547(3) 0.3696(4) 0.5354(3) 0.0617(9) Uani 1 1 d . . .
H2A H 0.2953 0.3648 0.5230 0.074 Uiso 1 1 calc R . .
H2B H 0.3533 0.2995 0.4971 0.074 Uiso 1 1 calc R . .
C3 C 0.4496(3) 0.2425(3) 0.6953(3) 0.0684(10) Uani 1 1 d . . .
H3A H 0.4415 0.1685 0.6554 0.082 Uiso 1 1 calc R . .
H3B H 0.3994 0.2381 0.6984 0.082 Uiso 1 1 calc R . .
C4 C 0.6365(3) 0.6370(4) 0.7003(3) 0.0660(9) Uani 1 1 d . . .
H4A H 0.5835 0.6405 0.6234 0.079 Uiso 1 1 calc R . .
H4B H 0.6982 0.6225 0.7185 0.079 Uiso 1 1 calc R . .
C5 C 0.6418(3) 0.7638(4) 0.7466(4) 0.0653(9) Uani 1 1 d . . .
H5A H 0.6970 0.7634 0.8233 0.078 Uiso 1 1 calc R . .
H5B H 0.6511 0.8344 0.7171 0.078 Uiso 1 1 calc R . .
C6 C 0.5478(3) 0.8942(3) 0.7633(4) 0.0670(10) Uani 1 1 d . . .
H6A H 0.5516 0.9700 0.7330 0.080 Uiso 1 1 calc R . .
H6B H 0.6034 0.8962 0.8399 0.080 Uiso 1 1 calc R . .
C7 C 0.6147(3) 1.0050(4) 0.5125(3) 0.0585(9) Uani 1 1 d . . .
C8 C 0.4550(3) 0.8246(4) 0.4331(4) 0.0662(10) Uani 1 1 d . . .
N1 N 0.3689(2) 0.6048(3) 0.5614(2) 0.0556(7) Uani 1 1 d . . .
H1C H 0.3112 0.6136 0.5443 0.067 Uiso 1 1 calc R . .
H1D H 0.3807 0.6793 0.5447 0.067 Uiso 1 1 calc R . .
N2 N 0.6185(2) 0.5286(3) 0.7409(3) 0.0555(7) Uani 1 1 d . . .
H2C H 0.6762 0.5080 0.8065 0.067 Uiso 1 1 calc R . .
H2D H 0.5991 0.4592 0.6989 0.067 Uiso 1 1 calc R . .
N3 N 0.6804(3) 1.0178(5) 0.5209(3) 0.0805(11) Uani 1 1 d . . .
N4 N 0.4251(4) 0.7246(4) 0.3959(4) 0.0971(14) Uani 1 1 d . . .
O1 O 0.44044(19) 0.3602(2) 0.6460(2) 0.0592(6) Uani 1 1 d . . .
O2 O 0.55124(19) 0.7797(2) 0.7205(2) 0.0592(6) Uani 1 1 d . . .
Pd1 Pd 0.5000 1.0000 0.5000 0.05062(13) Uani 1 2 d S . .
Cd1 Cd 0.5000 0.56733(3) 0.7500 0.04714(12) Uani 1 2 d S . .


_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
C1 N1 1.473(5) . ?
C1 C2 1.504(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O1 1.420(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O1 1.425(4) . ?
C3 C3 1.489(9) 2_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N2 1.475(5) . ?
C4 C5 1.501(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O2 1.419(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 O2 1.419(4) . ?
C6 C6 1.498(8) 2_656 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N3 1.131(5) . ?
C7 Pd1 1.989(4) . ?
C8 N4 1.139(6) . ?
C8 Pd1 1.996(4) . ?
N1 Cd1 2.408(3) . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N2 Cd1 2.346(3) . ?
N2 H2C 0.9000 . ?
N2 H2D 0.9000 . ?
O1 Cd1 2.509(2) . ?
O2 Cd1 2.576(2) . ?
Pd1 C7 1.989(4) 5_676 ?
Pd1 C8 1.996(4) 5_676 ?
Cd1 N2 2.346(3) 2_656 ?
Cd1 N1 2.408(3) 2_656 ?
Cd1 O1 2.509(2) 2_656 ?
Cd1 O2 2.576(2) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 110.7(3) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
O1 C2 C1 106.9(3) . . ?
O1 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
O1 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
O1 C3 C3 106.8(3) . 2_656 ?
O1 C3 H3A 110.4 . . ?
C3 C3 H3A 110.4 2_656 . ?
O1 C3 H3B 110.4 . . ?
C3 C3 H3B 110.4 2_656 . ?
H3A C3 H3B 108.6 . . ?
N2 C4 C5 111.2(3) . . ?
N2 C4 H4A 109.4 . . ?
C5 C4 H4A 109.4 . . ?
N2 C4 H4B 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O2 C5 C4 107.6(3) . . ?
O2 C5 H5A 110.2 . . ?
C4 C5 H5A 110.2 . . ?
O2 C5 H5B 110.2 . . ?
C4 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
O2 C6 C6 108.0(3) . 2_656 ?
O2 C6 H6A 110.1 . . ?
C6 C6 H6A 110.1 2_656 . ?
O2 C6 H6B 110.1 . . ?
C6 C6 H6B 110.1 2_656 . ?
H6A C6 H6B 108.4 . . ?
N3 C7 Pd1 174.7(4) . . ?
N4 C8 Pd1 175.4(4) . . ?
C1 N1 Cd1 112.0(2) . . ?
C1 N1 H1C 109.2 . . ?
Cd1 N1 H1C 109.2 . . ?
C1 N1 H1D 109.2 . . ?
Cd1 N1 H1D 109.2 . . ?
H1C N1 H1D 107.9 . . ?
C4 N2 Cd1 115.5(2) . . ?
C4 N2 H2C 108.4 . . ?
Cd1 N2 H2C 108.4 . . ?
C4 N2 H2D 108.4 . . ?
Cd1 N2 H2D 108.4 . . ?
H2C N2 H2D 107.5 . . ?
C2 O1 C3 115.2(3) . . ?
C2 O1 Cd1 116.2(2) . . ?
C3 O1 Cd1 119.0(2) . . ?
C6 O2 C5 113.5(3) . . ?
C6 O2 Cd1 116.7(2) . . ?
C5 O2 Cd1 110.9(2) . . ?
C7 Pd1 C7 180.000(1) . 5_676 ?
C7 Pd1 C8 85.55(16) . 5_676 ?
C7 Pd1 C8 94.45(16) 5_676 5_676 ?
C7 Pd1 C8 94.45(16) . . ?
C7 Pd1 C8 85.55(16) 5_676 . ?
C8 Pd1 C8 180.000(1) 5_676 . ?
N2 Cd1 N2 160.37(16) . 2_656 ?
N2 Cd1 N1 89.75(11) . 2_656 ?
N2 Cd1 N1 93.39(11) 2_656 2_656 ?
N2 Cd1 N1 93.39(11) . . ?
N2 Cd1 N1 89.75(11) 2_656 . ?
N1 Cd1 N1 161.51(14) 2_656 . ?
N2 Cd1 O1 77.22(10) . . ?
N2 Cd1 O1 86.03(11) 2_656 . ?
N1 Cd1 O1 130.17(9) 2_656 . ?
N1 Cd1 O1 68.21(9) . . ?
N2 Cd1 O1 86.03(10) . 2_656 ?
N2 Cd1 O1 77.22(10) 2_656 2_656 ?
N1 Cd1 O1 68.21(9) 2_656 2_656 ?
N1 Cd1 O1 130.17(9) . 2_656 ?
O1 Cd1 O1 63.11(12) . 2_656 ?
N2 Cd1 O2 68.93(10) . . ?
N2 Cd1 O2 130.51(10) 2_656 . ?
N1 Cd1 O2 87.94(9) 2_656 . ?
N1 Cd1 O2 76.26(9) . . ?
O1 Cd1 O2 128.60(8) . . ?
O1 Cd1 O2 145.68(8) 2_656 . ?
N2 Cd1 O2 130.51(10) . 2_656 ?
N2 Cd1 O2 68.93(10) 2_656 2_656 ?
N1 Cd1 O2 76.26(9) 2_656 2_656 ?
N1 Cd1 O2 87.94(9) . 2_656 ?
O1 Cd1 O2 145.68(8) . 2_656 ?
O1 Cd1 O2 128.60(8) 2_656 2_656 ?
O2 Cd1 O2 63.42(11) . 2_656 ?

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

N1 C1 C2 O1 -56.3(4) . . . . ?
N2 C4 C5 O2 -57.7(4) . . . . ?
C2 C1 N1 Cd1 50.9(4) . . . . ?
C5 C4 N2 Cd1 42.6(4) . . . . ?
C1 C2 O1 C3 -178.8(3) . . . . ?
C1 C2 O1 Cd1 35.2(4) . . . . ?
C3 C3 O1 C2 170.9(4) 2_656 . . . ?
C3 C3 O1 Cd1 -44.2(5) 2_656 . . . ?
C6 C6 O2 C5 -176.0(4) 2_656 . . . ?
C6 C6 O2 Cd1 -45.2(5) 2_656 . . . ?
C4 C5 O2 C6 177.6(3) . . . . ?
C4 C5 O2 Cd1 43.9(4) . . . . ?
C4 N2 Cd1 N2 159.4(3) . . . 2_656 ?
C4 N2 Cd1 N1 -101.2(3) . . . 2_656 ?
C4 N2 Cd1 N1 60.6(3) . . . . ?
C4 N2 Cd1 O1 127.3(3) . . . . ?
C4 N2 Cd1 O1 -169.4(3) . . . 2_656 ?
C4 N2 Cd1 O2 -13.3(2) . . . . ?
C4 N2 Cd1 O2 -29.6(3) . . . 2_656 ?
C1 N1 Cd1 N2 52.4(3) . . . . ?
C1 N1 Cd1 N2 -108.2(3) . . . 2_656 ?
C1 N1 Cd1 N1 151.8(2) . . . 2_656 ?
C1 N1 Cd1 O1 -22.4(2) . . . . ?
C1 N1 Cd1 O1 -35.3(3) . . . 2_656 ?
C1 N1 Cd1 O2 119.7(3) . . . . ?
C1 N1 Cd1 O2 -177.1(2) . . . 2_656 ?
C2 O1 Cd1 N2 -106.9(3) . . . . ?
C3 O1 Cd1 N2 108.5(3) . . . . ?
C2 O1 Cd1 N2 83.4(3) . . . 2_656 ?
C3 O1 Cd1 N2 -61.2(3) . . . 2_656 ?
C2 O1 Cd1 N1 174.5(2) . . . 2_656 ?
C3 O1 Cd1 N1 29.9(3) . . . 2_656 ?
C2 O1 Cd1 N1 -7.9(2) . . . . ?
C3 O1 Cd1 N1 -152.5(3) . . . . ?
C2 O1 Cd1 O1 161.0(3) . . . 2_656 ?
C3 O1 Cd1 O1 16.5(2) . . . 2_656 ?
C2 O1 Cd1 O2 -57.7(3) . . . . ?
C3 O1 Cd1 O2 157.7(3) . . . . ?
C2 O1 Cd1 O2 41.2(3) . . . 2_656 ?
C3 O1 Cd1 O2 -103.4(3) . . . 2_656 ?
C6 O2 Cd1 N2 -149.6(3) . . . . ?
C5 O2 Cd1 N2 -17.6(2) . . . . ?
C6 O2 Cd1 N2 33.6(3) . . . 2_656 ?
C5 O2 Cd1 N2 165.6(2) . . . 2_656 ?
C6 O2 Cd1 N1 -59.1(3) . . . 2_656 ?
C5 O2 Cd1 N1 72.9(2) . . . 2_656 ?
C6 O2 Cd1 N1 111.2(3) . . . . ?
C5 O2 Cd1 N1 -116.8(2) . . . . ?
C6 O2 Cd1 O1 158.0(2) . . . . ?
C5 O2 Cd1 O1 -70.0(3) . . . . ?
C6 O2 Cd1 O1 -103.7(3) . . . 2_656 ?
C5 O2 Cd1 O1 28.3(3) . . . 2_656 ?
C6 O2 Cd1 O2 16.6(2) . . . 2_656 ?
C5 O2 Cd1 O2 148.6(3) . . . 2_656 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1C N3 0.90 2.39 3.192(5) 149 3_445
N2 H2C N3 0.90 2.26 3.128(5) 163 4_646
N2 H2D N4 0.90 2.34 3.232(5) 171 5_666

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        27.77
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.130


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

data_omer26
_database_code_depnum_ccdc_archive 'CCDC 971718'
_audit_update_record             
;
2013-11-13 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
(2,2'-(ethylenedioxy)bis-(ethylamine))zinc(II) tetracyanidonickelate(II) 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 N6 Ni O2 Zn'
_chemical_formula_sum            'C10 H16 N6 Ni O2 Zn'
_chemical_formula_weight         376.37

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'

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

_cell_length_a                   11.4630(10)
_cell_length_b                   8.9492(8)
_cell_length_c                   14.7436(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1512.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12350
_cell_measurement_theta_min      1.78
_cell_measurement_theta_max      28.00

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.720
_exptl_crystal_size_mid          0.527
_exptl_crystal_size_min          0.320
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    2.840
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.2128
_exptl_absorpt_correction_T_max  0.4714
_exptl_absorpt_process_details   'STOE X-RED32'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 1 -28 0.1590
0 0 1 0.1450
23 6 -3 0.3370
-22 -13 25 0.3584
-19 3 12 0.3048
-14 29 -21 0.2600
-4 -5 -11 0.3026
-1 11 23 0.2340
-2 0 3 0.2800
1 -5 25 0.2257
17 -7 20 0.1918
-2 -27 -7 0.2890
-29 15 -24 0.3256
25 -7 12 0.2797
22 -13 -29 0.2744
2 -19 -28 0.2784
-10 1 -29 0.1810
24 3 -20 0.3350
-1 1 -6 0.1590
-15 7 3 0.3361


_exptl_special_details           
; 
 ? 
;

_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_voltage           50
_diffrn_source_current           45
_diffrn_source_power             2.25
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_ambient_temperature      293
_diffrn_measurement_method       'rotation method'
_diffrn_measurement_details      
; 126 frames, detector distance = 100 mm
;
_diffrn_reflns_number            7963
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         27.54
_reflns_number_total             1738
_reflns_number_gt                1431
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0313P)²+1.9615P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0092(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1738
_refine_ls_number_parameters     94
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0823
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
Ni1 Ni 0.5000 1.0000 0.0000 0.03574(17) Uani 1 2 d S . .
Zn1 Zn 0.5000 0.62233(5) 0.2500 0.03246(15) Uani 1 2 d S . .
N1 N 0.5173(2) 0.7739(3) 0.14915(16) 0.0405(6) Uani 1 1 d . . .
O1 O 0.4465(2) 0.4339(3) 0.39380(14) 0.0554(6) Uani 1 1 d . . .
C1 C 0.5118(2) 0.8606(3) 0.09273(19) 0.0374(6) Uani 1 1 d . . .
C2 C 0.6039(3) 0.8892(3) -0.0707(2) 0.0476(7) Uani 1 1 d . . .
C3 C 0.2841(3) 0.4501(6) 0.2958(3) 0.0760(13) Uani 1 1 d . . .
H3A H 0.2483 0.5323 0.3284 0.091 Uiso 1 1 calc R . .
H3B H 0.2216 0.3898 0.2706 0.091 Uiso 1 1 calc R . .
C4 C 0.3471(4) 0.3618(5) 0.3584(3) 0.0786(14) Uani 1 1 d . . .
H4A H 0.2958 0.3348 0.4081 0.094 Uiso 1 1 calc R . .
H4B H 0.3712 0.2702 0.3286 0.094 Uiso 1 1 calc R . .
C5 C 0.4389(3) 0.4830(4) 0.48464(18) 0.0436(7) Uani 1 1 d . . .
H5A H 0.4047 0.4059 0.5224 0.052 Uiso 1 1 calc R . .
H5B H 0.3907 0.5719 0.4886 0.052 Uiso 1 1 calc R . .
N2 N 0.6665(3) 0.8212(4) -0.1146(2) 0.0745(11) Uani 1 1 d . . .
N3 N 0.3520(2) 0.5113(3) 0.22131(16) 0.0361(5) Uani 1 1 d . . .
H3C H 0.3054 0.5735 0.1899 0.043 Uiso 1 1 calc R . .
H3D H 0.3705 0.4353 0.1840 0.043 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
Ni1 C1 1.855(3) 5_675 ?
Ni1 C1 1.855(3) . ?
Ni1 C2 1.868(3) . ?
Ni1 C2 1.868(3) 5_675 ?
Zn1 N3 2.011(2) . ?
Zn1 N3 2.011(2) 4_655 ?
Zn1 N1 2.022(2) 4_655 ?
Zn1 N1 2.022(2) . ?
N1 C1 1.140(4) . ?
O1 C4 1.410(4) . ?
O1 C5 1.412(3) . ?
C2 N2 1.142(4) . ?
C3 C4 1.413(6) . ?
C3 N3 1.453(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C5 1.503(6) 5_666 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?

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
C1 Ni1 C1 180.00(17) 5_675 . ?
C1 Ni1 C2 89.55(13) 5_675 . ?
C1 Ni1 C2 90.45(13) . . ?
C1 Ni1 C2 90.45(13) 5_675 5_675 ?
C1 Ni1 C2 89.55(13) . 5_675 ?
C2 Ni1 C2 180.0 . 5_675 ?
N3 Zn1 N3 120.77(14) . 4_655 ?
N3 Zn1 N1 113.79(10) . 4_655 ?
N3 Zn1 N1 105.03(9) 4_655 4_655 ?
N3 Zn1 N1 105.03(9) . . ?
N3 Zn1 N1 113.79(10) 4_655 . ?
N1 Zn1 N1 95.76(14) 4_655 . ?
C1 N1 Zn1 171.2(2) . . ?
C4 O1 C5 116.4(3) . . ?
N1 C1 Ni1 178.8(3) . . ?
N2 C2 Ni1 179.2(4) . . ?
C4 C3 N3 115.5(3) . . ?
C4 C3 H3A 108.4 . . ?
N3 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
N3 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
O1 C4 C3 113.6(3) . . ?
O1 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
O1 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
O1 C5 C5 106.9(3) . 5_666 ?
O1 C5 H5A 110.3 . . ?
C5 C5 H5A 110.3 5_666 . ?
O1 C5 H5B 110.3 . . ?
C5 C5 H5B 110.3 5_666 . ?
H5A C5 H5B 108.6 . . ?
C3 N3 Zn1 118.7(2) . . ?
C3 N3 H3C 107.7 . . ?
Zn1 N3 H3C 107.7 . . ?
C3 N3 H3D 107.7 . . ?
Zn1 N3 H3D 107.7 . . ?
H3C N3 H3D 107.1 . . ?

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
N3 Zn1 N1 C1 35.9(16) . . . . ?
N3 Zn1 N1 C1 170.2(16) 4_655 . . . ?
N1 Zn1 N1 C1 -80.6(16) 4_655 . . . ?
Zn1 N1 C1 Ni1 -38(15) . . . . ?
C1 Ni1 C1 N1 64(100) 5_675 . . . ?
C2 Ni1 C1 N1 -96(14) . . . . ?
C2 Ni1 C1 N1 84(14) 5_675 . . . ?
C1 Ni1 C2 N2 -63(23) 5_675 . . . ?
C1 Ni1 C2 N2 117(23) . . . . ?
C2 Ni1 C2 N2 80(100) 5_675 . . . ?
C5 O1 C4 C3 106.7(4) . . . . ?
N3 C3 C4 O1 53.1(6) . . . . ?
C4 O1 C5 C5 165.0(3) . . . 5_666 ?
C4 C3 N3 Zn1 -51.0(5) . . . . ?
N3 Zn1 N3 C3 79.4(3) 4_655 . . . ?
N1 Zn1 N3 C3 -46.9(3) 4_655 . . . ?
N1 Zn1 N3 C3 -150.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.062
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_omer27
_database_code_depnum_ccdc_archive 'CCDC 971719'
_audit_update_record             
;
2013-11-13 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
(2,2'-(ethylenedioxy)bis-(ethylamine))cadmium(II) tetracyanonickelate(II) 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 Cd N6 Ni O2 '
_chemical_formula_sum            'C10 H16 Cd N6 Ni O2'
_chemical_formula_weight         423.40

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'
Ni Ni 0.3393 1.1124 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   10.8081(5)
_cell_length_b                   10.4606(4)
_cell_length_c                   14.2364(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.209(3)
_cell_angle_gamma                90.00
_cell_volume                     1537.50(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    30074
_cell_measurement_theta_min      1.50
_cell_measurement_theta_max      28.04

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.610
_exptl_crystal_size_mid          0.517
_exptl_crystal_size_min          0.410
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    2.617
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.3182
_exptl_absorpt_correction_T_max  0.4041
_exptl_absorpt_process_details   'STOE X-RED32'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -5 2 0.1880
5 6 -1 0.2280
-2 2 1 0.2570
3 -4 1 0.2740
2 2 -7 0.3020
-4 -4 -7 0.2950
4 3 -5 0.2670
0 -3 -7 0.2600
-1 3 5 0.2860
1 -2 -6 0.2580
1 -1 -2 0.2540
1 3 -8 0.3360
5 -4 2 0.2580
1 0 7 0.2900
6 3 1 0.2730
4 2 -5 0.2510
1 5 5 0.2700
2 5 -3 0.3030
-4 3 -1 0.3240
-2 3 -7 0.3590
-2 -1 -1 0.3010
-1 0 4 0.3310
5 -1 -5 0.2770


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_voltage           50
_diffrn_source_current           45
_diffrn_source_power             2.25
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_measurement_method       'rotation method'
_diffrn_measurement_details      
; 360 frames, detector distance = 100 mm
;
_diffrn_reflns_number            12464
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.77
_diffrn_reflns_theta_max         27.52
_reflns_number_total             1772
_reflns_number_gt                1749
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0124P)²+1.4092P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1772
_refine_ls_number_parameters     93
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_ref         0.0410
_refine_ls_wR_factor_gt          0.0408
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_restrained_S_all      1.231
_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
C1 C 0.32818(18) 0.63126(17) 0.59659(13) 0.0321(4) Uani 1 1 d . . .
C2 C 0.33209(18) 0.67606(18) 0.41548(13) 0.0324(4) Uani 1 1 d . . .
C3 C 0.2351(2) 0.2074(2) 0.65061(18) 0.0518(6) Uani 1 1 d . . .
H3A H 0.2568 0.1620 0.7128 0.062 Uiso 1 1 calc R . .
H3B H 0.1970 0.1467 0.5986 0.062 Uiso 1 1 calc R . .
C4 C 0.1396(2) 0.3104(2) 0.65052(17) 0.0518(6) Uani 1 1 d . . .
H4A H 0.0655 0.2748 0.6666 0.062 Uiso 1 1 calc R . .
H4B H 0.1790 0.3746 0.6994 0.062 Uiso 1 1 calc R . .
C5 C 0.0177(2) 0.4734(2) 0.55126(16) 0.0499(5) Uani 1 1 d . . .
H5A H 0.0623 0.5377 0.5982 0.060 Uiso 1 1 calc R . .
H5B H -0.0598 0.4477 0.5674 0.060 Uiso 1 1 calc R . .
N1 N 0.37652(17) 0.55888(16) 0.65609(13) 0.0412(4) Uani 1 1 d . . .
N2 N 0.38214(17) 0.63259(17) 0.36246(12) 0.0411(4) Uani 1 1 d . . .
N3 N 0.35386(18) 0.26185(18) 0.63577(14) 0.0465(4) Uani 1 1 d . . .
H3C H 0.3286 0.3057 0.5789 0.056 Uiso 1 1 calc R . .
H3D H 0.4007 0.1951 0.6253 0.056 Uiso 1 1 calc R . .
O1 O 0.09905(16) 0.36691(16) 0.55503(12) 0.0499(4) Uani 1 1 d . . .
Ni1 Ni 0.2500 0.7500 0.5000 0.02654(8) Uani 1 2 d S . .
Cd1 Cd 0.5000 0.396018(16) 0.7500 0.02666(6) Uani 1 2 d S . .


_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
C1 N1 1.141(2) . ?
C1 Ni1 1.8601(18) . ?
C2 N2 1.145(2) . ?
C2 Ni1 1.8615(19) . ?
C3 N3 1.475(3) . ?
C3 C4 1.492(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O1 1.427(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O1 1.411(3) . ?
C5 C5 1.502(5) 5_566 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N1 Cd1 2.3270(16) . ?
N2 Cd1 2.3414(17) 5_666 ?
N3 Cd1 2.3641(17) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
Ni1 C1 1.8601(18) 7_566 ?
Ni1 C2 1.8615(19) 7_566 ?
Cd1 N1 2.3270(16) 2_656 ?
Cd1 N2 2.3414(17) 5_666 ?
Cd1 N2 2.3414(17) 6_566 ?
Cd1 N3 2.3641(17) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 Ni1 179.7(2) . . ?
N2 C2 Ni1 178.74(17) . . ?
N3 C3 C4 110.62(18) . . ?
N3 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N3 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
O1 C4 C3 108.5(2) . . ?
O1 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
O1 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
O1 C5 C5 107.8(2) . 5_566 ?
O1 C5 H5A 110.1 . . ?
C5 C5 H5A 110.1 5_566 . ?
O1 C5 H5B 110.1 . . ?
C5 C5 H5B 110.1 5_566 . ?
H5A C5 H5B 108.5 . . ?
C1 N1 Cd1 166.19(16) . . ?
C2 N2 Cd1 163.81(17) . 5_666 ?
C3 N3 Cd1 124.27(14) . . ?
C3 N3 H3C 106.3 . . ?
Cd1 N3 H3C 106.3 . . ?
C3 N3 H3D 106.3 . . ?
Cd1 N3 H3D 106.3 . . ?
H3C N3 H3D 106.4 . . ?
C5 O1 C4 112.05(19) . . ?
C1 Ni1 C1 180.0 . 7_566 ?
C1 Ni1 C2 90.07(8) . . ?
C1 Ni1 C2 89.93(8) 7_566 . ?
C1 Ni1 C2 89.93(8) . 7_566 ?
C1 Ni1 C2 90.07(8) 7_566 7_566 ?
C2 Ni1 C2 180.000(1) . 7_566 ?
N1 Cd1 N1 85.87(9) 2_656 . ?
N1 Cd1 N2 98.67(7) 2_656 5_666 ?
N1 Cd1 N2 92.08(6) . 5_666 ?
N1 Cd1 N2 92.08(6) 2_656 6_566 ?
N1 Cd1 N2 98.67(7) . 6_566 ?
N2 Cd1 N2 165.31(9) 5_666 6_566 ?
N1 Cd1 N3 169.32(7) 2_656 . ?
N1 Cd1 N3 83.48(6) . . ?
N2 Cd1 N3 80.89(7) 5_666 . ?
N2 Cd1 N3 90.38(6) 6_566 . ?
N1 Cd1 N3 83.48(6) 2_656 2_656 ?
N1 Cd1 N3 169.32(7) . 2_656 ?
N2 Cd1 N3 90.38(6) 5_666 2_656 ?
N2 Cd1 N3 80.89(7) 6_566 2_656 ?
N3 Cd1 N3 107.17(10) . 2_656 ?

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
N3 C3 C4 O1 65.1(2) . . . . ?
Ni1 C1 N1 Cd1 -104(36) . . . . ?
Ni1 C2 N2 Cd1 32(9) . . . 5_666 ?
C4 C3 N3 Cd1 66.8(2) . . . . ?
C5 C5 O1 C4 179.2(2) 5_566 . . . ?
C3 C4 O1 C5 -174.43(18) . . . . ?
N1 C1 Ni1 C1 62(100) . . . 7_566 ?
N1 C1 Ni1 C2 109(37) . . . . ?
N1 C1 Ni1 C2 -71(37) . . . 7_566 ?
N2 C2 Ni1 C1 -162(8) . . . . ?
N2 C2 Ni1 C1 18(8) . . . 7_566 ?
N2 C2 Ni1 C2 -138(100) . . . 7_566 ?
C1 N1 Cd1 N1 106.9(7) . . . 2_656 ?
C1 N1 Cd1 N2 8.4(7) . . . 5_666 ?
C1 N1 Cd1 N2 -161.6(7) . . . 6_566 ?
C1 N1 Cd1 N3 -72.2(7) . . . . ?
C1 N1 Cd1 N3 111.6(7) . . . 2_656 ?
C3 N3 Cd1 N1 -98.4(4) . . . 2_656 ?
C3 N3 Cd1 N1 -93.73(18) . . . . ?
C3 N3 Cd1 N2 173.09(18) . . . 5_666 ?
C3 N3 Cd1 N2 4.95(17) . . . 6_566 ?
C3 N3 Cd1 N3 85.53(17) . . . 2_656 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.056
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelxlakaradag-cdcnni-09-09
_database_code_depnum_ccdc_archive 'CCDC 977823'
_audit_update_record             
;
2013-12-18 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_date             2013-12-18T10:27:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H32 Cd N4 O4, C4 N4 Ni, 2(H2 O)'

_chemical_formula_sum            'C16 H36 Cd N8 Ni O6'
_chemical_formula_weight         607.64
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_Int_Tables_number      19
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   9.6656(4)
_cell_length_b                   14.9615(4)
_cell_length_c                   17.9211(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     2591.60(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.591
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.826

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_number            55476
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_full        26.42
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             5323
_reflns_number_gt                4890
_reflns_threshold_expression     >2σ(I)
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           40.0000
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_detector       RX
_diffrn_measurement_device       
;
RAXIS conversion
;
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             3033
_diffrn_reflns_av_sigmaI/detI    0.1887
_diffrn_reflns_reduction_process 'Lp corrections applied'


#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0222P)²+0.3517P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0080(3)
_refine_ls_number_reflns         5323
_refine_ls_number_parameters     300
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0644
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_restrained_S_all      1.07
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(17)
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.057

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

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
Cd Cd 0.34055(2) 0.489224(15) 0.897516(12) 0.04546(9) Uani 1 1 d . . .
Ni Ni 0.07441(5) 0.78268(3) 0.78199(3) 0.05480(14) Uani 1 1 d . . .
O3 O 0.0920(3) 0.55380(18) 0.87336(16) 0.0659(7) Uani 1 1 d . . .
O1 O 0.5026(3) 0.39191(18) 0.98400(14) 0.0602(7) Uani 1 1 d . . .
O2 O 0.5565(3) 0.56156(17) 0.95199(15) 0.0629(7) Uani 1 1 d . . .
N2 N 0.4955(3) 0.4223(2) 0.81532(16) 0.0601(8) Uani 1 1 d . . .
H2C H 0.5476 0.465 0.7939 0.072 Uiso 1 1 calc R . .
H2D H 0.5523 0.3861 0.8412 0.072 Uiso 1 1 calc R . .
O4 O 0.2156(3) 0.44374(19) 0.77610(14) 0.0665(7) Uani 1 1 d . . .
N4 N 0.2348(3) 0.35160(19) 0.93145(17) 0.0564(8) Uani 1 1 d . . .
H4C H 0.1673 0.3631 0.9647 0.068 Uiso 1 1 calc R . .
H4D H 0.1946 0.3281 0.8906 0.068 Uiso 1 1 calc R . .
N1 N 0.2460(3) 0.5506(2) 1.00578(16) 0.0543(7) Uani 1 1 d . . .
H1D H 0.2236 0.5056 1.0368 0.065 Uiso 1 1 calc R . .
H1C H 0.3118 0.5834 1.0285 0.065 Uiso 1 1 calc R . .
N3 N 0.3897(4) 0.6292(2) 0.83958(19) 0.0731(10) Uani 1 1 d . . .
H3C H 0.4307 0.6193 0.7953 0.088 Uiso 1 1 calc R . .
H3D H 0.3097 0.6582 0.831 0.088 Uiso 1 1 calc R . .
C16 C -0.0373(4) 0.7883(3) 0.8665(2) 0.0582(9) Uani 1 1 d . . .
C1 C 0.3281(5) 0.2843(2) 0.9636(2) 0.0738(11) Uani 1 1 d . . .
H1A H 0.3831 0.2577 0.9241 0.089 Uiso 1 1 calc R . .
H1B H 0.2739 0.2373 0.9867 0.089 Uiso 1 1 calc R . .
C14 C 0.1939(4) 0.7722(3) 0.7013(2) 0.0699(11) Uani 1 1 d . . .
C2 C 0.4226(5) 0.3254(3) 1.0209(2) 0.0698(11) Uani 1 1 d . . .
H2A H 0.3689 0.3521 1.0608 0.084 Uiso 1 1 calc R . .
H2B H 0.4826 0.2801 1.0421 0.084 Uiso 1 1 calc R . .
C4 C 0.6623(4) 0.5083(3) 0.9844(2) 0.0679(10) Uani 1 1 d . . .
H4A H 0.7235 0.545 1.0145 0.081 Uiso 1 1 calc R . .
H4B H 0.7166 0.4793 0.9459 0.081 Uiso 1 1 calc R . .
C3 C 0.5923(4) 0.4410(3) 1.0314(2) 0.0699(11) Uani 1 1 d . . .
H3A H 0.6597 0.4015 1.0542 0.084 Uiso 1 1 calc R . .
H3B H 0.5399 0.47 1.0707 0.084 Uiso 1 1 calc R . .
N7 N -0.1065(4) 0.7904(3) 0.9179(2) 0.0790(11) Uani 1 1 d . . .
C5 C 0.6027(5) 0.6361(3) 0.9110(3) 0.0820(14) Uani 1 1 d . . .
H5A H 0.6571 0.6167 0.8685 0.098 Uiso 1 1 calc R . .
H5B H 0.6603 0.6739 0.9422 0.098 Uiso 1 1 calc R . .
C15 C -0.0669(4) 0.7234(3) 0.7305(2) 0.0598(10) Uani 1 1 d . . .
C8 C 0.0230(4) 0.5650(3) 0.9429(3) 0.0742(13) Uani 1 1 d . . .
H8A H -0.007 0.5075 0.9621 0.089 Uiso 1 1 calc R . .
H8B H -0.0576 0.6029 0.9368 0.089 Uiso 1 1 calc R . .
C12 C 0.4265(5) 0.3698(4) 0.7565(3) 0.0837(15) Uani 1 1 d . . .
H12A H 0.3874 0.3161 0.7782 0.1 Uiso 1 1 calc R . .
H12B H 0.4942 0.352 0.7194 0.1 Uiso 1 1 calc R . .
N8 N 0.2732(4) 0.7646(3) 0.6540(2) 0.1030(16) Uani 1 1 d . . .
N6 N -0.1580(4) 0.6903(3) 0.7007(2) 0.0807(10) Uani 1 1 d . . .
C13 C 0.2077(4) 0.8510(3) 0.8301(2) 0.0692(12) Uani 1 1 d . . .
C10 C 0.1025(5) 0.4977(3) 0.7517(2) 0.0826(13) Uani 1 1 d . . .
H10A H 0.0525 0.468 0.7119 0.099 Uiso 1 1 calc R . .
H10B H 0.1357 0.5548 0.7334 0.099 Uiso 1 1 calc R . .
C9 C 0.0115(5) 0.5107(3) 0.8172(3) 0.0835(14) Uani 1 1 d . . .
H9A H -0.0674 0.5475 0.8038 0.1 Uiso 1 1 calc R . .
H9B H -0.0222 0.4536 0.8352 0.1 Uiso 1 1 calc R . .
C6 C 0.4802(6) 0.6861(3) 0.8855(3) 0.0878(15) Uani 1 1 d . . .
H6A H 0.429 0.7076 0.9285 0.105 Uiso 1 1 calc R . .
H6B H 0.5095 0.7375 0.8566 0.105 Uiso 1 1 calc R . .
C7 C 0.1230(4) 0.6071(3) 0.9954(3) 0.0726(12) Uani 1 1 d . . .
H7A H 0.151 0.6649 0.976 0.087 Uiso 1 1 calc R . .
H7B H 0.0784 0.6167 1.0432 0.087 Uiso 1 1 calc R . .
C11 C 0.3156(5) 0.4216(4) 0.7199(2) 0.0939(17) Uani 1 1 d . . .
H11A H 0.3533 0.4756 0.6979 0.113 Uiso 1 1 calc R . .
H11B H 0.2729 0.3864 0.6807 0.113 Uiso 1 1 calc R . .
N5 N 0.2887(4) 0.8971(3) 0.8570(3) 0.1011(15) Uani 1 1 d . . .
O1W O 0.4096(3) 0.6141(2) 0.58203(17) 0.0829(9) Uani 1 1 d D . .
O2W O 0.6117(4) 0.5695(3) 0.6906(2) 0.0908(10) Uani 1 1 d D . .
H1F H 0.4869 0.5974 0.6086 0.070(13) Uiso 1 1 d . . .
H1E H 0.3791 0.6592 0.6002 0.072(14) Uiso 1 1 d D . .
H2E H 0.646(6) 0.523(3) 0.675(3) 0.14(3) Uiso 1 1 d D . .
H2F H 0.675(4) 0.604(3) 0.691(3) 0.11(2) Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Cd N2 2.327(3) . ?
Cd N1 2.333(3) . ?
Cd N4 2.378(3) . ?
Cd N3 2.386(3) . ?
Cd O2 2.546(3) . ?
Cd O4 2.580(3) . ?
Cd O3 2.625(3) . ?
Cd O1 2.641(3) . ?
Ni C13 1.857(5) . ?
Ni C14 1.857(5) . ?
Ni C16 1.862(4) . ?
Ni C15 1.872(4) . ?
O3 C9 1.426(5) . ?
O3 C8 1.423(5) . ?
O1 C3 1.419(5) . ?
O1 C2 1.423(5) . ?
O2 C5 1.408(5) . ?
O2 C4 1.421(4) . ?
N2 C12 1.474(5) . ?
N2 H2C 0.9 . ?
N2 H2D 0.9 . ?
O4 C10 1.427(5) . ?
O4 C11 1.435(5) . ?
N4 C1 1.469(5) . ?
N4 H4C 0.9 . ?
N4 H4D 0.9 . ?
N1 C7 1.472(5) . ?
N1 H1D 0.9 . ?
N1 H1C 0.9 . ?
N3 C6 1.472(5) . ?
N3 H3C 0.9 . ?
N3 H3D 0.9 . ?
C16 N7 1.139(5) . ?
C1 C2 1.505(6) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C14 N8 1.148(5) . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C4 C3 1.477(6) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C3 H3A 0.97 . ?
C3 H3B 0.97 . ?
C5 C6 1.473(7) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C15 N6 1.142(5) . ?
C8 C7 1.489(6) . ?
C8 H8A 0.97 . ?
C8 H8B 0.97 . ?
C12 C11 1.476(7) . ?
C12 H12A 0.97 . ?
C12 H12B 0.97 . ?
C13 N5 1.149(5) . ?
C10 C9 1.479(6) . ?
C10 H10A 0.97 . ?
C10 H10B 0.97 . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C11 H11A 0.97 . ?
C11 H11B 0.97 . ?
O1W H1F 0.921(3) . ?
O1W H1E 0.805(3) . ?
O2W H2E 0.81(2) . ?
O2W H2F 0.80(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cd N1 161.42(11) . . ?
N2 Cd N4 93.77(11) . . ?
N1 Cd N4 87.68(11) . . ?
N2 Cd N3 88.53(13) . . ?
N1 Cd N3 95.42(12) . . ?
N4 Cd N3 163.17(11) . . ?
N2 Cd O2 84.15(10) . . ?
N1 Cd O2 80.50(11) . . ?
N4 Cd O2 128.51(10) . . ?
N3 Cd O2 68.31(10) . . ?
N2 Cd O4 69.74(11) . . ?
N1 Cd O4 128.46(11) . . ?
N4 Cd O4 77.64(10) . . ?
N3 Cd O4 87.58(10) . . ?
O2 Cd O4 145.01(9) . . ?
N2 Cd O3 130.01(10) . . ?
N1 Cd O3 68.53(10) . . ?
N4 Cd O3 88.13(10) . . ?
N3 Cd O3 77.72(11) . . ?
O2 Cd O3 131.08(9) . . ?
O4 Cd O3 61.94(9) . . ?
N2 Cd O1 75.67(10) . . ?
N1 Cd O1 87.77(9) . . ?
N4 Cd O1 68.14(10) . . ?
N3 Cd O1 128.42(11) . . ?
O2 Cd O1 61.52(9) . . ?
O4 Cd O1 128.84(9) . . ?
O3 Cd O1 147.38(9) . . ?
C13 Ni C14 88.64(18) . . ?
C13 Ni C16 90.00(17) . . ?
C14 Ni C16 176.16(18) . . ?
C13 Ni C15 174.87(19) . . ?
C14 Ni C15 91.72(17) . . ?
C16 Ni C15 89.96(17) . . ?
C9 O3 C8 114.6(3) . . ?
C9 O3 Cd 116.7(2) . . ?
C8 O3 Cd 109.1(2) . . ?
C3 O1 C2 114.6(3) . . ?
C3 O1 Cd 115.4(2) . . ?
C2 O1 Cd 109.6(2) . . ?
C5 O2 C4 115.4(3) . . ?
C5 O2 Cd 113.4(2) . . ?
C4 O2 Cd 120.6(2) . . ?
C12 N2 Cd 113.0(2) . . ?
C12 N2 H2C 109 . . ?
Cd N2 H2C 109 . . ?
C12 N2 H2D 109 . . ?
Cd N2 H2D 109 . . ?
H2C N2 H2D 107.8 . . ?
C10 O4 C11 115.6(3) . . ?
C10 O4 Cd 117.9(2) . . ?
C11 O4 Cd 109.7(2) . . ?
C1 N4 Cd 115.4(2) . . ?
C1 N4 H4C 108.4 . . ?
Cd N4 H4C 108.4 . . ?
C1 N4 H4D 108.4 . . ?
Cd N4 H4D 108.4 . . ?
H4C N4 H4D 107.5 . . ?
C7 N1 Cd 116.0(2) . . ?
C7 N1 H1D 108.3 . . ?
Cd N1 H1D 108.3 . . ?
C7 N1 H1C 108.3 . . ?
Cd N1 H1C 108.3 . . ?
H1D N1 H1C 107.4 . . ?
C6 N3 Cd 112.5(2) . . ?
C6 N3 H3C 109.1 . . ?
Cd N3 H3C 109.1 . . ?
C6 N3 H3D 109.1 . . ?
Cd N3 H3D 109.1 . . ?
H3C N3 H3D 107.8 . . ?
N7 C16 Ni 178.9(4) . . ?
N4 C1 C2 111.1(3) . . ?
N4 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N4 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108 . . ?
N8 C14 Ni 176.4(4) . . ?
O1 C2 C1 107.4(3) . . ?
O1 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
O1 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O2 C4 C3 106.6(3) . . ?
O2 C4 H4A 110.4 . . ?
C3 C4 H4A 110.4 . . ?
O2 C4 H4B 110.4 . . ?
C3 C4 H4B 110.4 . . ?
H4A C4 H4B 108.6 . . ?
O1 C3 C4 106.9(3) . . ?
O1 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
O1 C3 H3B 110.3 . . ?
C4 C3 H3B 110.3 . . ?
H3A C3 H3B 108.6 . . ?
O2 C5 C6 108.0(4) . . ?
O2 C5 H5A 110.1 . . ?
C6 C5 H5A 110.1 . . ?
O2 C5 H5B 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
N6 C15 Ni 176.3(4) . . ?
O3 C8 C7 107.4(3) . . ?
O3 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
O3 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
N2 C12 C11 111.5(4) . . ?
N2 C12 H12A 109.3 . . ?
C11 C12 H12A 109.3 . . ?
N2 C12 H12B 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 108 . . ?
N5 C13 Ni 176.1(5) . . ?
O4 C10 C9 106.7(3) . . ?
O4 C10 H10A 110.4 . . ?
C9 C10 H10A 110.4 . . ?
O4 C10 H10B 110.4 . . ?
C9 C10 H10B 110.4 . . ?
H10A C10 H10B 108.6 . . ?
O3 C9 C10 107.2(3) . . ?
O3 C9 H9A 110.3 . . ?
C10 C9 H9A 110.3 . . ?
O3 C9 H9B 110.3 . . ?
C10 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
N3 C6 C5 111.0(4) . . ?
N3 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N3 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108 . . ?
N1 C7 C8 111.2(3) . . ?
N1 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N1 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108 . . ?
O4 C11 C12 107.4(3) . . ?
O4 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
O4 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
H1F O1W H1E 108.5(3) . . ?
H2E O2W H2F 104(6) . . ?

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
N2 Cd O3 C9 32.2(3) . . . . ?
N1 Cd O3 C9 -149.4(3) . . . . ?
N4 Cd O3 C9 -61.2(3) . . . . ?
N3 Cd O3 C9 109.7(3) . . . . ?
O2 Cd O3 C9 155.9(3) . . . . ?
O4 Cd O3 C9 15.8(3) . . . . ?
O1 Cd O3 C9 -103.2(3) . . . . ?
N2 Cd O3 C8 164.0(2) . . . . ?
N1 Cd O3 C8 -17.6(2) . . . . ?
N4 Cd O3 C8 70.7(2) . . . . ?
N3 Cd O3 C8 -118.5(3) . . . . ?
O2 Cd O3 C8 -72.3(3) . . . . ?
O4 Cd O3 C8 147.6(3) . . . . ?
O1 Cd O3 C8 28.6(3) . . . . ?
N2 Cd O1 C3 111.1(3) . . . . ?
N1 Cd O1 C3 -60.4(3) . . . . ?
N4 Cd O1 C3 -148.8(3) . . . . ?
N3 Cd O1 C3 34.7(3) . . . . ?
O2 Cd O1 C3 20.0(2) . . . . ?
O4 Cd O1 C3 159.4(2) . . . . ?
O3 Cd O1 C3 -102.6(3) . . . . ?
N2 Cd O1 C2 -117.8(3) . . . . ?
N1 Cd O1 C2 70.7(2) . . . . ?
N4 Cd O1 C2 -17.7(2) . . . . ?
N3 Cd O1 C2 165.9(2) . . . . ?
O2 Cd O1 C2 151.1(3) . . . . ?
O4 Cd O1 C2 -69.4(3) . . . . ?
O3 Cd O1 C2 28.5(3) . . . . ?
N2 Cd O2 C5 80.4(3) . . . . ?
N1 Cd O2 C5 -110.1(3) . . . . ?
N4 Cd O2 C5 170.6(3) . . . . ?
N3 Cd O2 C5 -10.3(3) . . . . ?
O4 Cd O2 C5 39.3(3) . . . . ?
O3 Cd O2 C5 -59.8(3) . . . . ?
O1 Cd O2 C5 157.3(3) . . . . ?
N2 Cd O2 C4 -62.6(3) . . . . ?
N1 Cd O2 C4 106.9(3) . . . . ?
N4 Cd O2 C4 27.5(3) . . . . ?
N3 Cd O2 C4 -153.4(3) . . . . ?
O4 Cd O2 C4 -103.7(3) . . . . ?
O3 Cd O2 C4 157.2(2) . . . . ?
O1 Cd O2 C4 14.2(2) . . . . ?
N1 Cd N2 C12 151.1(4) . . . . ?
N4 Cd N2 C12 57.2(3) . . . . ?
N3 Cd N2 C12 -106.2(3) . . . . ?
O2 Cd N2 C12 -174.5(3) . . . . ?
O4 Cd N2 C12 -18.2(3) . . . . ?
O3 Cd N2 C12 -33.6(4) . . . . ?
O1 Cd N2 C12 123.4(3) . . . . ?
N2 Cd O4 C10 -148.2(3) . . . . ?
N1 Cd O4 C10 36.2(3) . . . . ?
N4 Cd O4 C10 113.1(3) . . . . ?
N3 Cd O4 C10 -58.8(3) . . . . ?
O2 Cd O4 C10 -103.9(3) . . . . ?
O3 Cd O4 C10 18.5(3) . . . . ?
O1 Cd O4 C10 161.3(3) . . . . ?
N2 Cd O4 C11 -13.0(3) . . . . ?
N1 Cd O4 C11 171.3(3) . . . . ?
N4 Cd O4 C11 -111.8(3) . . . . ?
N3 Cd O4 C11 76.3(3) . . . . ?
O2 Cd O4 C11 31.2(3) . . . . ?
O3 Cd O4 C11 153.7(3) . . . . ?
O1 Cd O4 C11 -63.6(3) . . . . ?
N2 Cd N4 C1 58.6(3) . . . . ?
N1 Cd N4 C1 -102.9(3) . . . . ?
N3 Cd N4 C1 156.0(4) . . . . ?
O2 Cd N4 C1 -27.0(3) . . . . ?
O4 Cd N4 C1 126.9(3) . . . . ?
O3 Cd N4 C1 -171.5(3) . . . . ?
O1 Cd N4 C1 -14.4(2) . . . . ?
N2 Cd N1 C7 162.2(3) . . . . ?
N4 Cd N1 C7 -102.9(3) . . . . ?
N3 Cd N1 C7 60.5(3) . . . . ?
O2 Cd N1 C7 127.4(3) . . . . ?
O4 Cd N1 C7 -30.7(3) . . . . ?
O3 Cd N1 C7 -14.0(2) . . . . ?
O1 Cd N1 C7 -171.1(3) . . . . ?
N2 Cd N3 C6 -104.5(3) . . . . ?
N1 Cd N3 C6 57.4(3) . . . . ?
N4 Cd N3 C6 157.4(4) . . . . ?
O2 Cd N3 C6 -20.2(3) . . . . ?
O4 Cd N3 C6 -174.2(3) . . . . ?
O3 Cd N3 C6 124.0(3) . . . . ?
O1 Cd N3 C6 -34.1(4) . . . . ?
C13 Ni C16 N7 -15E1(2) . . . . ?
C14 Ni C16 N7 -8E1(2) . . . . ?
C15 Ni C16 N7 4E1(2) . . . . ?
Cd N4 C1 C2 45.1(4) . . . . ?
C13 Ni C14 N8 48(7) . . . . ?
C16 Ni C14 N8 -21(8) . . . . ?
C15 Ni C14 N8 -137(7) . . . . ?
C3 O1 C2 C1 176.6(3) . . . . ?
Cd O1 C2 C1 45.0(4) . . . . ?
N4 C1 C2 O1 -60.7(4) . . . . ?
C5 O2 C4 C3 173.6(3) . . . . ?
Cd O2 C4 C3 -44.1(4) . . . . ?
C2 O1 C3 C4 -178.0(3) . . . . ?
Cd O1 C3 C4 -49.3(4) . . . . ?
O2 C4 C3 O1 58.6(4) . . . . ?
C4 O2 C5 C6 -176.7(4) . . . . ?
Cd O2 C5 C6 38.3(4) . . . . ?
C13 Ni C15 N6 -48(7) . . . . ?
C14 Ni C15 N6 -142(6) . . . . ?
C16 Ni C15 N6 42(6) . . . . ?
C9 O3 C8 C7 177.7(3) . . . . ?
Cd O3 C8 C7 44.7(4) . . . . ?
Cd N2 C12 C11 49.6(4) . . . . ?
C14 Ni C13 N5 70(6) . . . . ?
C16 Ni C13 N5 -114(6) . . . . ?
C15 Ni C13 N5 -24(7) . . . . ?
C11 O4 C10 C9 178.8(3) . . . . ?
Cd O4 C10 C9 -48.6(4) . . . . ?
C8 O3 C9 C10 -175.1(3) . . . . ?
Cd O3 C9 C10 -45.8(4) . . . . ?
O4 C10 C9 O3 59.6(4) . . . . ?
Cd N3 C6 C5 49.8(5) . . . . ?
O2 C5 C6 N3 -58.4(5) . . . . ?
Cd N1 C7 C8 44.7(4) . . . . ?
O3 C8 C7 N1 -60.1(5) . . . . ?
C10 O4 C11 C12 177.4(4) . . . . ?
Cd O4 C11 C12 41.1(4) . . . . ?
N2 C12 C11 O4 -61.1(5) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
