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


data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H10 Cd Cl2 N10 O0'
_chemical_formula_weight         453.58

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   3.694(4)
_cell_length_b                   8.184(9)
_cell_length_c                   23.62(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.49
_cell_angle_gamma                90.00
_cell_volume                     712.1(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    296
_cell_measurement_theta_min      1.99
_cell_measurement_theta_max      21.05

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             444
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3837
_diffrn_reflns_av_R_equivalents  0.1500
_diffrn_reflns_av_sigmaI/netI    0.3001
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         26.41
_reflns_number_total             1451
_reflns_number_gt                546
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.
  The model shows relatively high R factor, due to the low quality of the
 crystals. Multiple crystals from different reaction conditions have been
 tried, and the quality improvement was not obvious.
 The crystals are in thin needels shape. A large residue peak can
 be found in the square center formed by Cd and Cl. This place is not possible
 for any atom due to the close distance to Cd and Cl. Splitting atoms such as
 C5 does not lead to stable refinement. Nevertheless, the infinite chain of CdCl
 can be clearly located. 
;

_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)+(0.1501P)²+44.5225P] 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     SHELXL
_refine_ls_extinction_coef       0.075(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1451
_refine_ls_number_parameters     107
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.2346
_refine_ls_R_factor_gt           0.1511
_refine_ls_wR_factor_ref         0.4467
_refine_ls_wR_factor_gt          0.4242
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.072
_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 1.0000 0.5000 0.5000 0.0524(17) Uani 1 2 d S . .
Cl2 Cl 1.482(2) 0.7202(10) 0.4774(3) 0.046(2) Uani 1 1 d . . .
N5 N 0.646(8) 0.472(3) 0.3154(10) 0.051(7) Uani 1 1 d . . .
C5 C 0.780(16) 0.497(6) 0.370(2) 0.12(2) Uani 1 1 d . . .
H5 H 0.7540 0.6046 0.3812 0.141 Uiso 1 1 calc R . .
N1 N 0.931(8) 0.409(4) 0.4078(12) 0.053(8) Uani 1 1 d . . .
N4 N 0.478(10) 0.289(3) 0.2473(12) 0.077(11) Uani 1 1 d . . .
H4A H 0.3802 0.3651 0.2260 0.092 Uiso 1 1 calc R . .
H4B H 0.4733 0.1896 0.2356 0.092 Uiso 1 1 calc R . .
N2 N 1.091(10) 0.123(3) 0.4154(12) 0.072(10) Uani 1 1 d . . .
C4 C 0.636(9) 0.326(4) 0.2974(14) 0.050(9) Uani 1 1 d . . .
C1 C 0.996(11) 0.002(5) 0.3818(17) 0.084(13) Uani 1 1 d U . .
H1 H 1.0275 -0.1061 0.3930 0.100 Uiso 1 1 calc R . .
N3 N 0.848(8) 0.043(3) 0.3301(13) 0.056(8) Uani 1 1 d . . .
H3 H 0.7936 -0.0176 0.3010 0.067 Uiso 1 1 calc R . .
C3 C 0.809(10) 0.198(4) 0.3358(12) 0.053(9) Uani 1 1 d . . .
C2 C 0.940(9) 0.254(4) 0.3881(14) 0.046(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.30(3) 3_766 ?
Cd1 N1 2.30(3) . ?
Cd1 Cl2 2.618(8) 3_766 ?
Cd1 Cl2 2.618(8) . ?
Cd1 Cl2 2.651(8) 3_866 ?
Cd1 Cl2 2.651(8) 1_455 ?
Cl2 Cd1 2.651(8) 1_655 ?
N5 C4 1.27(4) . ?
N5 C5 1.35(6) . ?
C5 N1 1.25(7) . ?
N1 C2 1.35(4) . ?
N4 C4 1.31(4) . ?
N2 C1 1.30(4) . ?
N2 C2 1.35(4) . ?
C4 C3 1.49(4) . ?
C1 N3 1.34(5) . ?
N3 C3 1.29(4) . ?
C3 C2 1.37(4) . ?

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 180.000(10) 3_766 . ?
N1 Cd1 Cl2 93.2(8) 3_766 3_766 ?
N1 Cd1 Cl2 86.8(8) . 3_766 ?
N1 Cd1 Cl2 86.8(8) 3_766 . ?
N1 Cd1 Cl2 93.2(8) . . ?
Cl2 Cd1 Cl2 180.0(2) 3_766 . ?
N1 Cd1 Cl2 90.3(7) 3_766 3_866 ?
N1 Cd1 Cl2 89.7(7) . 3_866 ?
Cl2 Cd1 Cl2 89.0(3) 3_766 3_866 ?
Cl2 Cd1 Cl2 91.0(3) . 3_866 ?
N1 Cd1 Cl2 89.7(7) 3_766 1_455 ?
N1 Cd1 Cl2 90.3(7) . 1_455 ?
Cl2 Cd1 Cl2 91.0(3) 3_766 1_455 ?
Cl2 Cd1 Cl2 89.0(3) . 1_455 ?
Cl2 Cd1 Cl2 180.000(3) 3_866 1_455 ?
Cd1 Cl2 Cd1 89.0(3) . 1_655 ?
C4 N5 C5 117(3) . . ?
N1 C5 N5 135(4) . . ?
C5 N1 C2 108(3) . . ?
C5 N1 Cd1 121(3) . . ?
C2 N1 Cd1 129(2) . . ?
C1 N2 C2 103(3) . . ?
N5 C4 N4 121(3) . . ?
N5 C4 C3 117(3) . . ?
N4 C4 C3 122(3) . . ?
N2 C1 N3 116(4) . . ?
C3 N3 C1 101(3) . . ?
N3 C3 C2 113(3) . . ?
N3 C3 C4 132(3) . . ?
C2 C3 C4 115(3) . . ?
N2 C2 N1 127(3) . . ?
N2 C2 C3 106(3) . . ?
N1 C2 C3 127(3) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.41
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         4.760
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.350
_database_code_depnum_ccdc_archive 'CCDC 974455'

data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H32 Cd3 N10 O10'
_chemical_formula_weight         933.78

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   9.1560(12)
_cell_length_b                   12.1449(16)
_cell_length_c                   14.1202(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.271(2)
_cell_angle_gamma                90.00
_cell_volume                     1563.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    468
_cell_measurement_theta_min      1.95
_cell_measurement_theta_max      21.76

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             916
_exptl_absorpt_coefficient_mu    2.089
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8415
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3187
_reflns_number_gt                2193
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0988P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3187
_refine_ls_number_parameters     212
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0817
_refine_ls_wR_factor_gt          0.0726
_refine_ls_goodness_of_fit_ref   0.487
_refine_ls_restrained_S_all      0.487
_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 -0.14083(3) 1.12527(2) 0.209579(18) 0.02851(11) Uani 1 1 d . . .
Cd2 Cd 0.0000 1.0000 0.0000 0.02721(12) Uani 1 2 d S . .
N6 N 0.4191(4) 0.5470(3) 0.1171(2) 0.0444(10) Uani 1 1 d . . .
H6A H 0.4817 0.5012 0.0979 0.053 Uiso 1 1 calc R . .
H6B H 0.3944 0.5430 0.1744 0.053 Uiso 1 1 calc R . .
N5 N 0.4039(4) 0.6268(3) -0.0321(2) 0.0347(8) Uani 1 1 d . . .
N2 N 0.1226(4) 0.8533(3) 0.0518(2) 0.0305(8) Uani 1 1 d . . .
C4 C 0.3604(5) 0.6244(3) 0.0582(3) 0.0328(9) Uani 1 1 d . . .
C3 C 0.2622(4) 0.7038(3) 0.0824(3) 0.0290(9) Uani 1 1 d . . .
C2 C 0.2125(4) 0.7806(3) 0.0126(3) 0.0263(8) Uani 1 1 d . . .
N4 N -0.2516(4) 1.2194(3) 0.0786(2) 0.0303(8) Uani 1 1 d . . .
O1 O -0.1987(4) 0.9437(3) 0.0864(2) 0.0542(9) Uani 1 1 d . . .
C6 C -0.3075(5) 0.9414(4) 0.1316(3) 0.0398(11) Uani 1 1 d . . .
N1 N -0.2017(4) 1.2292(2) 0.3338(2) 0.0305(8) Uani 1 1 d . . .
O2 O -0.3267(4) 1.0050(3) 0.1988(2) 0.0546(9) Uani 1 1 d . . .
C5 C 0.3476(5) 0.7019(3) -0.0924(3) 0.0353(10) Uani 1 1 d . . .
H5 H 0.3798 0.6993 -0.1529 0.042 Uiso 1 1 calc R . .
C1 C 0.1222(5) 0.8177(3) 0.1425(3) 0.0352(10) Uani 1 1 d . . .
H1 H 0.0686 0.8536 0.1861 0.042 Uiso 1 1 calc R . .
C7 C -0.4270(6) 0.8602(5) 0.1069(4) 0.084(2) Uani 1 1 d . . .
H7A H -0.4718 0.8751 0.0440 0.126 Uiso 1 1 calc R . .
H7B H -0.4994 0.8661 0.1517 0.126 Uiso 1 1 calc R . .
H7C H -0.3869 0.7871 0.1090 0.126 Uiso 1 1 calc R . .
O10 O 0.0744(3) 1.0973(2) 0.14355(19) 0.0353(7) Uani 1 1 d . . .
O11 O -0.0454(4) 0.9966(3) 0.3277(2) 0.0520(9) Uani 1 1 d D . .
O12 O 0.0711(4) 1.2670(3) 0.1954(2) 0.0539(9) Uani 1 1 d . . .
C21 C 0.1364(5) 1.1903(4) 0.1580(3) 0.0374(10) Uani 1 1 d . . .
C30 C 0.2880(6) 1.2042(6) 0.1304(5) 0.084(2) Uani 1 1 d . . .
H30A H 0.2843 1.2250 0.0646 0.125 Uiso 1 1 calc R . .
H30B H 0.3405 1.1360 0.1398 0.125 Uiso 1 1 calc R . .
H30C H 0.3372 1.2605 0.1689 0.125 Uiso 1 1 calc R . .
C40 C 0.0961(7) 0.9977(5) 0.3747(5) 0.084(2) Uani 1 1 d . . .
H40A H 0.1648 0.9758 0.3298 0.101 Uiso 1 1 calc R . .
H40B H 0.1007 0.9426 0.4246 0.101 Uiso 1 1 calc R . .
C41 C 0.1449(8) 1.1024(5) 0.4170(5) 0.090(2) Uani 1 1 d . . .
H41A H 0.1425 1.1579 0.3684 0.135 Uiso 1 1 calc R . .
H41B H 0.2433 1.0949 0.4462 0.135 Uiso 1 1 calc R . .
H41C H 0.0812 1.1235 0.4641 0.135 Uiso 1 1 calc R . .
H100 H -0.085(6) 0.927(4) 0.317(4) 0.08(2) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O2 2.237(3) . ?
Cd1 N1 2.272(3) . ?
Cd1 O10 2.281(3) . ?
Cd1 N4 2.326(3) . ?
Cd1 O11 2.392(3) . ?
Cd1 O12 2.615(3) . ?
Cd2 N2 2.195(3) 3_575 ?
Cd2 N2 2.195(3) . ?
Cd2 O1 2.382(3) . ?
Cd2 O1 2.382(3) 3_575 ?
Cd2 O10 2.390(3) . ?
Cd2 O10 2.390(3) 3_575 ?
N6 C4 1.335(5) . ?
N5 C5 1.319(5) . ?
N5 C4 1.371(5) . ?
N2 C1 1.352(5) . ?
N2 C2 1.359(5) . ?
C4 C3 1.383(5) . ?
C3 N1 1.386(5) 2_545 ?
C3 C2 1.403(5) . ?
C2 N4 1.367(5) 3_575 ?
N4 C5 1.325(5) 3_575 ?
N4 C2 1.367(5) 3_575 ?
O1 C6 1.232(5) . ?
C6 O2 1.249(5) . ?
C6 C7 1.490(6) . ?
N1 C1 1.323(5) 2 ?
N1 C3 1.386(5) 2 ?
C5 N4 1.325(5) 3_575 ?
C1 N1 1.323(5) 2_545 ?
O10 C21 1.273(5) . ?
O11 C40 1.401(7) . ?
O12 C21 1.250(5) . ?
C21 C30 1.485(6) . ?
C40 C41 1.457(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cd1 N1 100.16(12) . . ?
O2 Cd1 O10 123.71(11) . . ?
N1 Cd1 O10 132.89(11) . . ?
O2 Cd1 N4 89.63(13) . . ?
N1 Cd1 N4 102.78(11) . . ?
O10 Cd1 N4 94.48(11) . . ?
O2 Cd1 O11 81.23(13) . . ?
N1 Cd1 O11 85.68(12) . . ?
O10 Cd1 O11 85.04(12) . . ?
N4 Cd1 O11 168.57(12) . . ?
O2 Cd1 O12 171.75(11) . . ?
N1 Cd1 O12 85.96(11) . . ?
O10 Cd1 O12 52.56(10) . . ?
N4 Cd1 O12 83.58(11) . . ?
O11 Cd1 O12 104.91(12) . . ?
N2 Cd2 N2 180.0 3_575 . ?
N2 Cd2 O1 90.71(12) 3_575 . ?
N2 Cd2 O1 89.29(12) . . ?
N2 Cd2 O1 89.29(12) 3_575 3_575 ?
N2 Cd2 O1 90.71(12) . 3_575 ?
O1 Cd2 O1 180.0 . 3_575 ?
N2 Cd2 O10 88.79(11) 3_575 . ?
N2 Cd2 O10 91.21(11) . . ?
O1 Cd2 O10 83.06(11) . . ?
O1 Cd2 O10 96.94(11) 3_575 . ?
N2 Cd2 O10 91.21(11) 3_575 3_575 ?
N2 Cd2 O10 88.79(11) . 3_575 ?
O1 Cd2 O10 96.94(11) . 3_575 ?
O1 Cd2 O10 83.06(11) 3_575 3_575 ?
O10 Cd2 O10 180.0 . 3_575 ?
C5 N5 C4 119.1(3) . . ?
C1 N2 C2 103.5(3) . . ?
C1 N2 Cd2 122.0(3) . . ?
C2 N2 Cd2 134.5(2) . . ?
N6 C4 N5 117.5(4) . . ?
N6 C4 C3 124.8(4) . . ?
N5 C4 C3 117.8(4) . . ?
C4 C3 N1 133.4(4) . 2_545 ?
C4 C3 C2 117.8(3) . . ?
N1 C3 C2 108.8(3) 2_545 . ?
N2 C2 N4 127.2(3) . 3_575 ?
N2 C2 C3 108.3(3) . . ?
N4 C2 C3 124.5(3) 3_575 . ?
C5 N4 C2 111.9(3) 3_575 3_575 ?
C5 N4 Cd1 118.9(2) 3_575 . ?
C2 N4 Cd1 128.0(2) 3_575 . ?
C6 O1 Cd2 164.6(3) . . ?
O1 C6 O2 123.9(4) . . ?
O1 C6 C7 120.3(4) . . ?
O2 C6 C7 115.8(4) . . ?
C1 N1 C3 102.7(3) 2 2 ?
C1 N1 Cd1 118.6(3) 2 . ?
C3 N1 Cd1 132.9(2) 2 . ?
C6 O2 Cd1 107.2(3) . . ?
N5 C5 N4 128.9(4) . 3_575 ?
N1 C1 N2 116.7(4) 2_545 . ?
C21 O10 Cd1 101.1(3) . . ?
C21 O10 Cd2 131.5(3) . . ?
Cd1 O10 Cd2 103.35(11) . . ?
C40 O11 Cd1 125.9(4) . . ?
C21 O12 Cd1 85.9(3) . . ?
O12 C21 O10 120.4(4) . . ?
O12 C21 C30 121.4(4) . . ?
O10 C21 C30 118.2(4) . . ?
O11 C40 C41 116.0(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.112
_database_code_depnum_ccdc_archive 'CCDC 974456'

data_platon

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H8 Cd4 Cl7 N10'
_chemical_formula_weight         966.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      Orthorhombic
_space_group_IT_number           55
_space_group_name_H-M_alt        'P b a m'
_space_group_name_Hall           '-P 2 2ab'

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

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

_cell_length_a                   14.857(5)
_cell_length_b                   23.615(9)
_cell_length_c                   3.7317(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1309.2(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1206
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      20.47

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.450
_exptl_crystal_F_000             898
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    3.938
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
;
# 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 0.000 0.500 -0.124 142 18 ' '
2 0.500 0.000 -0.127 142 18 ' '
_platon_squeeze_details          
;
Very little remaining electron density was left, 
because of the highly disordered nature of solvent 
molecules.
;


_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6994
_diffrn_reflns_av_unetI/netI     0.1879
_diffrn_reflns_av_R_equivalents  0.1426
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         1.619
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1562
_reflns_number_gt                737
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

 Cations in the pores could not be located. The model shows 
 relatively high R factor, due to the low quality of the
 crystals. ISOR was used for C1 with relative high ADP max/min
 ratio. Some void space remain in the structure, even after
 SQUEEZE was applied.

;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1646P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1562
_refine_ls_number_parameters     95
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.0918
_refine_ls_wR_factor_ref         0.2693
_refine_ls_wR_factor_gt          0.2457
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_restrained_S_all      0.853
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.77229(13) 0.26032(8) 0.5000 0.0376(6) Uani 1 2 d S T P . .
Cl3 Cl 0.7011(5) 0.1963(3) 0.0000 0.0471(18) Uani 1 2 d S T P . .
Cl4 Cl 0.8461(4) 0.3249(3) 0.0000 0.0441(17) Uani 1 2 d S T P . .
Cd2 Cd 0.61063(14) 0.50827(10) 0.5000 0.0593(8) Uani 1 2 d S T P . .
Cl99 Cl 0.7310(6) 0.5177(6) 1.0000 0.106(4) Uani 1 2 d S T P . .
N21 N 0.9388(15) 0.1015(10) 0.5000 0.049(6) Uani 1 2 d S T P . .
N23 N 0.9004(15) 0.1996(14) 0.5000 0.064(8) Uani 1 2 d S T P . .
C2 C 0.523(2) 0.3784(10) 0.5000 0.041(7) Uani 1 2 d S T P . .
C1 C 1.066(2) 0.1733(10) 0.5000 0.047(7) Uani 1 2 d S TU P . .
N24 N 0.6496(13) 0.3243(11) 0.5000 0.042(6) Uani 1 2 d S T P . .
C3 C 0.877(2) 0.1452(14) 0.5000 0.062(10) Uani 1 2 d S T P . .
H3 H 0.8162 0.1361 0.5000 0.075 Uiso 1 2 calc R U P . .
N20 N 1.0191(15) 0.2752(10) 0.5000 0.061(7) Uani 1 2 d S T P . .
H20A H 1.0738 0.2871 0.5000 0.073 Uiso 1 2 calc R U P . .
H20B H 0.9754 0.2992 0.5000 0.073 Uiso 1 2 calc R U P . .
C4 C 1.0011(14) 0.2173(10) 0.5000 0.023(5) Uani 1 2 d S T P . .
N50 N 0.5964(15) 0.4132(9) 0.5000 0.045(6) Uani 1 2 d S T P . .
C20 C 0.674(2) 0.3777(13) 0.5000 0.051(8) Uani 1 2 d S T P . .
H20 H 0.7329 0.3905 0.5000 0.061 Uiso 1 2 calc R U P . .
Cl98 Cl 0.5000 0.5000 0.0000 0.201(14) Uani 1 4 d S T P . .


_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 N24 2.37(2) . ?
Cd1 N23 2.38(2) . ?
Cd1 Cl3 2.624(5) 1_556 ?
Cd1 Cl3 2.624(5) . ?
Cd1 Cl4 2.648(5) . ?
Cd1 Cl4 2.649(5) 1_556 ?
Cl3 Cd1 2.624(5) 1_554 ?
Cl4 Cd1 2.648(5) 1_554 ?
Cd2 N50 2.25(2) . ?
Cd2 N21 2.32(3) 3_656 ?
Cd2 Cl98 2.4942(15) . ?
Cd2 Cl98 2.4942(15) 1_556 ?
Cd2 Cl99 2.594(7) . ?
Cd2 Cl99 2.594(7) 1_554 ?
Cd2 Cd2 3.310(4) 5_666 ?
Cl99 Cd2 2.594(7) 1_556 ?
N21 C2 1.33(3) 7_665 ?
N21 C3 1.38(3) . ?
N21 Cd2 2.32(3) 3_646 ?
N23 C3 1.33(4) . ?
N23 C4 1.55(3) . ?
C2 N21 1.33(3) 7_565 ?
C2 N50 1.37(3) . ?
C2 C1 1.38(3) 7_565 ?
C1 N24 1.25(3) 7_665 ?
C1 C2 1.38(3) 7_665 ?
C1 C4 1.41(3) . ?
C1 C20 2.01(4) 7_665 ?
N24 C1 1.25(3) 7_565 ?
N24 C20 1.31(4) . ?
N20 C4 1.39(3) . ?
N50 C20 1.42(3) . ?
C20 C1 2.01(4) 7_565 ?
Cl98 Cd2 2.4942(15) 5_665 ?
Cl98 Cd2 2.4942(15) 5_666 ?
Cl98 Cd2 2.4942(15) 1_554 ?

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
N24 Cd1 N23 177.3(10) . . ?
N24 Cd1 Cl3 93.3(4) . 1_556 ?
N23 Cd1 Cl3 88.6(6) . 1_556 ?
N24 Cd1 Cl3 93.3(4) . . ?
N23 Cd1 Cl3 88.6(6) . . ?
Cl3 Cd1 Cl3 90.7(2) 1_556 . ?
N24 Cd1 Cl4 87.2(4) . . ?
N23 Cd1 Cl4 90.9(6) . . ?
Cl3 Cd1 Cl4 179.25(19) 1_556 . ?
Cl3 Cd1 Cl4 89.88(16) . . ?
N24 Cd1 Cl4 87.2(4) . 1_556 ?
N23 Cd1 Cl4 90.9(6) . 1_556 ?
Cl3 Cd1 Cl4 89.88(16) 1_556 1_556 ?
Cl3 Cd1 Cl4 179.25(19) . 1_556 ?
Cl4 Cd1 Cl4 89.6(2) . 1_556 ?
Cd1 Cl3 Cd1 90.7(2) . 1_554 ?
Cd1 Cl4 Cd1 89.6(2) 1_554 . ?
N50 Cd2 N21 156.2(7) . 3_656 ?
N50 Cd2 Cl98 82.0(4) . . ?
N21 Cd2 Cl98 82.3(3) 3_656 . ?
N50 Cd2 Cl98 82.0(4) . 1_556 ?
N21 Cd2 Cl98 82.3(3) 3_656 1_556 ?
Cl98 Cd2 Cl98 96.85(8) . 1_556 ?
N50 Cd2 Cl99 98.6(5) . . ?
N21 Cd2 Cl99 97.9(5) 3_656 . ?
Cl98 Cd2 Cl99 177.56(16) . . ?
Cl98 Cd2 Cl99 85.58(15) 1_556 . ?
N50 Cd2 Cl99 98.6(5) . 1_554 ?
N21 Cd2 Cl99 97.9(5) 3_656 1_554 ?
Cl98 Cd2 Cl99 85.58(15) . 1_554 ?
Cl98 Cd2 Cl99 177.56(16) 1_556 1_554 ?
Cl99 Cd2 Cl99 92.0(3) . 1_554 ?
N50 Cd2 Cd2 77.8(5) . 5_666 ?
N21 Cd2 Cd2 78.3(5) 3_656 5_666 ?
Cl98 Cd2 Cd2 48.42(4) . 5_666 ?
Cl98 Cd2 Cd2 48.42(4) 1_556 5_666 ?
Cl99 Cd2 Cd2 134.00(15) . 5_666 ?
Cl99 Cd2 Cd2 134.00(15) 1_554 5_666 ?
Cd2 Cl99 Cd2 92.0(3) 1_556 . ?
C2 N21 C3 111(3) 7_665 . ?
C2 N21 Cd2 129.3(17) 7_665 3_646 ?
C3 N21 Cd2 120(2) . 3_646 ?
C3 N23 C4 121(2) . . ?
C3 N23 Cd1 112(2) . . ?
C4 N23 Cd1 127(2) . . ?
N21 C2 N50 122(2) 7_565 . ?
N21 C2 C1 139(3) 7_565 7_565 ?
N50 C2 C1 99(2) . 7_565 ?
N24 C1 C2 120(3) 7_665 7_665 ?
N24 C1 C4 130(2) 7_665 . ?
C2 C1 C4 109(3) 7_665 . ?
N24 C1 C20 39.4(17) 7_665 7_665 ?
C2 C1 C20 80.8(19) 7_665 7_665 ?
C4 C1 C20 170(2) . 7_665 ?
C1 N24 C20 103(3) 7_565 . ?
C1 N24 Cd1 143(2) 7_565 . ?
C20 N24 Cd1 113.8(17) . . ?
N23 C3 N21 123(3) . . ?
N20 C4 C1 126(2) . . ?
N20 C4 N23 117(2) . . ?
C1 C4 N23 117(2) . . ?
C2 N50 C20 107(2) . . ?
C2 N50 Cd2 132.2(16) . . ?
C20 N50 Cd2 120.8(19) . . ?
N24 C20 N50 110(2) . . ?
N24 C20 C1 37.2(14) . 7_565 ?
N50 C20 C1 73.1(16) . 7_565 ?
Cd2 Cl98 Cd2 180.0 . 5_665 ?
Cd2 Cl98 Cd2 83.15(8) . 5_666 ?
Cd2 Cl98 Cd2 96.85(8) 5_665 5_666 ?
Cd2 Cl98 Cd2 96.85(8) . 1_554 ?
Cd2 Cl98 Cd2 83.15(8) 5_665 1_554 ?
Cd2 Cl98 Cd2 180.00(11) 5_666 1_554 ?

_refine_diff_density_max         1.767
_refine_diff_density_min         -1.960
_refine_diff_density_rms         0.384

_shelxl_version_number           2013-2



_database_code_depnum_ccdc_archive 'CCDC 974457'
