# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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
_audit_block_doi                 10.5517/cc1j4p1d
_database_code_depnum_ccdc_archive 'CCDC 1404673'
_audit_update_record             
;
2015-09-21 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H61 Cd3 N28 O12'
_chemical_formula_weight         1499.39

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

_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+1/2, -y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.044(3)
_cell_length_b                   20.297(4)
_cell_length_c                   23.635(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6737(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    46595
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      28.1

_exptl_crystal_description       slice
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_F_000             3020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.010
_shelx_estimated_absorpt_T_min   0.824
_shelx_estimated_absorpt_T_max   0.906
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  SCX-MINI
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5939
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.965
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5939
_reflns_number_gt                3758
_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.
;

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1257P)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         5939
_refine_ls_number_parameters     278
_refine_ls_number_restraints     203
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0818
_refine_ls_wR_factor_ref         0.2257
_refine_ls_wR_factor_gt          0.2123
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
N13 N 0.4796(5) 0.7040(4) 1.0832(3) 0.043(2) Uani 1 1 d . U . . .
C16 C 0.5646(8) 0.6832(6) 1.0805(5) 0.068(3) Uani 1 1 d . U . . .
H16 H 0.5923 0.6708 1.1147 0.082 Uiso 1 1 calc R U . . .
C15 C 0.4410(8) 0.7206(7) 1.0333(5) 0.070(4) Uani 1 1 d . U . . .
H15 H 0.3793 0.7372 1.0328 0.084 Uiso 1 1 calc R U . . .
Cd1 Cd 0.89999(5) 0.73070(4) 0.83136(3) 0.0339(3) Uani 1 1 d . U . . .
Cd2 Cd 0.65567(7) 0.7500 0.7500 0.0322(3) Uani 1 2 d S TU P . .
O1 O 0.8155(8) 0.7500 0.7500 0.072(3) Uani 1 2 d S TU P . .
N1 N 0.8870(6) 0.8427(4) 0.8565(3) 0.044(2) Uani 1 1 d . U . . .
N2 N 0.8814(8) 0.8639(5) 0.9071(4) 0.072(3) Uani 1 1 d . U . . .
N3 N 0.8749(7) 0.9287(5) 0.9041(4) 0.071(3) Uani 1 1 d . U . . .
N4 N 0.8846(5) 0.8910(4) 0.8181(3) 0.042(2) Uani 1 1 d . U . . .
N5 N 0.8553(6) 1.1433(4) 0.7886(3) 0.0387(18) Uani 1 1 d . U . . .
N9 N 0.7504(6) 0.7023(4) 0.8719(3) 0.046(2) Uani 1 1 d . U . . .
N10 N 0.6675(6) 0.7072(4) 0.8432(3) 0.044(2) Uani 1 1 d . U . . .
N11 N 0.5938(5) 0.7039(4) 0.8782(3) 0.044(2) Uani 1 1 d . U . . .
N12 N 0.7294(5) 0.6938(5) 0.9263(3) 0.050(2) Uani 1 1 d . U . . .
N6 N 1.0392(6) 0.7525(4) 0.7793(3) 0.048(2) Uani 1 1 d . U . . .
N7 N 1.1275(6) 0.7494(5) 0.7973(4) 0.060(3) Uani 1 1 d . U . . .
N8 N 1.4861(7) 0.7500 0.7500 0.044(3) Uani 1 2 d S TU P . .
O2 O 0.9208(6) 0.6209(4) 0.8012(3) 0.067(2) Uani 1 1 d . U . . .
C1 C 0.8811(7) 0.9448(5) 0.8499(4) 0.041(2) Uani 1 1 d . U . . .
C2 C 0.8742(7) 1.0129(5) 0.8287(4) 0.047(3) Uani 1 1 d . U . . .
C3 C 0.8654(8) 1.0653(5) 0.8658(4) 0.060(3) Uani 1 1 d . U . . .
H3 H 0.8655 1.0581 0.9046 0.072 Uiso 1 1 calc R U . . .
C4 C 0.8712(10) 1.0285(6) 0.7700(5) 0.073(4) Uani 1 1 d . U . . .
H4 H 0.8732 0.9954 0.7428 0.087 Uiso 1 1 calc R U . . .
C5 C 0.8564(9) 1.1295(6) 0.8443(4) 0.060(3) Uani 1 1 d . U . . .
H5 H 0.8509 1.1642 0.8698 0.072 Uiso 1 1 calc R U . . .
C6 C 0.8654(10) 1.0916(6) 0.7547(4) 0.065(3) Uani 1 1 d . U . . .
H6 H 0.8688 1.1004 0.7162 0.078 Uiso 1 1 calc R U . . .
C11 C 0.6340(6) 0.6964(5) 0.9305(3) 0.035(2) Uani 1 1 d . U . . .
C12 C 0.5807(5) 0.6947(4) 0.9821(3) 0.028(2) Uani 1 1 d . U . . .
C13 C 0.4879(7) 0.7143(6) 0.9835(4) 0.057(3) Uani 1 1 d . U . . .
H13 H 0.4564 0.7234 0.9498 0.069 Uiso 1 1 calc R U . . .
C14 C 0.6221(8) 0.6766(6) 1.0319(4) 0.059(3) Uani 1 1 d . U . . .
H14 H 0.6842 0.6609 1.0337 0.070 Uiso 1 1 calc R U . . .
C7 C 1.1804(9) 0.7500 0.7500 0.043(3) Uani 1 2 d S TU P . .
C8 C 1.2839(10) 0.7500 0.7500 0.041(3) Uani 1 2 d S TU P . .
C10 C 1.4370(8) 0.7644(5) 0.7969(5) 0.055(3) Uani 1 1 d . U . . .
H10 H 1.4701 0.7747 0.8298 0.066 Uiso 1 1 calc R U . . .
C9 C 1.3406(10) 0.7644(7) 0.7980(6) 0.085(4) Uani 1 1 d . U . . .
H9 H 1.3101 0.7743 0.8319 0.102 Uiso 1 1 calc R U . . .


_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
N13 C16 1.268(13) . ?
N13 C15 1.341(14) . ?
N13 Cd1 2.371(7) 6_557 ?
C16 C14 1.411(13) . ?
C16 H16 0.9300 . ?
C15 C13 1.355(13) . ?
C15 H15 0.9300 . ?
Cd1 O1 2.294(6) . ?
Cd1 N6 2.352(8) . ?
Cd1 O2 2.357(7) . ?
Cd1 N1 2.357(8) . ?
Cd1 N13 2.371(7) 6_657 ?
Cd1 N9 2.380(8) . ?
Cd2 O1 2.244(11) . ?
Cd2 N5 2.355(7) 4_646 ?
Cd2 N5 2.355(7) 2_675 ?
Cd2 N10 2.374(8) 3_566 ?
Cd2 N10 2.374(8) . ?
Cd2 N8 2.382(10) 1_455 ?
O1 Cd1 2.294(6) 3_566 ?
N1 N2 1.274(10) . ?
N1 N4 1.336(11) . ?
N2 N3 1.319(12) . ?
N3 C1 1.325(11) . ?
N4 C1 1.326(12) . ?
N5 C6 1.326(12) . ?
N5 C5 1.346(11) . ?
N5 Cd2 2.355(7) 2_675 ?
N9 N12 1.330(10) . ?
N9 N10 1.351(11) . ?
N10 N11 1.327(10) . ?
N11 C11 1.367(10) . ?
N12 C11 1.345(11) . ?
N6 N7 1.312(11) . ?
N6 N6 1.389(15) 3_566 ?
N7 C7 1.342(11) . ?
N8 C10 1.337(13) 3_566 ?
N8 C10 1.337(13) . ?
N8 Cd2 2.382(10) 1_655 ?
C1 C2 1.473(14) . ?
C2 C3 1.385(14) . ?
C2 C4 1.424(14) . ?
C3 C5 1.403(15) . ?
C3 H3 0.9300 . ?
C4 C6 1.333(16) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C11 C12 1.432(11) . ?
C12 C14 1.363(12) . ?
C12 C13 1.363(12) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C7 N7 1.342(11) 3_566 ?
C7 C8 1.454(18) . ?
C8 C9 1.416(16) 3_566 ?
C8 C9 1.416(16) . ?
C10 C9 1.355(17) . ?
C10 H10 0.9300 . ?
C9 H9 0.9300 . ?

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
C16 N13 C15 114.9(9) . . ?
C16 N13 Cd1 124.2(8) . 6_557 ?
C15 N13 Cd1 120.1(6) . 6_557 ?
N13 C16 C14 127.6(11) . . ?
N13 C16 H16 116.2 . . ?
C14 C16 H16 116.2 . . ?
N13 C15 C13 122.9(11) . . ?
N13 C15 H15 118.5 . . ?
C13 C15 H15 118.5 . . ?
O1 Cd1 N6 87.7(3) . . ?
O1 Cd1 O2 88.43(18) . . ?
N6 Cd1 O2 85.2(3) . . ?
O1 Cd1 N1 90.39(19) . . ?
N6 Cd1 N1 90.8(3) . . ?
O2 Cd1 N1 175.9(3) . . ?
O1 Cd1 N13 175.7(3) . 6_657 ?
N6 Cd1 N13 95.5(3) . 6_657 ?
O2 Cd1 N13 89.0(3) . 6_657 ?
N1 Cd1 N13 92.4(3) . 6_657 ?
O1 Cd1 N9 85.5(3) . . ?
N6 Cd1 N9 171.9(3) . . ?
O2 Cd1 N9 90.1(3) . . ?
N1 Cd1 N9 93.7(3) . . ?
N13 Cd1 N9 91.0(3) 6_657 . ?
O1 Cd2 N5 93.76(19) . 4_646 ?
O1 Cd2 N5 93.76(19) . 2_675 ?
N5 Cd2 N5 172.5(4) 4_646 2_675 ?
O1 Cd2 N10 85.98(19) . 3_566 ?
N5 Cd2 N10 89.0(3) 4_646 3_566 ?
N5 Cd2 N10 91.6(3) 2_675 3_566 ?
O1 Cd2 N10 85.98(19) . . ?
N5 Cd2 N10 91.6(3) 4_646 . ?
N5 Cd2 N10 89.0(3) 2_675 . ?
N10 Cd2 N10 172.0(4) 3_566 . ?
O1 Cd2 N8 180.0 . 1_455 ?
N5 Cd2 N8 86.24(19) 4_646 1_455 ?
N5 Cd2 N8 86.24(19) 2_675 1_455 ?
N10 Cd2 N8 94.02(19) 3_566 1_455 ?
N10 Cd2 N8 94.02(19) . 1_455 ?
Cd2 O1 Cd1 121.2(2) . . ?
Cd2 O1 Cd1 121.2(2) . 3_566 ?
Cd1 O1 Cd1 117.7(5) . 3_566 ?
N2 N1 N4 112.8(8) . . ?
N2 N1 Cd1 124.6(7) . . ?
N4 N1 Cd1 122.6(6) . . ?
N1 N2 N3 106.9(8) . . ?
N2 N3 C1 107.0(9) . . ?
C1 N4 N1 102.7(8) . . ?
C6 N5 C5 115.1(9) . . ?
C6 N5 Cd2 120.0(6) . 2_675 ?
C5 N5 Cd2 124.8(7) . 2_675 ?
N12 N9 N10 107.7(7) . . ?
N12 N9 Cd1 128.1(6) . . ?
N10 N9 Cd1 122.7(5) . . ?
N11 N10 N9 110.8(7) . . ?
N11 N10 Cd2 122.9(6) . . ?
N9 N10 Cd2 123.6(6) . . ?
N10 N11 C11 104.4(7) . . ?
N9 N12 C11 106.7(7) . . ?
N7 N6 N6 108.6(6) . 3_566 ?
N7 N6 Cd1 127.4(6) . . ?
N6 N6 Cd1 120.5(3) 3_566 . ?
N6 N7 C7 104.7(9) . . ?
C10 N8 C10 117.9(13) 3_566 . ?
C10 N8 Cd2 121.0(6) 3_566 1_655 ?
C10 N8 Cd2 121.0(6) . 1_655 ?
N4 C1 N3 110.3(9) . . ?
N4 C1 C2 125.5(9) . . ?
N3 C1 C2 123.8(9) . . ?
C3 C2 C4 116.3(10) . . ?
C3 C2 C1 120.8(9) . . ?
C4 C2 C1 122.9(9) . . ?
C2 C3 C5 119.5(10) . . ?
C2 C3 H3 120.2 . . ?
C5 C3 H3 120.2 . . ?
C6 C4 C2 118.6(11) . . ?
C6 C4 H4 120.7 . . ?
C2 C4 H4 120.7 . . ?
N5 C5 C3 123.2(10) . . ?
N5 C5 H5 118.4 . . ?
C3 C5 H5 118.4 . . ?
C4 C6 N5 127.1(10) . . ?
C4 C6 H6 116.5 . . ?
N5 C6 H6 116.5 . . ?
N12 C11 N11 110.4(7) . . ?
N12 C11 C12 125.7(8) . . ?
N11 C11 C12 123.9(7) . . ?
C14 C12 C13 117.8(8) . . ?
C14 C12 C11 121.3(8) . . ?
C13 C12 C11 120.8(8) . . ?
C15 C13 C12 120.8(10) . . ?
C15 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C12 C14 C16 115.7(9) . . ?
C12 C14 H14 122.2 . . ?
C16 C14 H14 122.2 . . ?
N7 C7 N7 112.7(12) 3_566 . ?
N7 C7 C8 123.6(6) 3_566 . ?
N7 C7 C8 123.6(6) . . ?
C9 C8 C9 111.6(16) 3_566 . ?
C9 C8 C7 124.2(8) 3_566 . ?
C9 C8 C7 124.2(8) . . ?
N8 C10 C9 122.1(12) . . ?
N8 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 C9 C8 123.1(14) . . ?
C10 C9 H9 118.4 . . ?
C8 C9 H9 118.4 . . ?

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
C15 N13 C16 C14 0.9(19) . . . . ?
Cd1 N13 C16 C14 -168.6(10) 6_557 . . . ?
C16 N13 C15 C13 1.5(18) . . . . ?
Cd1 N13 C15 C13 171.5(9) 6_557 . . . ?
N4 N1 N2 N3 0.0(13) . . . . ?
Cd1 N1 N2 N3 -179.9(7) . . . . ?
N1 N2 N3 C1 -2.6(13) . . . . ?
N2 N1 N4 C1 2.7(11) . . . . ?
Cd1 N1 N4 C1 -177.5(6) . . . . ?
N12 N9 N10 N11 1.8(11) . . . . ?
Cd1 N9 N10 N11 -165.1(6) . . . . ?
N12 N9 N10 Cd2 163.4(6) . . . . ?
Cd1 N9 N10 Cd2 -3.5(10) . . . . ?
N9 N10 N11 C11 -0.2(11) . . . . ?
Cd2 N10 N11 C11 -162.0(6) . . . . ?
N10 N9 N12 C11 -2.6(11) . . . . ?
Cd1 N9 N12 C11 163.3(6) . . . . ?
N6 N6 N7 C7 6.6(12) 3_566 . . . ?
Cd1 N6 N7 C7 165.4(5) . . . . ?
N1 N4 C1 N3 -4.3(11) . . . . ?
N1 N4 C1 C2 -178.0(9) . . . . ?
N2 N3 C1 N4 4.5(13) . . . . ?
N2 N3 C1 C2 178.3(10) . . . . ?
N4 C1 C2 C3 176.2(10) . . . . ?
N3 C1 C2 C3 3.3(17) . . . . ?
N4 C1 C2 C4 -0.4(17) . . . . ?
N3 C1 C2 C4 -173.3(12) . . . . ?
C4 C2 C3 C5 -1.4(17) . . . . ?
C1 C2 C3 C5 -178.2(10) . . . . ?
C3 C2 C4 C6 3.5(19) . . . . ?
C1 C2 C4 C6 -179.7(11) . . . . ?
C6 N5 C5 C3 -1.3(17) . . . . ?
Cd2 N5 C5 C3 -178.4(9) 2_675 . . . ?
C2 C3 C5 N5 0.4(18) . . . . ?
C2 C4 C6 N5 -5(2) . . . . ?
C5 N5 C6 C4 3.9(19) . . . . ?
Cd2 N5 C6 C4 -178.9(11) 2_675 . . . ?
N9 N12 C11 N11 2.6(12) . . . . ?
N9 N12 C11 C12 -174.9(9) . . . . ?
N10 N11 C11 N12 -1.5(11) . . . . ?
N10 N11 C11 C12 176.1(9) . . . . ?
N12 C11 C12 C14 -13.7(16) . . . . ?
N11 C11 C12 C14 169.2(10) . . . . ?
N12 C11 C12 C13 163.1(11) . . . . ?
N11 C11 C12 C13 -14.0(15) . . . . ?
N13 C15 C13 C12 -5(2) . . . . ?
C14 C12 C13 C15 5.3(17) . . . . ?
C11 C12 C13 C15 -171.6(11) . . . . ?
C13 C12 C14 C16 -2.9(16) . . . . ?
C11 C12 C14 C16 173.9(10) . . . . ?
N13 C16 C14 C12 0(2) . . . . ?
N6 N7 C7 N7 -2.6(5) . . . 3_566 ?
N6 N7 C7 C8 177.4(5) . . . . ?
N7 C7 C8 C9 -15.0(8) 3_566 . . 3_566 ?
N7 C7 C8 C9 165.0(8) . . . 3_566 ?
N7 C7 C8 C9 165.0(8) 3_566 . . . ?
N7 C7 C8 C9 -15.0(8) . . . . ?
C10 N8 C10 C9 0.3(9) 3_566 . . . ?
Cd2 N8 C10 C9 -179.7(9) 1_655 . . . ?
N8 C10 C9 C8 -0.6(18) . . . . ?
C9 C8 C9 C10 0.3(8) 3_566 . . . ?
C7 C8 C9 C10 -179.7(8) . . . . ?

_refine_diff_density_max         1.666
_refine_diff_density_min         -2.074
_refine_diff_density_rms         0.163


# 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 -0.007 0.000 0.007 1751 642 ' '
2 0.009 0.500 0.547 1748 636 ' '
_platon_squeeze_details          
;
The total potential solvent accessible void indicate more
solvent molecules can reside in the crystal structure. Based on the TG
and elemental analysis, two DMF molecules and one dimethylamine cation 
were included in the final molecules.
;
####################################################################### 
# 
# 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_2
_audit_block_doi                 10.5517/cc1j4p2f
_database_code_depnum_ccdc_archive 'CCDC 1404674'
_audit_update_record             
;
2015-09-21 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C61 H74 Cd5 N42 O13'
_chemical_formula_weight         2165.62

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6177(19)
_cell_length_b                   12.5869(18)
_cell_length_c                   28.561(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.843(2)
_cell_angle_gamma                90
_cell_volume                     4503.6(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    113
_cell_measurement_reflns_used    15763
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      28.7

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_F_000             2156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    1.239
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      113
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42658
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.770
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_full        25.005
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7926
_reflns_number_gt                7846
_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.
;

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalClear (Rigaku Inc., 2008)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1662P)²+577.4791P] 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         7926
_refine_ls_number_parameters     450
_refine_ls_number_restraints     442
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.1205
_refine_ls_wR_factor_ref         0.3058
_refine_ls_wR_factor_gt          0.3052
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_restrained_S_all      0.854
_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
Cd01 Cd 0.56519(9) 0.33108(9) 0.61115(4) 0.0047(3) Uani 1 1 d . U . . .
Cd02 Cd 0.35593(9) 0.54014(9) 0.60876(4) 0.0053(3) Uani 1 1 d . U . . .
Cd03 Cd 0.5000 0.5000 0.5000 0.0070(3) Uani 1 2 d S U P . .
O2 O 0.4419(9) 0.4281(9) 0.5637(4) 0.0067(6) Uani 1 1 d . U . . .
N4 N 0.9758(11) 0.0663(11) 0.8463(5) 0.0102(12) Uani 1 1 d . U . . .
N14 N 0.5271(11) 0.7656(11) 0.5331(5) 0.0086(8) Uani 1 1 d . U . . .
N3 N 0.8998(11) -0.0086(11) 0.8454(5) 0.0099(12) Uani 1 1 d . U . . .
N5 N 0.9454(11) 0.1366(11) 0.8118(5) 0.0099(11) Uani 1 1 d . U . . .
N1 N 0.6796(11) 0.2430(11) 0.6701(5) 0.0073(9) Uani 1 1 d . U . . .
N17 N 0.3231(11) 0.5288(11) 0.4608(5) 0.0089(8) Uani 1 1 d . U . . .
N15 N 0.5251(12) 1.1594(12) 0.5790(5) 0.0110(12) Uani 1 1 d . U . . .
N8 N 0.0799(11) 0.8123(12) 0.8414(5) 0.0107(12) Uani 1 1 d . U . . .
N10 N 0.2128(11) 0.8708(12) 0.8076(5) 0.0106(11) Uani 1 1 d . U . . .
N11 N 0.3899(11) 0.7835(11) 0.5742(5) 0.0085(8) Uani 1 1 d . U . . .
N13 N 0.4818(11) 0.6687(11) 0.5362(5) 0.0077(7) Uani 1 1 d . U . . .
N19 N 0.2015(11) 0.6288(12) 0.4236(5) 0.0094(10) Uani 1 1 d . U . . .
N9 N 0.1517(11) 0.8881(11) 0.8419(5) 0.0106(12) Uani 1 1 d . U . . .
N12 N 0.4021(11) 0.6808(11) 0.5615(5) 0.0076(7) Uani 1 1 d . U . . .
C17 C 0.8529(13) 0.1010(13) 0.7922(6) 0.0093(11) Uani 1 1 d . U . . .
N2 N 0.8214(11) 0.0128(11) 0.8120(5) 0.0100(11) Uani 1 1 d . U . . .
C00Q C 0.1578(13) 0.5438(14) 0.4431(6) 0.0099(10) Uani 1 1 d . U . . .
C11 C 0.1740(13) 0.7795(14) 0.7873(6) 0.0103(11) Uani 1 1 d . U . . .
N7 N 0.0917(11) 0.7426(12) 0.8087(5) 0.0108(11) Uani 1 1 d . U . . .
C13 C 0.8303(13) 0.2432(13) 0.7292(6) 0.0087(10) Uani 1 1 d . U . . .
H13 H 0.8918 0.2769 0.7430 0.010 Uiso 1 1 calc R U . . .
N6 N 0.2808(11) 0.6433(11) 0.6645(5) 0.0077(9) Uani 1 1 d . U . . .
C14 C 0.7927(13) 0.1504(13) 0.7503(6) 0.0093(11) Uani 1 1 d . U . . .
C15 C 0.6942(13) 0.1107(13) 0.7310(6) 0.0088(10) Uani 1 1 d . U . . .
H15 H 0.6631 0.0537 0.7450 0.011 Uiso 1 1 calc R U . . .
N16 N 0.2302(11) 0.4812(11) 0.4663(5) 0.0095(9) Uani 1 1 d . U . . .
C2 C -0.0297(14) 0.6083(14) 0.4228(6) 0.0108(11) Uani 1 1 d . U . . .
H2 H -0.0033 0.6753 0.4168 0.013 Uiso 1 1 calc R U . . .
N18 N 0.3047(11) 0.6153(11) 0.4362(5) 0.0089(9) Uani 1 1 d . U . . .
C3 C 0.0398(13) 0.5289(13) 0.4374(6) 0.0101(10) Uani 1 1 d . U . . .
C20 C 0.6003(14) 1.1000(14) 0.5633(6) 0.0105(11) Uani 1 1 d . U . . .
H20 H 0.6645 1.1320 0.5583 0.013 Uiso 1 1 calc R U . . .
C18 C 0.4120(14) 1.0104(14) 0.5771(6) 0.0104(11) Uani 1 1 d . U . . .
H18 H 0.3459 0.9823 0.5818 0.012 Uiso 1 1 calc R U . . .
C22 C 0.4913(13) 0.9443(13) 0.5625(6) 0.0096(9) Uani 1 1 d . U . . .
C12 C 0.7758(13) 0.2828(13) 0.6888(6) 0.0083(10) Uani 1 1 d . U . . .
H12 H 0.8054 0.3388 0.6735 0.010 Uiso 1 1 calc R U . . .
N20 N -0.1794(12) 0.4931(12) 0.4232(5) 0.0113(12) Uani 1 1 d . U . . .
C19 C 0.4322(14) 1.1166(14) 0.5844(6) 0.0105(11) Uani 1 1 d . U . . .
H19 H 0.3785 1.1598 0.5936 0.013 Uiso 1 1 calc R U . . .
C21 C 0.5875(13) 0.9924(14) 0.5540(6) 0.0104(10) Uani 1 1 d . U . . .
C7 C 0.2137(13) 0.7327(13) 0.7467(6) 0.0103(11) Uani 1 1 d . U . . .
C01B C 0.4698(13) 0.8312(13) 0.5563(6) 0.0093(9) Uani 1 1 d . U . . .
C8 C 0.1645(13) 0.6421(13) 0.7249(6) 0.0092(10) Uani 1 1 d . U . . .
H8 H 0.1077 0.6103 0.7375 0.011 Uiso 1 1 calc R U . . .
C5 C -0.1129(13) 0.4150(14) 0.4381(6) 0.0109(11) Uani 1 1 d . U . . .
H5 H -0.1412 0.3488 0.4440 0.013 Uiso 1 1 calc R U . . .
C6 C 0.2957(13) 0.7772(14) 0.7245(6) 0.0094(10) Uani 1 1 d . U . . .
H6 H 0.3287 0.8392 0.7365 0.011 Uiso 1 1 calc R U . . .
C16 C 0.6440(13) 0.1575(13) 0.6909(6) 0.0080(10) Uani 1 1 d . U . . .
H16 H 0.5805 0.1273 0.6773 0.010 Uiso 1 1 calc R U . . .
C9 C 0.1993(13) 0.6012(14) 0.6856(6) 0.0090(10) Uani 1 1 d . U . . .
H9 H 0.1656 0.5407 0.6723 0.011 Uiso 1 1 calc R U . . .
C1 C -0.1369(14) 0.5916(14) 0.4169(6) 0.0108(11) Uani 1 1 d . U . . .
H1 H -0.1825 0.6483 0.4084 0.013 Uiso 1 1 calc R U . . .
C10 C 0.3286(13) 0.7303(13) 0.6849(6) 0.0090(10) Uani 1 1 d . U . . .
H10 H 0.3859 0.7600 0.6719 0.011 Uiso 1 1 calc R U . . .
C4 C -0.0053(13) 0.4281(14) 0.4451(6) 0.0107(11) Uani 1 1 d . U . . .
H4 H 0.0387 0.3711 0.4549 0.013 Uiso 1 1 calc R U . . .
C1AA C 0.2905(12) 0.2866(12) 0.5153(5) 0.0041(18) Uani 1 1 d . U . . .
H1AA H 0.3207 0.2166 0.5150 0.006 Uiso 1 1 calc R U . . .
H1AB H 0.2241 0.2883 0.4950 0.006 Uiso 1 1 calc R U . . .
H1AC H 0.2782 0.3045 0.5469 0.006 Uiso 1 1 calc R U . . .
O1 O 0.3659(9) 0.3647(9) 0.4982(4) 0.0107(8) Uani 1 1 d . U . . .


_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
Cd01 O2 2.290(11) . ?
Cd01 N18 2.348(14) 3_666 ?
Cd01 N1 2.360(14) . ?
Cd01 N15 2.379(15) 1_545 ?
Cd01 N3 2.383(14) 2_656 ?
Cd01 N8 2.415(14) 2_546 ?
Cd02 O2 2.271(11) . ?
Cd02 N6 2.340(14) . ?
Cd02 N20 2.342(15) 3_566 ?
Cd02 N12 2.341(14) . ?
Cd02 N4 2.370(14) 2_656 ?
Cd02 N9 2.387(14) 2_546 ?
Cd03 O2 2.232(11) 3_666 ?
Cd03 O2 2.232(11) . ?
Cd03 O1 2.397(12) 3_666 ?
Cd03 O1 2.397(12) . ?
Cd03 N17 2.402(14) 3_666 ?
Cd03 N17 2.402(14) . ?
Cd03 N13 2.384(14) 3_666 ?
Cd03 N13 2.384(14) . ?
N4 N5 1.35(2) . ?
N4 N3 1.34(2) . ?
N4 Cd02 2.370(14) 2_646 ?
N14 C01B 1.33(2) . ?
N14 N13 1.35(2) . ?
N3 N2 1.32(2) . ?
N3 Cd01 2.383(14) 2_646 ?
N5 C17 1.31(2) . ?
N1 C16 1.33(2) . ?
N1 C12 1.36(2) . ?
N17 N18 1.30(2) . ?
N17 N16 1.34(2) . ?
N15 C19 1.32(2) . ?
N15 C20 1.33(2) . ?
N15 Cd01 2.379(15) 1_565 ?
N8 N9 1.31(2) . ?
N8 N7 1.30(2) . ?
N8 Cd01 2.416(14) 2_556 ?
N10 N9 1.33(2) . ?
N10 C11 1.35(2) . ?
N11 N12 1.36(2) . ?
N11 C01B 1.33(2) . ?
N13 N12 1.32(2) . ?
N19 N18 1.32(2) . ?
N19 C00Q 1.35(2) . ?
N9 Cd02 2.387(14) 2_556 ?
C17 N2 1.33(2) . ?
C17 C14 1.48(2) . ?
C00Q N16 1.32(2) . ?
C00Q C3 1.49(2) . ?
C11 N7 1.35(2) . ?
C11 C7 1.44(2) . ?
C13 C12 1.37(2) . ?
C13 C14 1.42(2) . ?
C13 H13 0.9300 . ?
N6 C10 1.35(2) . ?
N6 C9 1.36(2) . ?
C14 C15 1.39(2) . ?
C15 C16 1.37(2) . ?
C15 H15 0.9300 . ?
C2 C3 1.36(2) . ?
C2 C1 1.36(2) . ?
C2 H2 0.9300 . ?
N18 Cd01 2.348(14) 3_666 ?
C3 C4 1.42(2) . ?
C20 C21 1.39(2) . ?
C20 H20 0.9300 . ?
C18 C19 1.37(3) . ?
C18 C22 1.40(2) . ?
C18 H18 0.9300 . ?
C22 C21 1.40(2) . ?
C22 C01B 1.46(2) . ?
C12 H12 0.9300 . ?
N20 C5 1.33(2) . ?
N20 C1 1.37(2) . ?
N20 Cd02 2.342(14) 3_566 ?
C19 H19 0.9300 . ?
C7 C6 1.39(2) . ?
C7 C8 1.41(2) . ?
C8 C9 1.36(2) . ?
C8 H8 0.9300 . ?
C5 C4 1.36(2) . ?
C5 H5 0.9300 . ?
C6 C10 1.38(2) . ?
C6 H6 0.9300 . ?
C16 H16 0.9300 . ?
C9 H9 0.9300 . ?
C1 H1 0.9300 . ?
C10 H10 0.9300 . ?
C4 H4 0.9300 . ?
C1AA O1 1.490(19) . ?
C1AA H1AA 0.9600 . ?
C1AA H1AB 0.9600 . ?
C1AA H1AC 0.9600 . ?

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 Cd01 N18 88.7(4) . 3_666 ?
O2 Cd01 N1 170.9(4) . . ?
N18 Cd01 N1 97.8(5) 3_666 . ?
O2 Cd01 N15 99.0(5) . 1_545 ?
N18 Cd01 N15 99.8(5) 3_666 1_545 ?
N1 Cd01 N15 86.2(5) . 1_545 ?
O2 Cd01 N3 85.9(4) . 2_656 ?
N18 Cd01 N3 87.6(5) 3_666 2_656 ?
N1 Cd01 N3 88.1(5) . 2_656 ?
N15 Cd01 N3 171.2(5) 1_545 2_656 ?
O2 Cd01 N8 83.0(4) . 2_546 ?
N18 Cd01 N8 168.6(5) 3_666 2_546 ?
N1 Cd01 N8 89.6(5) . 2_546 ?
N15 Cd01 N8 89.3(5) 1_545 2_546 ?
N3 Cd01 N8 84.0(5) 2_656 2_546 ?
O2 Cd02 N6 171.8(4) . . ?
O2 Cd02 N20 99.5(5) . 3_566 ?
N6 Cd02 N20 85.5(5) . 3_566 ?
O2 Cd02 N12 88.5(4) . . ?
N6 Cd02 N12 96.9(5) . . ?
N20 Cd02 N12 101.6(5) 3_566 . ?
O2 Cd02 N4 86.3(4) . 2_656 ?
N6 Cd02 N4 87.9(5) . 2_656 ?
N20 Cd02 N4 170.1(5) 3_566 2_656 ?
N12 Cd02 N4 86.5(5) . 2_656 ?
O2 Cd02 N9 83.8(4) . 2_546 ?
N6 Cd02 N9 89.7(5) . 2_546 ?
N20 Cd02 N9 89.1(5) 3_566 2_546 ?
N12 Cd02 N9 167.8(5) . 2_546 ?
N4 Cd02 N9 83.5(5) 2_656 2_546 ?
O2 Cd03 O2 180.0 3_666 . ?
O2 Cd03 O1 55.2(4) 3_666 3_666 ?
O2 Cd03 O1 124.8(4) . 3_666 ?
O2 Cd03 O1 124.8(4) 3_666 . ?
O2 Cd03 O1 55.2(4) . . ?
O1 Cd03 O1 180.0 3_666 . ?
O2 Cd03 N17 93.6(4) 3_666 3_666 ?
O2 Cd03 N17 86.4(4) . 3_666 ?
O1 Cd03 N17 58.9(4) 3_666 3_666 ?
O1 Cd03 N17 121.1(4) . 3_666 ?
O2 Cd03 N17 86.4(4) 3_666 . ?
O2 Cd03 N17 93.6(4) . . ?
O1 Cd03 N17 121.1(4) 3_666 . ?
O1 Cd03 N17 58.9(4) . . ?
N17 Cd03 N17 180.0 3_666 . ?
O2 Cd03 N13 87.1(4) 3_666 3_666 ?
O2 Cd03 N13 92.9(4) . 3_666 ?
O1 Cd03 N13 122.5(4) 3_666 3_666 ?
O1 Cd03 N13 57.5(4) . 3_666 ?
N17 Cd03 N13 86.3(5) 3_666 3_666 ?
N17 Cd03 N13 93.7(5) . 3_666 ?
O2 Cd03 N13 92.9(4) 3_666 . ?
O2 Cd03 N13 87.1(4) . . ?
O1 Cd03 N13 57.5(4) 3_666 . ?
O1 Cd03 N13 122.5(4) . . ?
N17 Cd03 N13 93.7(5) 3_666 . ?
N17 Cd03 N13 86.3(5) . . ?
N13 Cd03 N13 180.0(6) 3_666 . ?
Cd03 O2 Cd02 115.8(5) . . ?
Cd03 O2 Cd01 115.7(5) . . ?
Cd02 O2 Cd01 109.4(4) . . ?
N5 N4 N3 107.9(13) . . ?
N5 N4 Cd02 130.3(11) . 2_646 ?
N3 N4 Cd02 120.3(10) . 2_646 ?
C01B N14 N13 105.7(13) . . ?
N2 N3 N4 110.1(14) . . ?
N2 N3 Cd01 128.8(11) . 2_646 ?
N4 N3 Cd01 119.8(10) . 2_646 ?
C17 N5 N4 104.4(14) . . ?
C16 N1 C12 117.0(14) . . ?
C16 N1 Cd01 119.2(11) . . ?
C12 N1 Cd01 123.2(11) . . ?
N18 N17 N16 109.5(13) . . ?
N18 N17 Cd03 118.3(10) . . ?
N16 N17 Cd03 130.9(10) . . ?
C19 N15 C20 119.5(15) . . ?
C19 N15 Cd01 118.5(12) . 1_565 ?
C20 N15 Cd01 120.9(11) . 1_565 ?
N9 N8 N7 111.0(14) . . ?
N9 N8 Cd01 119.4(11) . 2_556 ?
N7 N8 Cd01 128.8(11) . 2_556 ?
N9 N10 C11 104.0(14) . . ?
N12 N11 C01B 102.3(13) . . ?
N12 N13 N14 106.7(13) . . ?
N12 N13 Cd03 117.4(10) . . ?
N14 N13 Cd03 135.3(10) . . ?
N18 N19 C00Q 102.8(13) . . ?
N8 N9 N10 109.4(14) . . ?
N8 N9 Cd02 120.8(11) . 2_556 ?
N10 N9 Cd02 129.2(11) . 2_556 ?
N13 N12 N11 112.1(13) . . ?
N13 N12 Cd02 119.2(10) . . ?
N11 N12 Cd02 121.5(10) . . ?
N5 C17 N2 113.6(15) . . ?
N5 C17 C14 123.2(15) . . ?
N2 C17 C14 123.2(15) . . ?
N3 N2 C17 104.0(14) . . ?
N16 C00Q N19 112.7(15) . . ?
N16 C00Q C3 127.0(16) . . ?
N19 C00Q C3 120.3(15) . . ?
N7 C11 N10 110.9(15) . . ?
N7 C11 C7 125.8(16) . . ?
N10 C11 C7 123.2(15) . . ?
N8 N7 C11 104.7(14) . . ?
C12 C13 C14 119.9(16) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C10 N6 C9 116.6(14) . . ?
C10 N6 Cd02 123.3(11) . . ?
C9 N6 Cd02 118.2(11) . . ?
C15 C14 C13 117.1(15) . . ?
C15 C14 C17 121.2(15) . . ?
C13 C14 C17 121.6(15) . . ?
C16 C15 C14 118.5(16) . . ?
C16 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
C00Q N16 N17 103.7(14) . . ?
C3 C2 C1 121.3(17) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
N19 N18 N17 111.2(14) . . ?
N19 N18 Cd01 122.7(10) . 3_666 ?
N17 N18 Cd01 117.4(10) . 3_666 ?
C2 C3 C4 116.6(15) . . ?
C2 C3 C00Q 122.7(16) . . ?
C4 C3 C00Q 120.6(15) . . ?
N15 C20 C21 122.9(16) . . ?
N15 C20 H20 118.6 . . ?
C21 C20 H20 118.6 . . ?
C19 C18 C22 119.8(16) . . ?
C19 C18 H18 120.1 . . ?
C22 C18 H18 120.1 . . ?
C21 C22 C18 117.3(15) . . ?
C21 C22 C01B 123.6(16) . . ?
C18 C22 C01B 119.1(15) . . ?
N1 C12 C13 122.1(16) . . ?
N1 C12 H12 118.9 . . ?
C13 C12 H12 118.9 . . ?
C5 N20 C1 118.0(15) . . ?
C5 N20 Cd02 121.8(12) . 3_566 ?
C1 N20 Cd02 118.6(11) . 3_566 ?
N15 C19 C18 122.1(17) . . ?
N15 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
C22 C21 C20 118.2(16) . . ?
C6 C7 C8 115.8(15) . . ?
C6 C7 C11 123.4(16) . . ?
C8 C7 C11 120.6(15) . . ?
N14 C01B N11 113.2(15) . . ?
N14 C01B C22 124.5(15) . . ?
N11 C01B C22 122.3(15) . . ?
C9 C8 C7 120.4(16) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
N20 C5 C4 122.6(17) . . ?
N20 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C10 C6 C7 120.8(16) . . ?
C10 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
N1 C16 C15 124.9(16) . . ?
N1 C16 H16 117.6 . . ?
C15 C16 H16 117.6 . . ?
C8 C9 N6 123.7(16) . . ?
C8 C9 H9 118.1 . . ?
N6 C9 H9 118.1 . . ?
N20 C1 C2 121.5(16) . . ?
N20 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
N6 C10 C6 122.6(16) . . ?
N6 C10 H10 118.7 . . ?
C6 C10 H10 118.7 . . ?
C5 C4 C3 119.9(16) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
O1 C1AA H1AA 109.5 . . ?
O1 C1AA H1AB 109.5 . . ?
H1AA C1AA H1AB 109.5 . . ?
O1 C1AA H1AC 109.5 . . ?
H1AA C1AA H1AC 109.5 . . ?
H1AB C1AA H1AC 109.5 . . ?
C1AA O1 Cd03 159.8(9) . . ?

_refine_diff_density_max         6.714
_refine_diff_density_min         -5.527
_refine_diff_density_rms         0.522

# 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 -0.016 0.561 0.236 1878 1657 ' '
_platon_squeeze_details          
;
The total potential solvent accessible void is 1878 eA3, indicating more
solvent molecules can reside in the crystal structure. Based on the TG
and elemental analysis, two DMF molecules and one dimethylamine cation 
were included in the final molecules.
;
####################################################################### 
# 
# 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_3
_audit_block_doi                 10.5517/cc1j4p3g
_database_code_depnum_ccdc_archive 'CCDC 1404675'
_audit_update_record             
;
2015-09-21 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C115 H132 Cd9 N76 O21'
_chemical_formula_weight         3926.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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                   39.073(8)
_cell_length_b                   19.229(4)
_cell_length_c                   13.798(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.60(3)
_cell_angle_gamma                90
_cell_volume                     10076(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    273
_cell_measurement_theta_min      4.3
_cell_measurement_theta_max      26.2

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_F_000             3908
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.996
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  SCX-MINI
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43831
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_av_R_equivalents  0.1025
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.141
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_full        25.047
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9205
_reflns_number_gt                6762
_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. The structure was restricted by the orders of DELU and ISOR.
;

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0759P)²+30.2968P] 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         9205
_refine_ls_number_parameters     438
_refine_ls_number_restraints     350
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1531
_refine_ls_wR_factor_gt          0.1413
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.055
_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
C13 C 0.1297(2) 0.7967(4) 0.8358(6) 0.053(2) Uani 1 1 d . U . . .
H13 H 0.1421 0.7617 0.8756 0.063 Uiso 1 1 calc R U . . .
C14 C 0.1020(3) 0.8411(4) 0.6821(6) 0.068(3) Uani 1 1 d . U . . .
H14 H 0.0952 0.8386 0.6130 0.081 Uiso 1 1 calc R U . . .
C16 C 0.0951(3) 0.8979(4) 0.7294(6) 0.063(3) Uani 1 1 d . U . . .
H16 H 0.0824 0.9334 0.6914 0.076 Uiso 1 1 calc R U . . .
C11 C 0.12558(19) 0.7229(4) 0.6868(5) 0.0347(17) Uani 1 1 d . U . . .
C4 C 0.2957(3) 0.5000 0.9619(9) 0.051(3) Uani 1 2 d S TU P . .
H4 H 0.2763 0.5000 0.9902 0.062 Uiso 1 2 calc R U P . .
C5 C 0.3530(3) 0.5000 0.8898(9) 0.050(3) Uani 1 2 d S TU P . .
H5 H 0.3730 0.5000 0.8643 0.061 Uiso 1 2 calc R U P . .
C12 C 0.1191(2) 0.7870(4) 0.7355(5) 0.0398(19) Uani 1 1 d . U . . .
C23 C 0.0892(2) 0.2124(4) 0.2042(6) 0.043(2) Uani 1 1 d . U . . .
C26 C 0.0756(2) 0.1567(4) 0.1345(6) 0.0394(19) Uani 1 1 d . U . . .
C20 C -0.0303(2) 0.5000 0.6150(7) 0.030(2) Uani 1 2 d S TU P . .
C6 C 0.3285(3) 0.5000 1.0202(8) 0.043(3) Uani 1 2 d S TU P . .
H6 H 0.3308 0.5000 1.0888 0.052 Uiso 1 2 calc R U P . .
C2 C 0.2910(3) 0.5000 0.8600(9) 0.044(3) Uani 1 2 d S TU P . .
C3 C 0.3209(3) 0.5000 0.8258(8) 0.047(3) Uani 1 2 d S TU P . .
H3 H 0.3192 0.5000 0.7574 0.056 Uiso 1 2 calc R U P . .
C17 C 0.0618(2) 0.4446(5) 0.6499(8) 0.064(3) Uani 1 1 d . U . . .
H17 H 0.0736 0.4022 0.6571 0.076 Uiso 1 1 calc R U . . .
C18 C 0.0264(2) 0.4431(5) 0.6312(8) 0.067(3) Uani 1 1 d . U . . .
H18 H 0.0148 0.4008 0.6175 0.081 Uiso 1 1 calc R U . . .
C24 C 0.1224(2) 0.2343(5) 0.2182(7) 0.065(3) Uani 1 1 d . U . . .
H24 H 0.1374 0.2146 0.1827 0.078 Uiso 1 1 calc R U . . .
C22 C 0.0681(2) 0.2453(5) 0.2546(7) 0.066(3) Uani 1 1 d . U . . .
H22 H 0.0446 0.2324 0.2459 0.079 Uiso 1 1 calc R U . . .
C19 C 0.0080(2) 0.5000 0.6317(7) 0.030(2) Uani 1 2 d S TU P . .
C25 C 0.1339(2) 0.2858(5) 0.2852(7) 0.070(3) Uani 1 1 d . U . . .
H25 H 0.1573 0.2992 0.2965 0.084 Uiso 1 1 calc R U . . .
C9 C 0.1485(3) 0.5000 1.0602(8) 0.039(3) Uani 1 2 d S TU P . .
C8 C 0.1514(4) 0.4442(6) 1.0110(8) 0.112(4) Uani 1 1 d . U . . .
H8 H 0.1557 0.4020 1.0446 0.135 Uiso 1 1 calc R U . . .
C7 C 0.1481(4) 0.4461(6) 0.9054(8) 0.110(4) Uani 1 1 d . U . . .
H7 H 0.1481 0.4039 0.8726 0.132 Uiso 1 1 calc R U . . .
C21 C 0.0820(2) 0.2975(5) 0.3185(7) 0.067(3) Uani 1 1 d . U . . .
H21 H 0.0672 0.3201 0.3523 0.080 Uiso 1 1 calc R U . . .
C28 C 0.0216(3) 0.0000 0.2679(10) 0.085(5) Uani 1 2 d DS TU P . .
H28A H 0.0281 -0.0451 0.2960 0.127 Uiso 0.5 1 calc R U P . .
H28B H 0.0257 0.0342 0.3201 0.127 Uiso 0.5 1 calc R U P . .
H28C H 0.0355 0.0110 0.2211 0.127 Uiso 0.5 1 calc R U P . .
C27 C -0.0175(2) 0.0000 0.2145(7) 0.025(2) Uani 1 2 d DS TU P . .
C15 C 0.1225(2) 0.8558(4) 0.8778(6) 0.050(2) Uani 1 1 d . U . . .
H15 H 0.1301 0.8606 0.9466 0.060 Uiso 1 1 calc R U . . .
C1 C 0.2576(3) 0.5000 0.7928(8) 0.044(3) Uani 1 2 d S TU P . .
Cd1 Cd 0.14263(2) 0.5000 0.68679(5) 0.02060(18) Uani 1 2 d S TU P . .
Cd3 Cd 0.0000 0.0000 0.0000 0.0273(2) Uani 1 4 d S TU P . .
Cd2 Cd 0.13513(2) 0.40686(2) 0.43848(3) 0.02415(15) Uani 1 1 d . U . . .
Cd4 Cd 0.08573(2) 1.0000 0.90764(5) 0.02357(18) Uani 1 2 d S TU P . .
N9 N 0.13818(14) 0.6208(3) 0.6678(4) 0.0286(13) Uani 1 1 d . U . . .
N10 N 0.13682(15) 0.6666(3) 0.7358(4) 0.0321(14) Uani 1 1 d . U . . .
N11 N 0.12818(16) 0.6488(3) 0.5804(4) 0.0326(14) Uani 1 1 d . U . . .
N12 N 0.12027(18) 0.7146(3) 0.5909(5) 0.0470(17) Uani 1 1 d . U . . .
N13 N 0.10520(17) 0.9070(3) 0.8267(4) 0.0379(15) Uani 1 1 d . U . . .
N19 N 0.04333(15) 0.0809(3) 0.0548(5) 0.0381(15) Uani 1 1 d . U . . .
N17 N 0.11397(17) 0.3174(3) 0.3345(5) 0.0415(16) Uani 1 1 d . U . . .
N8 N 0.14723(17) 0.5329(3) 1.3036(4) 0.0403(16) Uani 1 1 d . U . . .
N7 N 0.14845(19) 0.5549(4) 1.2153(4) 0.0511(18) Uani 1 1 d . U . . .
N20 N 0.07260(15) 0.0806(3) 0.0262(4) 0.0354(14) Uani 1 1 d . U . . .
N18 N 0.04435(16) 0.1289(3) 0.1240(5) 0.0442(17) Uani 1 1 d . U . . .
N21 N 0.09362(15) 0.1285(3) 0.0756(5) 0.0423(16) Uani 1 1 d . U . . .
N16 N -0.08161(14) 0.4662(3) 0.5923(4) 0.0283(13) Uani 1 1 d . U . . .
N15 N -0.04913(14) 0.4441(3) 0.6069(4) 0.0359(14) Uani 1 1 d . U . . .
N5 N 0.35676(19) 0.5000 0.9889(6) 0.0301(19) Uani 1 2 d S TU P . .
N3 N 0.2271(2) 0.5000 0.8173(6) 0.043(2) Uani 1 2 d S TU P . .
N4 N 0.2536(3) 0.5000 0.6959(8) 0.073(3) Uani 1 2 d S TU P . .
N14 N 0.0802(2) 0.5000 0.6585(6) 0.035(2) Uani 1 2 d S TU P . .
N1 N 0.2031(2) 0.5000 0.7305(7) 0.046(2) Uani 1 2 d S TU P . .
N6 N 0.1453(2) 0.5000 0.8545(6) 0.040(2) Uani 1 2 d S TU P . .
N2 N 0.2183(3) 0.5000 0.6602(8) 0.069(3) Uani 1 2 d S TU P . .
O1 O 0.15295(15) 0.5000 0.5316(4) 0.0204(13) Uani 1 2 d S TU P . .
O3 O -0.02529(18) 0.0000 0.1309(6) 0.0468(19) Uani 1 2 d DS TU P . .
O4 O -0.0379(3) 0.0000 0.2709(7) 0.087(3) Uani 1 2 d S TU P . .
O2 O 0.1939(2) 0.3558(4) 0.4726(5) 0.113(3) Uani 1 1 d . U . . .
C10 C 0.1483(3) 0.5000 1.1626(6) 0.028(2) Uani 1 2 d S TU 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
C13 C15 1.336(10) . ?
C13 C12 1.360(10) . ?
C13 H13 0.9300 . ?
C14 C16 1.332(11) . ?
C14 C12 1.356(11) . ?
C14 H14 0.9300 . ?
C16 N13 1.320(10) . ?
C16 H16 0.9300 . ?
C11 N10 1.298(9) . ?
C11 N12 1.301(9) . ?
C11 C12 1.454(10) . ?
C4 C6 1.345(15) . ?
C4 C2 1.375(15) . ?
C4 H4 0.9300 . ?
C5 N5 1.340(13) . ?
C5 C3 1.354(15) . ?
C5 H5 0.9300 . ?
C23 C24 1.334(11) . ?
C23 C22 1.354(11) . ?
C23 C26 1.455(10) . ?
C26 N21 1.309(9) . ?
C26 N18 1.310(9) . ?
C20 N15 1.291(7) 6_565 ?
C20 N15 1.291(7) . ?
C20 C19 1.460(13) . ?
C6 N5 1.275(12) . ?
C6 H6 0.9300 . ?
C2 C3 1.356(14) . ?
C2 C1 1.414(14) . ?
C3 H3 0.9300 . ?
C17 N14 1.277(9) . ?
C17 C18 1.345(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.310(10) . ?
C18 H18 0.9300 . ?
C24 C25 1.356(11) . ?
C24 H24 0.9300 . ?
C22 C21 1.362(11) . ?
C22 H22 0.9300 . ?
C19 C18 1.310(10) 6_565 ?
C25 N17 1.298(10) . ?
C25 H25 0.9300 . ?
C9 C8 1.288(12) 6_565 ?
C9 C8 1.288(12) . ?
C9 C10 1.415(13) . ?
C8 C7 1.433(14) . ?
C8 H8 0.9300 . ?
C7 N6 1.242(12) . ?
C7 H7 0.9300 . ?
C21 N17 1.277(10) . ?
C21 H21 0.9300 . ?
C28 C27 1.531(8) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C27 O3 1.121(8) . ?
C27 O4 1.238(12) . ?
C15 N13 1.304(9) . ?
C15 H15 0.9300 . ?
C1 N4 1.309(14) . ?
C1 N3 1.311(13) . ?
Cd1 O1 2.271(5) . ?
Cd1 N6 2.292(8) . ?
Cd1 N1 2.299(8) . ?
Cd1 N9 2.339(5) 6_565 ?
Cd1 N9 2.339(5) . ?
Cd1 N14 2.377(8) . ?
Cd3 O3 2.254(8) 5 ?
Cd3 O3 2.254(8) . ?
Cd3 N19 2.293(6) 5 ?
Cd3 N19 2.293(6) 6 ?
Cd3 N19 2.293(6) 2 ?
Cd3 N19 2.293(6) . ?
Cd2 O1 2.219(3) . ?
Cd2 N17 2.268(6) . ?
Cd2 N11 2.303(5) 6_565 ?
Cd2 N16 2.331(5) 2_556 ?
Cd2 N8 2.333(5) 6_564 ?
Cd2 O2 2.439(8) . ?
Cd4 O3 2.296(7) 5_566 ?
Cd4 N13 2.328(6) 6_575 ?
Cd4 N13 2.328(5) . ?
Cd4 N5 2.362(8) 7_567 ?
Cd4 N20 2.395(5) 1_566 ?
Cd4 N20 2.395(6) 6_566 ?
N9 N11 1.294(7) . ?
N9 N10 1.298(7) . ?
N11 N12 1.318(8) . ?
N11 Cd2 2.303(5) 6_565 ?
N19 N20 1.295(8) . ?
N19 N18 1.322(8) . ?
N8 N8 1.265(11) 6_565 ?
N8 N7 1.302(8) . ?
N8 Cd2 2.333(5) 6_566 ?
N7 C10 1.281(8) . ?
N20 N21 1.314(7) . ?
N20 Cd4 2.395(5) 1_544 ?
N16 N16 1.302(10) 6_565 ?
N16 N15 1.308(7) . ?
N16 Cd2 2.331(5) 2_556 ?
N5 Cd4 2.362(7) 7_567 ?
N3 N1 1.335(12) . ?
N4 N2 1.353(13) . ?
N14 C17 1.277(9) 6_565 ?
N1 N2 1.249(12) . ?
N6 C7 1.242(12) 6_565 ?
O1 Cd2 2.218(3) 6_565 ?
O3 Cd4 2.296(7) 5_566 ?
C10 N7 1.281(8) 6_565 ?

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
C15 C13 C12 120.9(8) . . ?
C15 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C16 C14 C12 119.6(8) . . ?
C16 C14 H14 120.2 . . ?
C12 C14 H14 120.2 . . ?
N13 C16 C14 124.1(8) . . ?
N13 C16 H16 117.9 . . ?
C14 C16 H16 117.9 . . ?
N10 C11 N12 112.4(6) . . ?
N10 C11 C12 122.7(7) . . ?
N12 C11 C12 124.8(7) . . ?
C6 C4 C2 119.4(11) . . ?
C6 C4 H4 120.3 . . ?
C2 C4 H4 120.3 . . ?
N5 C5 C3 122.0(10) . . ?
N5 C5 H5 119.0 . . ?
C3 C5 H5 119.0 . . ?
C14 C12 C13 116.1(7) . . ?
C14 C12 C11 121.1(7) . . ?
C13 C12 C11 122.8(7) . . ?
C24 C23 C22 117.9(7) . . ?
C24 C23 C26 121.3(7) . . ?
C22 C23 C26 120.8(7) . . ?
N21 C26 N18 112.7(6) . . ?
N21 C26 C23 123.3(7) . . ?
N18 C26 C23 123.9(7) . . ?
N15 C20 N15 112.6(9) 6_565 . ?
N15 C20 C19 123.7(4) 6_565 . ?
N15 C20 C19 123.7(4) . . ?
N5 C6 C4 125.2(11) . . ?
N5 C6 H6 117.4 . . ?
C4 C6 H6 117.4 . . ?
C3 C2 C4 116.0(11) . . ?
C3 C2 C1 120.7(11) . . ?
C4 C2 C1 123.3(10) . . ?
C5 C3 C2 120.8(11) . . ?
C5 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
N14 C17 C18 124.6(9) . . ?
N14 C17 H17 117.7 . . ?
C18 C17 H17 117.7 . . ?
C19 C18 C17 121.5(9) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C23 C24 C25 118.9(8) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
C23 C22 C21 118.6(8) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C18 C19 C18 113.2(10) 6_565 . ?
C18 C19 C20 122.9(5) 6_565 . ?
C18 C19 C20 122.9(5) . . ?
N17 C25 C24 123.8(9) . . ?
N17 C25 H25 118.1 . . ?
C24 C25 H25 118.1 . . ?
C8 C9 C8 112.7(13) 6_565 . ?
C8 C9 C10 123.2(7) 6_565 . ?
C8 C9 C10 123.2(7) . . ?
C9 C8 C7 121.1(11) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
N6 C7 C8 124.8(11) . . ?
N6 C7 H7 117.6 . . ?
C8 C7 H7 117.6 . . ?
N17 C21 C22 123.9(8) . . ?
N17 C21 H21 118.1 . . ?
C22 C21 H21 118.1 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O3 C27 O4 125.9(9) . . ?
O3 C27 C28 119.6(9) . . ?
O4 C27 C28 114.5(10) . . ?
N13 C15 C13 122.9(7) . . ?
N13 C15 H15 118.6 . . ?
C13 C15 H15 118.6 . . ?
N4 C1 N3 111.6(10) . . ?
N4 C1 C2 122.5(11) . . ?
N3 C1 C2 125.9(11) . . ?
O1 Cd1 N6 167.5(3) . . ?
O1 Cd1 N1 81.2(3) . . ?
N6 Cd1 N1 86.3(3) . . ?
O1 Cd1 N9 85.36(13) . 6_565 ?
N6 Cd1 N9 95.62(13) . 6_565 ?
N1 Cd1 N9 94.26(14) . 6_565 ?
O1 Cd1 N9 85.36(14) . . ?
N6 Cd1 N9 95.62(13) . . ?
N1 Cd1 N9 94.26(14) . . ?
N9 Cd1 N9 166.3(3) 6_565 . ?
O1 Cd1 N14 104.4(2) . . ?
N6 Cd1 N14 88.1(3) . . ?
N1 Cd1 N14 174.4(3) . . ?
N9 Cd1 N14 86.28(14) 6_565 . ?
N9 Cd1 N14 86.28(14) . . ?
O3 Cd3 O3 180.0 5 . ?
O3 Cd3 N19 99.5(2) 5 5 ?
O3 Cd3 N19 80.5(2) . 5 ?
O3 Cd3 N19 80.5(2) 5 6 ?
O3 Cd3 N19 99.5(2) . 6 ?
N19 Cd3 N19 94.5(3) 5 6 ?
O3 Cd3 N19 99.5(2) 5 2 ?
O3 Cd3 N19 80.5(2) . 2 ?
N19 Cd3 N19 85.5(3) 5 2 ?
N19 Cd3 N19 180.0(3) 6 2 ?
O3 Cd3 N19 80.5(2) 5 . ?
O3 Cd3 N19 99.5(2) . . ?
N19 Cd3 N19 180.0 5 . ?
N19 Cd3 N19 85.5(3) 6 . ?
N19 Cd3 N19 94.5(3) 2 . ?
O1 Cd2 N17 175.4(2) . . ?
O1 Cd2 N11 88.10(18) . 6_565 ?
N17 Cd2 N11 95.0(2) . 6_565 ?
O1 Cd2 N16 81.77(19) . 2_556 ?
N17 Cd2 N16 94.5(2) . 2_556 ?
N11 Cd2 N16 95.9(2) 6_565 2_556 ?
O1 Cd2 N8 88.05(19) . 6_564 ?
N17 Cd2 N8 89.1(2) . 6_564 ?
N11 Cd2 N8 174.6(2) 6_565 6_564 ?
N16 Cd2 N8 87.3(2) 2_556 6_564 ?
O1 Cd2 O2 93.4(2) . . ?
N17 Cd2 O2 90.2(2) . . ?
N11 Cd2 O2 86.7(2) 6_565 . ?
N16 Cd2 O2 174.4(2) 2_556 . ?
N8 Cd2 O2 89.8(3) 6_564 . ?
O3 Cd4 N13 108.9(2) 5_566 6_575 ?
O3 Cd4 N13 108.9(2) 5_566 . ?
N13 Cd4 N13 100.3(3) 6_575 . ?
O3 Cd4 N5 157.1(3) 5_566 7_567 ?
N13 Cd4 N5 85.3(2) 6_575 7_567 ?
N13 Cd4 N5 85.3(2) . 7_567 ?
O3 Cd4 N20 77.6(2) 5_566 1_566 ?
N13 Cd4 N20 88.7(2) 6_575 1_566 ?
N13 Cd4 N20 166.2(2) . 1_566 ?
N5 Cd4 N20 85.0(2) 7_567 1_566 ?
O3 Cd4 N20 77.6(2) 5_566 6_566 ?
N13 Cd4 N20 166.2(2) 6_575 6_566 ?
N13 Cd4 N20 88.7(2) . 6_566 ?
N5 Cd4 N20 85.0(2) 7_567 6_566 ?
N20 Cd4 N20 80.7(3) 1_566 6_566 ?
N11 N9 N10 109.7(5) . . ?
N11 N9 Cd1 121.1(4) . . ?
N10 N9 Cd1 127.4(4) . . ?
N9 N10 C11 104.8(6) . . ?
N9 N11 N12 108.9(5) . . ?
N9 N11 Cd2 121.9(4) . 6_565 ?
N12 N11 Cd2 128.1(4) . 6_565 ?
C11 N12 N11 104.1(6) . . ?
C15 N13 C16 116.3(7) . . ?
C15 N13 Cd4 120.5(5) . . ?
C16 N13 Cd4 122.5(5) . . ?
N20 N19 N18 110.2(5) . . ?
N20 N19 Cd3 122.2(4) . . ?
N18 N19 Cd3 127.4(4) . . ?
C21 N17 C25 116.9(7) . . ?
C21 N17 Cd2 122.2(5) . . ?
C25 N17 Cd2 120.8(6) . . ?
N8 N8 N7 109.0(4) 6_565 . ?
N8 N8 Cd2 119.78(14) 6_565 6_566 ?
N7 N8 Cd2 130.1(5) . 6_566 ?
C10 N7 N8 105.5(6) . . ?
N19 N20 N21 109.1(5) . . ?
N19 N20 Cd4 123.9(4) . 1_544 ?
N21 N20 Cd4 126.9(4) . 1_544 ?
C26 N18 N19 103.5(6) . . ?
C26 N21 N20 104.5(6) . . ?
N16 N16 N15 108.9(3) 6_565 . ?
N16 N16 Cd2 119.28(13) 6_565 2_556 ?
N15 N16 Cd2 131.8(4) . 2_556 ?
C20 N15 N16 104.8(6) . . ?
C6 N5 C5 116.6(9) . . ?
C6 N5 Cd4 124.8(7) . 7_567 ?
C5 N5 Cd4 118.6(7) . 7_567 ?
C1 N3 N1 104.9(8) . . ?
C1 N4 N2 103.6(10) . . ?
C17 N14 C17 113.2(10) . 6_565 ?
C17 N14 Cd1 123.4(5) . . ?
C17 N14 Cd1 123.4(5) 6_565 . ?
N2 N1 N3 109.7(8) . . ?
N2 N1 Cd1 116.2(7) . . ?
N3 N1 Cd1 134.1(7) . . ?
C7 N6 C7 113.1(13) 6_565 . ?
C7 N6 Cd1 123.2(6) 6_565 . ?
C7 N6 Cd1 123.2(6) . . ?
N1 N2 N4 110.3(10) . . ?
Cd2 O1 Cd2 107.7(2) 6_565 . ?
Cd2 O1 Cd1 116.41(16) 6_565 . ?
Cd2 O1 Cd1 116.42(16) . . ?
C27 O3 Cd3 139.4(7) . . ?
C27 O3 Cd4 104.8(6) . 5_566 ?
Cd3 O3 Cd4 115.8(3) . 5_566 ?
N7 C10 N7 111.0(8) 6_565 . ?
N7 C10 C9 124.5(4) 6_565 . ?
N7 C10 C9 124.5(4) . . ?

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
C12 C14 C16 N13 3.1(17) . . . . ?
C16 C14 C12 C13 -3.3(14) . . . . ?
C16 C14 C12 C11 177.0(9) . . . . ?
C15 C13 C12 C14 2.0(14) . . . . ?
C15 C13 C12 C11 -178.4(8) . . . . ?
N10 C11 C12 C14 -169.1(8) . . . . ?
N12 C11 C12 C14 9.4(13) . . . . ?
N10 C11 C12 C13 11.3(12) . . . . ?
N12 C11 C12 C13 -170.2(8) . . . . ?
C24 C23 C26 N21 -5.8(13) . . . . ?
C22 C23 C26 N21 172.0(9) . . . . ?
C24 C23 C26 N18 173.8(9) . . . . ?
C22 C23 C26 N18 -8.3(13) . . . . ?
C2 C4 C6 N5 0.000(4) . . . . ?
C6 C4 C2 C3 0.000(4) . . . . ?
C6 C4 C2 C1 180.000(4) . . . . ?
N5 C5 C3 C2 0.000(4) . . . . ?
C4 C2 C3 C5 0.000(4) . . . . ?
C1 C2 C3 C5 180.000(3) . . . . ?
N14 C17 C18 C19 -8.2(18) . . . . ?
C22 C23 C24 C25 3.1(15) . . . . ?
C26 C23 C24 C25 -179.0(9) . . . . ?
C24 C23 C22 C21 -1.5(15) . . . . ?
C26 C23 C22 C21 -179.5(9) . . . . ?
C17 C18 C19 C18 13.4(19) . . . 6_565 ?
C17 C18 C19 C20 -177.8(9) . . . . ?
N15 C20 C19 C18 -6.2(16) 6_565 . . 6_565 ?
N15 C20 C19 C18 173.9(10) . . . 6_565 ?
N15 C20 C19 C18 -173.9(10) 6_565 . . . ?
N15 C20 C19 C18 6.2(16) . . . . ?
C23 C24 C25 N17 -2.8(17) . . . . ?
C8 C9 C8 C7 -16(2) 6_565 . . . ?
C10 C9 C8 C7 173.9(12) . . . . ?
C9 C8 C7 N6 6(2) . . . . ?
C23 C22 C21 N17 -0.6(17) . . . . ?
C12 C13 C15 N13 -0.1(14) . . . . ?
C3 C2 C1 N4 0.000(3) . . . . ?
C4 C2 C1 N4 180.000(3) . . . . ?
C3 C2 C1 N3 180.000(3) . . . . ?
C4 C2 C1 N3 0.000(4) . . . . ?
N11 N9 N10 C11 0.3(8) . . . . ?
Cd1 N9 N10 C11 -164.2(5) . . . . ?
N12 C11 N10 N9 -0.8(9) . . . . ?
C12 C11 N10 N9 177.9(7) . . . . ?
N10 N9 N11 N12 0.4(8) . . . . ?
Cd1 N9 N11 N12 166.0(5) . . . . ?
N10 N9 N11 Cd2 169.5(4) . . . 6_565 ?
Cd1 N9 N11 Cd2 -24.9(7) . . . 6_565 ?
N10 C11 N12 N11 1.1(9) . . . . ?
C12 C11 N12 N11 -177.6(7) . . . . ?
N9 N11 N12 C11 -0.9(8) . . . . ?
Cd2 N11 N12 C11 -169.1(5) 6_565 . . . ?
C13 C15 N13 C16 -0.4(13) . . . . ?
C13 C15 N13 Cd4 169.8(7) . . . . ?
C14 C16 N13 C15 -1.1(15) . . . . ?
C14 C16 N13 Cd4 -171.1(8) . . . . ?
C22 C21 N17 C25 1.0(15) . . . . ?
C22 C21 N17 Cd2 178.2(8) . . . . ?
C24 C25 N17 C21 0.7(15) . . . . ?
C24 C25 N17 Cd2 -176.6(8) . . . . ?
N8 N8 N7 C10 1.6(8) 6_565 . . . ?
Cd2 N8 N7 C10 -165.9(6) 6_566 . . . ?
N18 N19 N20 N21 -0.1(9) . . . . ?
Cd3 N19 N20 N21 -174.5(5) . . . . ?
N18 N19 N20 Cd4 177.0(5) . . . 1_544 ?
Cd3 N19 N20 Cd4 2.6(8) . . . 1_544 ?
N21 C26 N18 N19 0.2(9) . . . . ?
C23 C26 N18 N19 -179.5(7) . . . . ?
N20 N19 N18 C26 -0.1(8) . . . . ?
Cd3 N19 N18 C26 173.9(5) . . . . ?
N18 C26 N21 N20 -0.3(9) . . . . ?
C23 C26 N21 N20 179.4(7) . . . . ?
N19 N20 N21 C26 0.2(8) . . . . ?
Cd4 N20 N21 C26 -176.7(5) 1_544 . . . ?
N15 C20 N15 N16 0.3(11) 6_565 . . . ?
C19 C20 N15 N16 -179.7(8) . . . . ?
N16 N16 N15 C20 -0.2(7) 6_565 . . . ?
Cd2 N16 N15 C20 176.7(6) 2_556 . . . ?
C4 C6 N5 C5 0.000(4) . . . . ?
C4 C6 N5 Cd4 180.000(3) . . . 7_567 ?
C3 C5 N5 C6 0.000(4) . . . . ?
C3 C5 N5 Cd4 180.000(2) . . . 7_567 ?
N4 C1 N3 N1 0.000(2) . . . . ?
C2 C1 N3 N1 180.000(3) . . . . ?
N3 C1 N4 N2 0.000(2) . . . . ?
C2 C1 N4 N2 180.000(3) . . . . ?
C18 C17 N14 C17 1.6(19) . . . 6_565 ?
C18 C17 N14 Cd1 -178.1(8) . . . . ?
C1 N3 N1 N2 0.000(2) . . . . ?
C1 N3 N1 Cd1 180.000(2) . . . . ?
C8 C7 N6 C7 5(3) . . . 6_565 ?
C8 C7 N6 Cd1 177.2(10) . . . . ?
N3 N1 N2 N4 0.000(3) . . . . ?
Cd1 N1 N2 N4 180.000(2) . . . . ?
C1 N4 N2 N1 0.000(3) . . . . ?
O4 C27 O3 Cd3 180.000(1) . . . . ?
C28 C27 O3 Cd3 0.000(1) . . . . ?
O4 C27 O3 Cd4 0.000(0) . . . 5_566 ?
C28 C27 O3 Cd4 180.000(0) . . . 5_566 ?
N8 N7 C10 N7 -2.6(13) . . . 6_565 ?
N8 N7 C10 C9 178.5(9) . . . . ?
C8 C9 C10 N7 -173.8(12) 6_565 . . 6_565 ?
C8 C9 C10 N7 -4.9(19) . . . 6_565 ?
C8 C9 C10 N7 4.9(19) 6_565 . . . ?
C8 C9 C10 N7 173.8(12) . . . . ?

_refine_diff_density_max         1.896
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.130


# 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 -0.023 0.159 -0.107 5569 1141 ' '
_platon_squeeze_details          
;
The total potential solvent accessible void is 5569 eA3, indicating more
solvent molecules can reside in the crystal structure. Based on the TG
and elemental analysis, two DMF molecules and one dimethylamine cation 
were included in the final molecules.
;
#===END
