# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 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_1
_database_code_depnum_ccdc_archive 'CCDC 1051320'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

# SQUEEZE RESULTS (APPEND TO CIF)
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 0.250 0.000 -0.037 374 41 ' '
2 0.750 0.000 -0.030 374 41 ' '
3 0.250 0.500 -0.044 374 41 ' '
4 0.750 0.500 -0.031 374 41 ' '
_platon_squeeze_details          
;
The 164 electrons were removed from the unit-cell 
contents by using SQUEEZE process, which is equivalent
to 20.5 electrons per asymmetric unit. As the formula 
unit is composed of two asymmetric units, this implies 
that 41 electrons should be associated with the 
disordered solvent. The total electrons (40 electrons)
with the contribution of disorder solvents
including 0.5 DMF and two water molecules are 
consistent with the SQUEEZE results.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28.50 H25.5 Cd2 Cl N9.50 O8.50'
_chemical_formula_weight         897.34

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'
Cd Cd -0.8075 1.2024 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   25.786(5)
_cell_length_b                   21.045(4)
_cell_length_c                   7.4123(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4022.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle-like
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7065
_exptl_absorpt_correction_T_max  0.7359
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku R-AXIS SPIDER'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            27144
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4047
_reflns_number_gt                3338
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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)+(0.0498P)²+11.6548P] 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         4047
_refine_ls_number_parameters     230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1287
_refine_ls_wR_factor_gt          0.1243
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_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 0.43286(2) 0.2500 0.67260(7) 0.03676(17) Uani 1 2 d S . .
Cd2 Cd 0.48602(2) 0.2500 1.23166(7) 0.03804(17) Uani 1 2 d S . .
Cl1 Cl 0.41117(8) 0.2500 1.0087(3) 0.0476(5) Uani 1 2 d S . .
N1 N 0.44009(18) -0.0806(2) 0.0151(6) 0.0434(11) Uani 1 1 d . . .
N2 N 0.4125(2) -0.0822(3) -0.1417(7) 0.0616(15) Uani 1 1 d . . .
N3 N 0.46738(17) -0.1641(2) -0.1272(6) 0.0419(11) Uani 1 1 d . . .
N4 N 0.7620(3) 0.2500 0.8678(10) 0.066(2) Uani 1 2 d S . .
N5 N 0.7729(3) 0.2500 1.0473(12) 0.127(6) Uani 1 2 d S . .
N6 N 0.8457(3) 0.2500 0.8858(10) 0.060(2) Uani 1 2 d S . .
O1 O 0.43751(15) 0.18334(19) 0.4239(5) 0.0475(10) Uani 1 1 d . . .
O2 O 0.43660(19) 0.1218(2) 0.6649(5) 0.0617(12) Uani 1 1 d . . .
O3 O 0.5186(2) 0.2500 0.7389(7) 0.0492(14) Uani 1 2 d S . .
O4 O 0.5473(2) 0.2500 0.4514(7) 0.0525(15) Uani 1 2 d S . .
C1 C 0.4297(3) -0.1336(3) -0.2209(9) 0.0538(16) Uani 1 1 d . . .
H1A H 0.4172 -0.1479 -0.3314 0.065 Uiso 1 1 calc R . .
C2 C 0.4724(2) -0.1292(3) 0.0193(7) 0.0414(13) Uani 1 1 d . . .
H2A H 0.4955 -0.1376 0.1126 0.050 Uiso 1 1 calc R . .
C3 C 0.4354(2) -0.0288(3) 0.1381(8) 0.0452(13) Uani 1 1 d . . .
C4 C 0.4413(3) -0.0391(3) 0.3220(8) 0.0561(16) Uani 1 1 d . . .
H4A H 0.4459 -0.0801 0.3663 0.067 Uiso 1 1 calc R . .
C5 C 0.4401(3) 0.0119(3) 0.4378(8) 0.0530(15) Uani 1 1 d . . .
H5A H 0.4446 0.0053 0.5609 0.064 Uiso 1 1 calc R . .
C6 C 0.4323(2) 0.0729(3) 0.3732(7) 0.0424(13) Uani 1 1 d . . .
C7 C 0.4236(2) 0.0813(3) 0.1889(8) 0.0467(14) Uani 1 1 d . . .
H7A H 0.4166 0.1218 0.1446 0.056 Uiso 1 1 calc R . .
C8 C 0.4251(2) 0.0308(3) 0.0722(8) 0.0478(14) Uani 1 1 d . . .
H8A H 0.4193 0.0369 -0.0504 0.057 Uiso 1 1 calc R . .
C9 C 0.4357(2) 0.1290(3) 0.4975(8) 0.0420(13) Uani 1 1 d . . .
C10 C 0.8237(4) 0.2500 1.0479(14) 0.111(6) Uani 1 2 d S . .
H10A H 0.8430 0.2500 1.1540 0.133 Uiso 1 2 calc SR . .
C11 C 0.8061(3) 0.2500 0.7789(12) 0.065(3) Uani 1 2 d S . .
H11A H 0.8085 0.2500 0.6537 0.078 Uiso 1 2 calc SR . .
C13 C 0.6704(3) 0.2500 0.9323(12) 0.055(2) Uani 1 2 d S . .
H13A H 0.6776 0.2500 1.0552 0.066 Uiso 1 2 calc SR . .
C14 C 0.6192(3) 0.2500 0.8685(10) 0.0427(19) Uani 1 2 d S . .
H14A H 0.5918 0.2500 0.9501 0.051 Uiso 1 2 calc SR . .
C15 C 0.6093(3) 0.2500 0.6869(11) 0.046(2) Uani 1 2 d S . .
C16 C 0.6483(3) 0.2500 0.5635(13) 0.076(4) Uani 1 2 d S . .
H16A H 0.6410 0.2500 0.4406 0.091 Uiso 1 2 calc SR . .
C17 C 0.6988(4) 0.2500 0.6236(13) 0.111(6) Uani 1 2 d S . .
H17A H 0.7261 0.2500 0.5416 0.133 Uiso 1 2 calc SR . .
C18 C 0.7088(3) 0.2500 0.8095(12) 0.055(2) Uani 1 2 d S . .
C19 C 0.5537(3) 0.2500 0.6198(11) 0.0413(19) 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
Cd1 O3 2.264(5) . ?
Cd1 N6 2.288(7) 6_557 ?
Cd1 O1 2.319(4) . ?
Cd1 O1 2.319(4) 7_565 ?
Cd1 Cl1 2.553(2) . ?
Cd2 O4 2.269(5) 1_556 ?
Cd2 N3 2.305(5) 3_656 ?
Cd2 N3 2.305(5) 5_656 ?
Cd2 O1 2.359(4) 7_566 ?
Cd2 O1 2.359(4) 1_556 ?
Cd2 Cl1 2.541(2) . ?
N1 C2 1.320(7) . ?
N1 N2 1.363(7) . ?
N1 C3 1.427(7) . ?
N2 C1 1.308(8) . ?
N3 C2 1.317(7) . ?
N3 C1 1.357(7) . ?
N3 Cd2 2.305(5) 5_656 ?
N4 C11 1.314(11) . ?
N4 N5 1.360(11) . ?
N4 C18 1.439(10) . ?
N5 C10 1.310(12) . ?
N6 C11 1.292(11) . ?
N6 C10 1.329(12) . ?
N6 Cd1 2.288(7) 6_657 ?
O1 C9 1.267(7) . ?
O1 Cd2 2.359(4) 1_554 ?
O2 C9 1.250(7) . ?
O3 C19 1.265(9) . ?
O4 C19 1.259(9) . ?
O4 Cd2 2.269(5) 1_554 ?
C3 C8 1.372(8) . ?
C3 C4 1.389(8) . ?
C4 C5 1.374(9) . ?
C5 C6 1.386(8) . ?
C6 C7 1.396(8) . ?
C6 C9 1.500(8) . ?
C7 C8 1.371(8) . ?
C13 C18 1.345(12) . ?
C13 C14 1.402(10) . ?
C14 C15 1.370(11) . ?
C15 C16 1.360(11) . ?
C15 C19 1.516(9) . ?
C16 C17 1.376(12) . ?
C17 C18 1.402(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cd1 N6 178.4(2) . 6_557 ?
O3 Cd1 O1 97.01(15) . . ?
N6 Cd1 O1 84.29(18) 6_557 . ?
O3 Cd1 O1 97.01(15) . 7_565 ?
N6 Cd1 O1 84.29(18) 6_557 7_565 ?
O1 Cd1 O1 74.4(2) . 7_565 ?
O3 Cd1 Cl1 90.12(15) . . ?
N6 Cd1 Cl1 88.24(19) 6_557 . ?
O1 Cd1 Cl1 141.88(10) . . ?
O1 Cd1 Cl1 141.88(10) 7_565 . ?
O4 Cd2 N3 83.02(14) 1_556 3_656 ?
O4 Cd2 N3 83.02(14) 1_556 5_656 ?
N3 Cd2 N3 103.3(2) 3_656 5_656 ?
O4 Cd2 O1 86.29(15) 1_556 7_566 ?
N3 Cd2 O1 90.75(15) 3_656 7_566 ?
N3 Cd2 O1 161.09(15) 5_656 7_566 ?
O4 Cd2 O1 86.29(15) 1_556 1_556 ?
N3 Cd2 O1 161.09(15) 3_656 1_556 ?
N3 Cd2 O1 90.75(15) 5_656 1_556 ?
O1 Cd2 O1 72.98(19) 7_566 1_556 ?
O4 Cd2 Cl1 174.68(15) 1_556 . ?
N3 Cd2 Cl1 100.22(12) 3_656 . ?
N3 Cd2 Cl1 100.22(12) 5_656 . ?
O1 Cd2 Cl1 89.43(11) 7_566 . ?
O1 Cd2 Cl1 89.43(11) 1_556 . ?
Cd2 Cl1 Cd1 117.92(8) . . ?
C2 N1 N2 109.3(5) . . ?
C2 N1 C3 129.1(5) . . ?
N2 N1 C3 121.3(5) . . ?
C1 N2 N1 103.1(5) . . ?
C2 N3 C1 103.2(5) . . ?
C2 N3 Cd2 131.5(4) . 5_656 ?
C1 N3 Cd2 124.9(4) . 5_656 ?
C11 N4 N5 108.2(7) . . ?
C11 N4 C18 132.4(8) . . ?
N5 N4 C18 119.4(7) . . ?
C10 N5 N4 102.2(8) . . ?
C11 N6 C10 102.5(8) . . ?
C11 N6 Cd1 131.3(6) . 6_657 ?
C10 N6 Cd1 126.2(6) . 6_657 ?
C9 O1 Cd1 101.6(3) . . ?
C9 O1 Cd2 144.6(4) . 1_554 ?
Cd1 O1 Cd2 98.50(15) . 1_554 ?
C19 O3 Cd1 123.2(5) . . ?
C19 O4 Cd2 143.5(5) . 1_554 ?
N2 C1 N3 113.8(5) . . ?
N1 C2 N3 110.5(5) . . ?
C8 C3 C4 120.9(6) . . ?
C8 C3 N1 119.2(5) . . ?
C4 C3 N1 119.9(6) . . ?
C5 C4 C3 119.2(6) . . ?
C4 C5 C6 120.8(6) . . ?
C5 C6 C7 118.6(6) . . ?
C5 C6 C9 120.6(5) . . ?
C7 C6 C9 120.7(5) . . ?
C8 C7 C6 121.0(6) . . ?
C7 C8 C3 119.3(5) . . ?
O2 C9 O1 122.4(6) . . ?
O2 C9 C6 121.0(6) . . ?
O1 C9 C6 116.6(5) . . ?
N5 C10 N6 115.0(9) . . ?
N6 C11 N4 112.1(8) . . ?
C18 C13 C14 117.7(8) . . ?
C15 C14 C13 120.5(7) . . ?
C16 C15 C14 121.4(7) . . ?
C16 C15 C19 118.6(7) . . ?
C14 C15 C19 120.0(7) . . ?
C15 C16 C17 118.8(9) . . ?
C16 C17 C18 119.5(9) . . ?
C13 C18 C17 121.9(8) . . ?
C13 C18 N4 120.0(8) . . ?
C17 C18 N4 118.1(8) . . ?
O4 C19 O3 126.7(7) . . ?
O4 C19 C15 116.8(7) . . ?
O3 C19 C15 116.6(7) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.109
