# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_p-delta

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H22 Cd N7 O,NO3,C2H6O,C3H7NO'
_chemical_formula_sum            'C32 H35 Cd N9 O6'
_chemical_formula_weight         754.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   'F23  '

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

_cell_length_a                   25.3961(9)
_cell_length_b                   25.3961(9)
_cell_length_c                   25.3961(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     16379.5(10)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1888
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      15.46

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6176
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9180
_exptl_absorpt_correction_T_max  0.9550
_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18992
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.66
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2412
_reflns_number_gt                1497
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1700P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(13)
_refine_ls_number_reflns         2412
_refine_ls_number_parameters     97
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.2091
_refine_ls_wR_factor_gt          0.1884
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_restrained_S_all      0.829
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.20011(2) 0.29989(2) 0.20011(2) 0.0794(4) Uani 1 3 d S . .
O1 O 0.2964(3) 0.2964(3) 0.2036(3) 0.106(3) Uani 1 3 d S . .
H1 H 0.3192 0.3192 0.1808 0.127 Uiso 1 3 calc SR . .
C1 C 0.1890(5) 0.4234(4) 0.2379(4) 0.114(2) Uani 1 1 d U . .
H1A H 0.1864 0.4126 0.2737 0.137 Uiso 1 1 calc R . .
C2 C 0.1960(6) 0.4243(4) 0.1574(4) 0.120(2) Uani 1 1 d U . .
H2 H 0.2010 0.4142 0.1217 0.144 Uiso 1 1 calc R . .
C3 C 0.1866(5) 0.4723(4) 0.1715(5) 0.125(2) Uani 1 1 d U . .
H3 H 0.1824 0.5016 0.1487 0.150 Uiso 1 1 calc R . .
C4 C 0.1770(4) 0.5182(3) 0.2536(3) 0.144(2) Uani 1 1 d GU . .
C5 C 0.1659(4) 0.5659(3) 0.2292(3) 0.154(3) Uani 1 1 d GU . .
H5 H 0.1652 0.5681 0.1918 0.185 Uiso 1 1 calc R . .
C6 C 0.1559(4) 0.6105(3) 0.2593(3) 0.162(3) Uani 1 1 d GU . .
H6 H 0.1483 0.6431 0.2426 0.195 Uiso 1 1 calc R . .
C7 C 0.1569(5) 0.6073(3) 0.3140(3) 0.164(3) Uani 1 1 d GU . .
C8 C 0.1680(5) 0.5596(3) 0.3384(3) 0.161(3) Uani 1 1 d GU . .
H8 H 0.1687 0.5574 0.3758 0.194 Uiso 1 1 calc R . .
C9 C 0.1780(4) 0.5150(3) 0.3082(3) 0.155(3) Uani 1 1 d GU . .
H9 H 0.1855 0.4824 0.3249 0.186 Uiso 1 1 calc R . .
N1 N 0.1980(4) 0.3893(3) 0.1982(3) 0.1147(19) Uani 1 1 d U . .
N2 N 0.1841(4) 0.4730(3) 0.2229(4) 0.1245(18) Uani 1 1 d U . .
N3 N 0.1553(7) 0.6553(7) 0.3447(7) 0.174(10) Uani 1 3 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0794(4) 0.0794(4) 0.0794(4) -0.0027(3) 0.0027(3) -0.0027(3)
O1 0.106(3) 0.106(3) 0.106(3) -0.040(5) -0.040(5) 0.040(5)
C1 0.149(4) 0.095(4) 0.099(4) -0.025(3) -0.014(4) 0.005(4)
C2 0.162(5) 0.099(4) 0.099(4) -0.031(3) -0.009(4) 0.004(4)
C3 0.172(5) 0.096(4) 0.107(4) -0.031(4) -0.010(4) 0.004(4)
C4 0.186(5) 0.115(4) 0.129(4) -0.036(4) -0.036(4) 0.033(4)
C5 0.195(5) 0.126(4) 0.141(5) -0.039(4) -0.040(5) 0.041(4)
C6 0.204(6) 0.129(5) 0.153(5) -0.041(4) -0.041(5) 0.045(5)
C7 0.202(6) 0.136(5) 0.153(5) -0.042(5) -0.045(5) 0.045(5)
C8 0.206(6) 0.137(5) 0.141(5) -0.044(4) -0.046(5) 0.037(5)
C9 0.201(5) 0.127(4) 0.137(5) -0.042(4) -0.044(5) 0.035(4)
N1 0.146(4) 0.098(4) 0.100(4) -0.024(3) -0.009(4) -0.005(4)
N2 0.167(4) 0.099(3) 0.108(3) -0.030(3) -0.020(4) 0.011(3)
N3 0.174(10) 0.174(10) 0.174(10) -0.098(12) -0.098(12) 0.098(12)

_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 N1 2.271(9) 48 ?
Cd1 N1 2.271(9) 18 ?
Cd1 N1 2.271(9) . ?
Cd1 O1 2.450(7) . ?
Cd1 O1 2.450(7) 27 ?
Cd1 O1 2.450(7) 38 ?
O1 Cd1 2.450(7) 27 ?
O1 Cd1 2.450(7) 38 ?
O1 H1 1.0000 . ?
C1 N2 1.322(13) . ?
C1 N1 1.350(12) . ?
C1 H1A 0.9500 . ?
C2 C3 1.293(13) . ?
C2 N1 1.366(14) . ?
C2 H2 0.9500 . ?
C3 N2 1.307(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 C9 1.3900 . ?
C4 N2 1.399(10) . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 C7 1.3900 . ?
C6 H6 0.9500 . ?
C7 C8 1.3900 . ?
C7 N3 1.448(7) . ?
C8 C9 1.3900 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
N3 C7 1.448(11) 35_465 ?
N3 C7 1.448(9) 44_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N1 87.4(3) 48 18 ?
N1 Cd1 N1 87.4(3) 48 . ?
N1 Cd1 N1 87.4(3) 18 . ?
N1 Cd1 O1 178.9(3) 48 . ?
N1 Cd1 O1 93.3(3) 18 . ?
N1 Cd1 O1 93.5(3) . . ?
N1 Cd1 O1 93.5(3) 48 27 ?
N1 Cd1 O1 178.9(3) 18 27 ?
N1 Cd1 O1 93.3(3) . 27 ?
O1 Cd1 O1 85.8(4) . 27 ?
N1 Cd1 O1 93.3(3) 48 38 ?
N1 Cd1 O1 93.5(3) 18 38 ?
N1 Cd1 O1 178.9(3) . 38 ?
O1 Cd1 O1 85.8(4) . 38 ?
O1 Cd1 O1 85.8(4) 27 38 ?
Cd1 O1 Cd1 94.0(3) . 27 ?
Cd1 O1 Cd1 94.0(3) . 38 ?
Cd1 O1 Cd1 94.0(3) 27 38 ?
Cd1 O1 H1 122.4 . . ?
Cd1 O1 H1 122.4 27 . ?
Cd1 O1 H1 122.4 38 . ?
N2 C1 N1 114.3(10) . . ?
N2 C1 H1A 122.8 . . ?
N1 C1 H1A 122.8 . . ?
C3 C2 N1 114.2(10) . . ?
C3 C2 H2 122.9 . . ?
N1 C2 H2 122.9 . . ?
C2 C3 N2 107.5(12) . . ?
C2 C3 H3 126.3 . . ?
N2 C3 H3 126.3 . . ?
C5 C4 C9 120.0 . . ?
C5 C4 N2 119.5(6) . . ?
C9 C4 N2 120.4(7) . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 N3 119.9(9) . . ?
C6 C7 N3 119.3(11) . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C4 120.0 . . ?
C8 C9 H9 120.0 . . ?
C4 C9 H9 120.0 . . ?
C1 N1 C2 98.2(8) . . ?
C1 N1 Cd1 129.0(8) . . ?
C2 N1 Cd1 131.9(6) . . ?
C3 N2 C1 105.6(9) . . ?
C3 N2 C4 125.0(10) . . ?
C1 N2 C4 129.3(9) . . ?
C7 N3 C7 117.6(8) 35_465 . ?
C7 N3 C7 117.6(7) 35_465 44_556 ?
C7 N3 C7 117.6(9) . 44_556 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.077

# 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 -0.053 -0.019 -0.012 7788 1595 ' '
2 0.164 0.164 0.664 5 5 ' '
3 0.164 0.336 0.836 5 5 ' '
4 0.164 0.664 0.164 5 5 ' '
5 0.164 0.836 0.336 5 5 ' '
6 0.251 0.250 0.750 105 101 ' '
7 0.251 0.750 0.250 105 101 ' '
8 0.338 0.162 0.838 4 4 ' '
9 0.338 0.338 0.662 4 4 ' '
10 0.338 0.662 0.338 4 4 ' '
11 0.338 0.838 0.162 4 4 ' '
12 0.664 0.164 0.164 5 5 ' '
13 0.664 0.336 0.336 5 5 ' '
14 0.664 0.664 0.664 5 5 ' '
15 0.664 0.836 0.836 5 5 ' '
16 0.751 0.250 0.250 105 101 ' '
17 0.751 0.750 0.750 105 101 ' '
18 0.838 0.162 0.338 4 4 ' '
19 0.838 0.338 0.162 4 4 ' '
20 0.838 0.662 0.838 4 4 ' '
21 0.838 0.838 0.662 4 4 ' '
_platon_squeeze_details          
;
Complex 1 has unusually large voids. 
The voids in the framework are filled with many disordered solvent
molecules and anions, which can not be located. Hence reflect on a high R(int)
value. In the refinement we used SQEEZE procedure 
(Spek, A.L. (2008) Utrecht University, Utrecht, 
The Netherlands) to remove solvent electron
density from voids which give a smaller final R(int) and R-value compared
with the original R(int) and R-value.
A main residual electron density of 1595 electrons/cell in cell-remaining voids 
where the residual electron density was tentatively assigned to 
1 NO3-, 1 EtOH and 1 DMF molecules [1595/16 = 99 for per formula of 1; 
98 = 40 (DMF) + 26 (EtOH) + 32 (NO3-)]. The numbers of and EtOH and 
DMF were also proved by the TGA and EA.
;

# start Validation Reply Form
_vrf_CHEMW03_p-delta             
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased from
the atom count to account for 1 NO3-, 1 EtOH and 1 DMF molecules 
omitted by SQUEEZE.
;
_database_code_depnum_ccdc_archive 'CCDC 967807'
#######################################################################
#
#                 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_p-Lambda

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H22 Cd N7 O,NO3,C2H6O,C3H7NO'
_chemical_formula_sum            'C32 H35 Cd N9 O6'
_chemical_formula_weight         754.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   'F23  '

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

_cell_length_a                   25.704(3)
_cell_length_b                   25.704(3)
_cell_length_c                   25.704(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     16983(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    585
_cell_measurement_theta_min      4.25
_cell_measurement_theta_max      25.3

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6176
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9359
_exptl_absorpt_correction_T_max  0.9461
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10189
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         24.97
_reflns_number_total             2402
_reflns_number_gt                1364
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0780P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(8)
_refine_ls_number_reflns         2402
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.1337
_refine_ls_wR_factor_gt          0.1259
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_restrained_S_all      0.836
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.010

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 0.199490(18) 0.800510(18) 0.300510(18) 0.0714(3) Uani 1 3 d S . .
O1 O 0.2022(2) 0.7022(2) 0.2978(2) 0.103(3) Uani 1 3 d S . .
H1 H 0.1802 0.6802 0.3198 0.124 Uiso 1 3 calc SR . .
N1 N 0.1971(3) 0.8035(2) 0.3917(2) 0.0870(17) Uani 1 1 d . . .
C1 C 0.2359(3) 0.8123(3) 0.4235(3) 0.079(2) Uani 1 1 d . . .
H1A H 0.2703 0.8148 0.4125 0.095 Uiso 1 1 calc R . .
N2 N 0.2212(3) 0.8175(2) 0.4745(2) 0.0868(18) Uani 1 1 d . . .
C2 C 0.1552(4) 0.8030(5) 0.4233(3) 0.131(3) Uani 1 1 d . . .
H2 H 0.1212 0.7999 0.4112 0.157 Uiso 1 1 calc R . .
C3 C 0.1667(4) 0.8070(6) 0.4709(4) 0.181(6) Uani 1 1 d . . .
H3 H 0.1438 0.8037 0.4987 0.217 Uiso 1 1 calc R . .
C4 C 0.2520(4) 0.8254(3) 0.5214(4) 0.101(3) Uani 1 1 d . . .
C7 C 0.3119(6) 0.8398(4) 0.6073(4) 0.142(4) Uani 1 1 d . . .
C8 C 0.3341(4) 0.8274(5) 0.5660(5) 0.138(4) Uani 1 1 d . . .
H8 H 0.3701 0.8240 0.5651 0.166 Uiso 1 1 calc R . .
C5 C 0.2291(4) 0.8342(4) 0.5692(4) 0.118(3) Uani 1 1 d . . .
H5 H 0.1931 0.8341 0.5727 0.141 Uiso 1 1 calc R . .
C6 C 0.2598(5) 0.8428(5) 0.6106(4) 0.158(5) Uani 1 1 d . . .
H6 H 0.2446 0.8511 0.6424 0.190 Uiso 1 1 calc R . .
C9 C 0.3024(4) 0.8179(4) 0.5176(4) 0.149(4) Uani 1 1 d . . .
H9 H 0.3178 0.8072 0.4866 0.179 Uiso 1 1 calc R . .
N3 N 0.3432(4) 0.8432(4) 0.6568(4) 0.158(7) Uani 1 3 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0714(3) 0.0714(3) 0.0714(3) 0.0035(3) -0.0035(3) -0.0035(3)
O1 0.103(3) 0.103(3) 0.103(3) -0.050(6) -0.050(6) 0.050(6)
N1 0.076(3) 0.097(4) 0.088(4) 0.015(4) -0.013(4) -0.015(5)
C1 0.084(5) 0.064(5) 0.090(6) 0.000(4) -0.007(4) 0.011(4)
N2 0.087(4) 0.099(5) 0.074(4) -0.006(3) -0.010(3) 0.018(3)
C2 0.099(7) 0.214(10) 0.080(6) -0.009(7) -0.027(5) -0.006(7)
C3 0.102(8) 0.360(19) 0.079(7) -0.039(10) -0.004(5) -0.043(11)
C4 0.074(6) 0.117(7) 0.113(8) -0.023(5) -0.032(5) 0.012(4)
C7 0.167(12) 0.143(8) 0.116(8) -0.074(6) -0.044(8) 0.063(7)
C8 0.078(6) 0.201(11) 0.136(10) -0.003(8) 0.003(6) 0.021(7)
C5 0.103(6) 0.161(8) 0.089(6) -0.028(6) -0.039(5) 0.022(6)
C6 0.131(9) 0.248(14) 0.096(8) -0.061(8) -0.034(7) 0.068(9)
C9 0.108(8) 0.231(12) 0.109(7) -0.038(6) -0.028(7) 0.007(9)
N3 0.158(7) 0.158(7) 0.158(7) -0.101(8) -0.101(8) 0.101(8)

_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 N1 2.347(6) . ?
Cd1 N1 2.347(6) 22_655 ?
Cd1 N1 2.347(6) 31_564 ?
Cd1 O1 2.529(5) 38_565 ?
Cd1 O1 2.529(5) . ?
Cd1 O1 2.529(5) 16_565 ?
O1 Cd1 2.529(5) 38_565 ?
O1 Cd1 2.529(5) 16_565 ?
O1 H1 0.9800 . ?
N1 C1 1.308(8) . ?
N1 C2 1.350(10) . ?
C1 N2 1.371(8) . ?
C1 H1A 0.9300 . ?
N2 C3 1.430(10) . ?
N2 C4 1.454(10) . ?
C2 C3 1.265(10) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C9 1.314(12) . ?
C4 C5 1.381(12) . ?
C7 C8 1.245(12) . ?
C7 C6 1.344(14) . ?
C7 N3 1.508(10) . ?
C8 C9 1.508(12) . ?
C8 H8 0.9300 . ?
C5 C6 1.344(11) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C9 H9 0.9300 . ?
N3 C7 1.508(10) 20_656 ?
N3 C7 1.508(10) 47_466 ?

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 Cd1 N1 86.6(2) . 22_655 ?
N1 Cd1 N1 86.6(2) . 31_564 ?
N1 Cd1 N1 86.6(2) 22_655 31_564 ?
N1 Cd1 O1 93.1(2) . 38_565 ?
N1 Cd1 O1 93.5(2) 22_655 38_565 ?
N1 Cd1 O1 179.68(17) 31_564 38_565 ?
N1 Cd1 O1 93.5(2) . . ?
N1 Cd1 O1 179.68(17) 22_655 . ?
N1 Cd1 O1 93.1(2) 31_564 . ?
O1 Cd1 O1 86.8(3) 38_565 . ?
N1 Cd1 O1 179.68(17) . 16_565 ?
N1 Cd1 O1 93.1(2) 22_655 16_565 ?
N1 Cd1 O1 93.5(2) 31_564 16_565 ?
O1 Cd1 O1 86.8(3) 38_565 16_565 ?
O1 Cd1 O1 86.8(3) . 16_565 ?
Cd1 O1 Cd1 93.1(3) 38_565 . ?
Cd1 O1 Cd1 93.1(3) 38_565 16_565 ?
Cd1 O1 Cd1 93.1(3) . 16_565 ?
Cd1 O1 H1 123.0 38_565 . ?
Cd1 O1 H1 123.0 . . ?
Cd1 O1 H1 123.0 16_565 . ?
C1 N1 C2 103.6(6) . . ?
C1 N1 Cd1 127.6(6) . . ?
C2 N1 Cd1 128.3(5) . . ?
N1 C1 N2 113.9(7) . . ?
N1 C1 H1A 123.1 . . ?
N2 C1 H1A 123.1 . . ?
C1 N2 C3 100.9(6) . . ?
C1 N2 C4 131.0(7) . . ?
C3 N2 C4 127.7(7) . . ?
C3 C2 N1 113.1(8) . . ?
C3 C2 H2 123.4 . . ?
N1 C2 H2 123.4 . . ?
C2 C3 N2 108.0(9) . . ?
C2 C3 H3 126.0 . . ?
N2 C3 H3 126.0 . . ?
C9 C4 C5 120.6(8) . . ?
C9 C4 N2 117.0(9) . . ?
C5 C4 N2 122.0(8) . . ?
C8 C7 C6 121.7(10) . . ?
C8 C7 N3 119.3(12) . . ?
C6 C7 N3 118.3(11) . . ?
C7 C8 C9 119.9(9) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C6 C5 C4 118.9(9) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.6 . . ?
C7 C6 C5 121.6(10) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C4 C9 C8 116.6(9) . . ?
C4 C9 H9 121.7 . . ?
C8 C9 H9 121.7 . . ?
C7 N3 C7 117.9(4) 20_656 47_466 ?
C7 N3 C7 117.9(4) 20_656 . ?
C7 N3 C7 117.9(4) 47_466 . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.075


# 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 -0.054 -0.016 -0.005 8196 1485 ' '
2 0.250 0.250 0.250 100 85 ' '
3 0.250 0.750 0.750 100 85 ' '
4 0.750 0.250 0.750 100 85 ' '
5 0.750 0.750 0.250 100 85 ' '
_platon_squeeze_details          
;
Complex 1 has unusually large voids. 
The voids in the framework are filled with many disordered solvent
molecules and anions, which can not be located. Hence reflect on a high R(int)
value. In the refinement we used SQEEZE procedure 
(Spek, A.L. (2008) Utrecht University, Utrecht, 
The Netherlands) to remove solvent electron
density from voids which give a smaller final R(int) and R-value compared
with the original R(int) and R-value.
A main residual electron density of 1595 electrons/cell in 
cell-remaining voids where the residual electron density was 
tentatively assigned to 1 NO3-, 1 EtOH and 1 DMF molecules 
[1595/16 = 99 for per formula of 1; 98 = 40 (DMF) + 26 (EtOH) + 32 (NO3-)]. 
The numbers of and EtOH and DMF were also proved by the TGA and EA.
;

# start Validation Reply Form
_vrf_CHEMW03_p-Lambda            
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE:  This is caused by the given molecular weight being increased from
the atom count to account for 1 NO3-, 1 EtOH and 1 DMF molecules 
omitted by SQUEEZE.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 967808'
