# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1528035'
_audit_update_record             
;
2017-06-02 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        1
_chemical_name_common            tppe-Cd
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H60 Cd Cl2 N4 O14'
_chemical_formula_sum            'C46 H60 Cd Cl2 N4 O14'
_chemical_formula_weight         1076.28

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'
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           23
_space_group_name_H-M_alt        'I 2 2 2'
_space_group_name_Hall           'I 2 2'

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

_cell_length_a                   12.0617(12)
_cell_length_b                   14.2056(11)
_cell_length_c                   17.7773(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3046.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3281
_cell_measurement_theta_min      3.1813
_cell_measurement_theta_max      29.1525

_exptl_crystal_description       sheet
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_F_000             1116
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.501
_shelx_estimated_absorpt_T_min   0.864
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68310
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.2375
_diffrn_reflns_number            6941
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.188
_diffrn_reflns_theta_max         29.217
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3573
_reflns_number_gt                3284
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_max     0.882
_reflns_Friedel_fraction_full    1.000

_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       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
'Refined as a 2-component inversion twin., Twin,SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0364P)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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.22(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3573
_refine_ls_number_parameters     123
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.0845
_refine_ls_wR_factor_gt          0.0807
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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 1.0000 1.0000 1.0000 0.03105(15) Uani 1 4 d S T P . .
C1 C 0.9196(6) 0.8290(4) 0.8841(3) 0.077(2) Uani 1 1 d . . . . .
H1 H 0.8606 0.8269 0.9177 0.093 Uiso 1 1 calc R U . . .
C2 C 0.9138(6) 0.7737(4) 0.8213(3) 0.088(2) Uani 1 1 d . . . . .
H2 H 0.8514 0.7368 0.8130 0.105 Uiso 1 1 calc R U . . .
C3 C 0.9986(10) 0.7722(2) 0.77088(17) 0.0437(7) Uani 1 1 d . . . . .
C4 C 1.0838(5) 0.8332(5) 0.7862(3) 0.0793(19) Uani 1 1 d . . . . .
H4 H 1.1416 0.8400 0.7520 0.095 Uiso 1 1 calc R U . . .
C5 C 1.0842(5) 0.8844(4) 0.8519(3) 0.079(2) Uani 1 1 d . . . . .
H5 H 1.1464 0.9207 0.8624 0.095 Uiso 1 1 calc R U . . .
C6 C 0.9974(9) 0.7137(2) 0.70173(16) 0.0388(7) Uani 1 1 d . . . . .
C7 C 0.9202(4) 0.6440(3) 0.6909(2) 0.0445(10) Uani 1 1 d . . . . .
H7 H 0.8675 0.6326 0.7279 0.053 Uiso 1 1 calc R U . . .
C8 C 0.9193(3) 0.5902(3) 0.6259(2) 0.0394(9) Uani 1 1 d . . . . .
H8 H 0.8648 0.5446 0.6193 0.047 Uiso 1 1 calc R U . . .
C9 C 0.9991(8) 0.60383(17) 0.57056(13) 0.0294(6) Uani 1 1 d . . . . .
C10 C 1.0752(4) 0.6745(3) 0.5803(2) 0.0458(10) Uani 1 1 d . . . . .
H10 H 1.1274 0.6861 0.5430 0.055 Uiso 1 1 calc R U . . .
C11 C 1.0752(4) 0.7287(3) 0.6450(2) 0.0521(11) Uani 1 1 d . . . . .
H11 H 1.1280 0.7759 0.6507 0.063 Uiso 1 1 calc R U . . .
C12 C 1.0000 0.5474(2) 0.5000 0.0281(8) Uani 1 2 d S T P . .
N1 N 1.0034(8) 0.88515(19) 0.90018(15) 0.0482(7) Uani 1 1 d . . . . .
Cl1 Cl 0.79071(9) 1.0000 1.0000 0.0456(3) Uani 1 2 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 N1 2.411(3) . ?
Cd1 N1 2.411(3) 3_577 ?
Cd1 N1 2.411(3) 4_757 ?
Cd1 N1 2.411(3) 2_775 ?
Cd1 Cl1 2.5244(11) 2_775 ?
Cd1 Cl1 2.5244(11) . ?
C1 N1 1.319(9) . ?
C1 C2 1.366(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.360(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(10) . ?
C3 C6 1.484(4) . ?
C4 C5 1.375(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.299(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.374(8) . ?
C6 C11 1.394(9) . ?
C7 C8 1.384(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.391(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.371(8) . ?
C9 C12 1.489(3) . ?
C10 C11 1.384(5) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C12 1.347(7) 2_765 ?
C12 C9 1.489(3) 4_756 ?

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 178.0(4) . 3_577 ?
N1 Cd1 N1 94.83(14) . 4_757 ?
N1 Cd1 N1 85.21(14) 3_577 4_757 ?
N1 Cd1 N1 85.21(14) . 2_775 ?
N1 Cd1 N1 94.83(14) 3_577 2_775 ?
N1 Cd1 N1 178.0(4) 4_757 2_775 ?
N1 Cd1 Cl1 89.0(2) . 2_775 ?
N1 Cd1 Cl1 89.0(2) 3_577 2_775 ?
N1 Cd1 Cl1 91.0(2) 4_757 2_775 ?
N1 Cd1 Cl1 91.0(2) 2_775 2_775 ?
N1 Cd1 Cl1 91.0(2) . . ?
N1 Cd1 Cl1 91.0(2) 3_577 . ?
N1 Cd1 Cl1 89.0(2) 4_757 . ?
N1 Cd1 Cl1 89.0(2) 2_775 . ?
Cl1 Cd1 Cl1 180.0 2_775 . ?
N1 C1 C2 124.3(5) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
C3 C2 C1 120.6(6) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 115.0(3) . . ?
C2 C3 C6 123.2(7) . . ?
C4 C3 C6 121.7(7) . . ?
C3 C4 C5 120.4(5) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
N1 C5 C4 124.2(5) . . ?
N1 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
C7 C6 C11 117.7(3) . . ?
C7 C6 C3 121.8(6) . . ?
C11 C6 C3 120.5(6) . . ?
C6 C7 C8 121.4(4) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C7 C8 C9 120.5(4) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C10 C9 C8 118.4(3) . . ?
C10 C9 C12 119.7(5) . . ?
C8 C9 C12 121.8(5) . . ?
C9 C10 C11 120.9(4) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C6 121.0(4) . . ?
C10 C11 H11 119.5 . . ?
C6 C11 H11 119.5 . . ?
C12 C12 C9 122.58(14) 2_765 . ?
C12 C12 C9 122.59(14) 2_765 4_756 ?
C9 C12 C9 114.8(3) . 4_756 ?
C5 N1 C1 115.3(3) . . ?
C5 N1 Cd1 120.3(4) . . ?
C1 N1 Cd1 123.8(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 1.4(13) . . . . ?
C1 C2 C3 C4 -3.6(12) . . . . ?
C1 C2 C3 C6 179.9(6) . . . . ?
C2 C3 C4 C5 5.5(11) . . . . ?
C6 C3 C4 C5 -178.0(6) . . . . ?
C3 C4 C5 N1 -5.6(12) . . . . ?
C2 C3 C6 C7 -12.4(9) . . . . ?
C4 C3 C6 C7 171.3(7) . . . . ?
C2 C3 C6 C11 167.1(7) . . . . ?
C4 C3 C6 C11 -9.2(9) . . . . ?
C11 C6 C7 C8 0.0(9) . . . . ?
C3 C6 C7 C8 179.5(5) . . . . ?
C6 C7 C8 C9 1.8(7) . . . . ?
C7 C8 C9 C10 -3.0(8) . . . . ?
C7 C8 C9 C12 -179.8(4) . . . . ?
C8 C9 C10 C11 2.4(8) . . . . ?
C12 C9 C10 C11 179.2(4) . . . . ?
C9 C10 C11 C6 -0.6(8) . . . . ?
C7 C6 C11 C10 -0.6(9) . . . . ?
C3 C6 C11 C10 179.8(5) . . . . ?
C10 C9 C12 C12 129.5(3) . . . 2_765 ?
C8 C9 C12 C12 -53.8(7) . . . 2_765 ?
C10 C9 C12 C9 -50.5(3) . . . 4_756 ?
C8 C9 C12 C9 126.2(7) . . . 4_756 ?
C4 C5 N1 C1 3.0(12) . . . . ?
C4 C5 N1 Cd1 -168.1(6) . . . . ?
C2 C1 N1 C5 -0.9(12) . . . . ?
C2 C1 N1 Cd1 169.9(6) . . . . ?

_refine_diff_density_max         0.806
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.052
# SQUEEZE RESULTS (Version = 120716)
# 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 -0.013 0.000 0.500 754 120 '12 H2O'
2 -0.010 0.500 0.000 754 120 '12 H2O'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains 24 H2O molecules which have been treated as a diffuse
contribution to the overall scattering and removed by SQUEEZE/PLATON.
The amount of these disordered solvent was determined by TGA, elemental analysis and SQUEEZE results.
A. L. Spek, J. Appl. Crystallogr., 2003, 36, 7-13.
A. L. Spek, Acta Crystallogr., 2009, D65, 148-155.
;


_exptl_crystal_recrystallization_method solvothermal
_chemical_properties_physical    ', Pressure-sensitive'
_exptl_crystal_preparation       ', Luminescent'
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1528036'
_audit_update_record             
;
2017-06-02 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        2
_chemical_name_common            tppe-Cd
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H52 Cd Cl2 N4 O10'
_chemical_formula_sum            'C46 H52 Cd Cl2 N4 O10'
_chemical_formula_weight         1004.21

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'
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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

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

_cell_length_a                   19.1291(10)
_cell_length_b                   12.4363(6)
_cell_length_c                   22.7970(15)
_cell_angle_alpha                90
_cell_angle_beta                 98.859(6)
_cell_angle_gamma                90
_cell_volume                     5358.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3063
_cell_measurement_theta_min      3.5770
_cell_measurement_theta_max      22.7960

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_F_000             2072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.560
_shelx_estimated_absorpt_T_min   0.850
_shelx_estimated_absorpt_T_max   0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.2375
_diffrn_reflns_number            23546
_diffrn_reflns_av_unetI/netI     0.2051
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.778
_diffrn_reflns_theta_max         29.169
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             12310
_reflns_number_gt                4237
_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       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0000P)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         12310
_refine_ls_number_parameters     503
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.2077
_refine_ls_R_factor_gt           0.0766
_refine_ls_wR_factor_ref         0.1242
_refine_ls_wR_factor_gt          0.1054
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.978
_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
Cd1 Cd 0.50756(3) 0.24676(4) -0.35089(2) 0.05144(14) Uani 1 1 d . . . . .
C1 C 0.4676(5) 0.1872(7) -0.2203(4) 0.119(4) Uani 1 1 d . . . . .
H1 H 0.4374 0.1417 -0.2448 0.143 Uiso 1 1 calc R U . . .
C2 C 0.4645(5) 0.1846(6) -0.1601(3) 0.119(4) Uani 1 1 d . . . . .
H2 H 0.4353 0.1353 -0.1452 0.143 Uiso 1 1 calc R U . . .
C3 C 0.5034(3) 0.2526(6) -0.1235(3) 0.0595(17) Uani 1 1 d . . . . .
C4 C 0.5456(4) 0.3220(6) -0.1488(3) 0.095(3) Uani 1 1 d . . . . .
H4 H 0.5736 0.3720 -0.1257 0.114 Uiso 1 1 calc R U . . .
C5 C 0.5459(4) 0.3166(6) -0.2081(3) 0.092(3) Uani 1 1 d . . . . .
H5 H 0.5746 0.3656 -0.2240 0.110 Uiso 1 1 calc R U . . .
C6 C 0.4990(2) 0.2534(4) -0.05819(16) 0.0582(17) Uani 1 1 d DG . . . .
C7 C 0.5156(4) 0.1600(4) -0.0255(2) 0.114(7) Uani 0.451(9) 1 d DG U P A 1
H7 H 0.5300 0.0989 -0.0440 0.137 Uiso 0.451(9) 1 calc R U P A 1
C8 C 0.5106(4) 0.1578(4) 0.0346(2) 0.139(9) Uani 0.451(9) 1 d DG U P A 1
H8 H 0.5218 0.0953 0.0565 0.167 Uiso 0.451(9) 1 calc R U P A 1
C9 C 0.4891(2) 0.2491(4) 0.06217(15) 0.0535(16) Uani 1 1 d DG . . A .
C10 C 0.4725(4) 0.3425(4) 0.0295(2) 0.099(7) Uani 0.451(9) 1 d DG U P A 1
H10 H 0.4581 0.4036 0.0480 0.119 Uiso 0.451(9) 1 calc R U P A 1
C11 C 0.4775(4) 0.3447(4) -0.0307(2) 0.110(7) Uani 0.451(9) 1 d DG U P A 1
H11 H 0.4664 0.4072 -0.0525 0.132 Uiso 0.451(9) 1 calc R U P A 1
C7' C 0.4755(4) 0.1622(6) -0.0319(3) 0.052(4) Uani 0.549(9) 1 d D U P A 2
H7' H 0.4626 0.1021 -0.0553 0.063 Uiso 0.549(9) 1 calc R U P A 2
C8' C 0.4705(4) 0.1576(5) 0.0283(3) 0.051(4) Uani 0.549(9) 1 d D U P A 2
H8' H 0.4553 0.0956 0.0453 0.061 Uiso 0.549(9) 1 calc R U P A 2
C10' C 0.5126(4) 0.3414(5) 0.0369(3) 0.042(3) Uani 0.549(9) 1 d D U P A 2
H10' H 0.5250 0.4018 0.0603 0.051 Uiso 0.549(9) 1 calc R U P A 2
C11' C 0.5175(4) 0.3437(5) -0.0233(3) 0.047(3) Uani 0.549(9) 1 d D U P A 2
H11' H 0.5332 0.4055 -0.0402 0.056 Uiso 0.549(9) 1 calc R U P A 2
C12 C 0.8381(4) 0.6886(6) 0.1331(4) 0.092(3) Uani 1 1 d . . . . .
H12 H 0.8342 0.7614 0.1239 0.110 Uiso 1 1 calc R U . . .
C13 C 0.7765(4) 0.6304(6) 0.1359(4) 0.104(3) Uani 1 1 d . . . . .
H13 H 0.7329 0.6647 0.1286 0.124 Uiso 1 1 calc R U . . .
C14 C 0.7798(3) 0.5242(5) 0.1492(3) 0.0495(17) Uani 1 1 d . . . . .
C15 C 0.8458(3) 0.4778(5) 0.1595(3) 0.071(2) Uani 1 1 d . . . . .
H15 H 0.8506 0.4052 0.1691 0.085 Uiso 1 1 calc R U . . .
C16 C 0.9051(4) 0.5398(6) 0.1555(3) 0.074(2) Uani 1 1 d . . . . .
H16 H 0.9491 0.5064 0.1619 0.089 Uiso 1 1 calc R U . . .
C17 C 0.7145(3) 0.4611(5) 0.1547(3) 0.0542(18) Uani 1 1 d . . . . .
C18 C 0.6589(4) 0.5063(5) 0.1755(4) 0.077(2) Uani 1 1 d . . . . .
H18 H 0.6613 0.5779 0.1875 0.093 Uiso 1 1 calc R U . . .
C19 C 0.5995(3) 0.4484(5) 0.1791(3) 0.080(2) Uani 1 1 d . . . . .
H19 H 0.5620 0.4824 0.1931 0.096 Uiso 1 1 calc R U . . .
C20 C 0.5923(3) 0.3419(5) 0.1631(3) 0.0512(17) Uani 1 1 d . . . . .
C21 C 0.6468(4) 0.2946(5) 0.1431(3) 0.083(2) Uani 1 1 d . . . . .
H21 H 0.6441 0.2225 0.1321 0.100 Uiso 1 1 calc R U . . .
C22 C 0.7094(3) 0.3552(6) 0.1389(3) 0.087(3) Uani 1 1 d . . . . .
H22 H 0.7473 0.3219 0.1252 0.104 Uiso 1 1 calc R U . . .
C23 C 0.4825(4) 0.3342(6) 0.5106(3) 0.084(3) Uani 1 1 d . . . . .
H23 H 0.4705 0.3962 0.5296 0.101 Uiso 1 1 calc R U . . .
C24 C 0.4806(4) 0.3387(5) 0.4496(3) 0.070(2) Uani 1 1 d . . . . .
H24 H 0.4656 0.4010 0.4288 0.084 Uiso 1 1 calc R U . . .
C25 C 0.5008(3) 0.2510(5) 0.4203(2) 0.0493(15) Uani 1 1 d . . . . .
C26 C 0.5184(4) 0.1589(5) 0.4529(3) 0.072(2) Uani 1 1 d . . . . .
H26 H 0.5306 0.0961 0.4347 0.086 Uiso 1 1 calc R U . . .
C27 C 0.5176(4) 0.1627(5) 0.5142(3) 0.073(2) Uani 1 1 d . . . . .
H27 H 0.5302 0.1003 0.5357 0.088 Uiso 1 1 calc R U . . .
C28 C 0.5052(3) 0.2540(5) 0.3566(2) 0.0484(15) Uani 1 1 d . . . . .
C29 C 0.4556(3) 0.3138(5) 0.3184(3) 0.0594(19) Uani 1 1 d . . . . .
H29 H 0.4192 0.3490 0.3332 0.071 Uiso 1 1 calc R U . . .
C30 C 0.4607(4) 0.3210(5) 0.2576(3) 0.0616(19) Uani 1 1 d . . . . .
H30 H 0.4273 0.3597 0.2321 0.074 Uiso 1 1 calc R U . . .
C31 C 0.5167(3) 0.2693(5) 0.2357(3) 0.0466(16) Uani 1 1 d . . . . .
C32 C 0.5654(4) 0.2130(5) 0.2743(3) 0.066(2) Uani 1 1 d . . . . .
H32 H 0.6035 0.1807 0.2605 0.079 Uiso 1 1 calc R U . . .
C33 C 0.5585(4) 0.2035(5) 0.3338(3) 0.069(2) Uani 1 1 d . . . . .
H33 H 0.5908 0.1619 0.3587 0.083 Uiso 1 1 calc R U . . .
C34 C 0.1118(4) -0.0287(7) 0.1673(3) 0.083(3) Uani 1 1 d . . . . .
H34 H 0.0695 0.0042 0.1725 0.099 Uiso 1 1 calc R U . . .
C35 C 0.1716(4) 0.0371(6) 0.1664(3) 0.078(2) Uani 1 1 d . . . . .
H35 H 0.1681 0.1114 0.1699 0.093 Uiso 1 1 calc R U . . .
C36 C 0.2346(4) -0.0097(6) 0.1604(3) 0.072(2) Uani 1 1 d . . . . .
C37 C 0.2376(4) -0.1223(6) 0.1551(4) 0.092(3) Uani 1 1 d . . . . .
H37 H 0.2796 -0.1575 0.1516 0.110 Uiso 1 1 calc R U . . .
C38 C 0.1739(4) -0.1794(5) 0.1554(4) 0.089(3) Uani 1 1 d . . . . .
H38 H 0.1756 -0.2537 0.1513 0.107 Uiso 1 1 calc R U . . .
C39 C 0.2991(4) 0.0577(6) 0.1548(3) 0.070(2) Uani 1 1 d . . . . .
C40 C 0.2917(4) 0.1574(6) 0.1293(3) 0.089(3) Uani 1 1 d . . . . .
H40 H 0.2469 0.1869 0.1183 0.107 Uiso 1 1 calc R U . . .
C41 C 0.3505(4) 0.2135(6) 0.1201(3) 0.089(3) Uani 1 1 d . . . . .
H41 H 0.3450 0.2790 0.1002 0.107 Uiso 1 1 calc R U . . .
C42 C 0.4171(4) 0.1759(5) 0.1394(3) 0.0535(18) Uani 1 1 d . . . . .
C43 C 0.4253(3) 0.0762(6) 0.1665(3) 0.074(2) Uani 1 1 d . . . . .
H43 H 0.4700 0.0487 0.1801 0.089 Uiso 1 1 calc R U . . .
C44 C 0.3641(4) 0.0180(5) 0.1728(3) 0.074(2) Uani 1 1 d . . . . .
H44 H 0.3687 -0.0501 0.1898 0.089 Uiso 1 1 calc R U . . .
C45 C 0.4812(3) 0.2383(5) 0.1271(3) 0.0538(17) Uani 1 1 d . . . . .
C46 C 0.5262(3) 0.2808(5) 0.1711(3) 0.0561(18) Uani 1 1 d . . . . .
N1 N 0.5098(3) 0.2491(5) -0.2454(2) 0.0603(14) Uani 1 1 d . . . . .
N2 N 0.9026(3) 0.6447(4) 0.1430(2) 0.0605(16) Uani 1 1 d . . . . .
N3 N 0.5003(3) 0.2474(5) 0.54415(19) 0.0647(15) Uani 1 1 d . . . . .
N4 N 0.1122(3) -0.1362(5) 0.1610(2) 0.0631(17) Uani 1 1 d . . . . .
Cl1 Cl 0.58360(9) 0.41639(14) -0.34882(8) 0.0654(5) Uani 1 1 d . . . . .
Cl2 Cl 0.43130(9) 0.07654(13) -0.36124(8) 0.0699(5) 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 N3 2.376(4) 1_554 ?
Cd1 N1 2.399(5) . ?
Cd1 N2 2.406(5) 4_565 ?
Cd1 N4 2.409(5) 4_655 ?
Cd1 Cl1 2.5587(19) . ?
Cd1 Cl2 2.5611(18) . ?
C1 N1 1.309(8) . ?
C1 C2 1.384(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.332(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.369(8) . ?
C3 C6 1.504(6) . ?
C4 C5 1.356(8) . ?
C4 H4 0.9300 . ?
C5 N1 1.312(8) . ?
C5 H5 0.9300 . ?
C6 C11' 1.3898(10) . ?
C6 C7' 1.3899(10) . ?
C6 C7 1.3900 . ?
C6 C11 1.3900 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 C10' 1.3898(10) . ?
C9 C8' 1.3899(10) . ?
C9 C10 1.3900 . ?
C9 C45 1.517(6) . ?
C10 C11 1.3900 . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C7' C8' 1.3904(10) . ?
C7' H7' 0.9300 . ?
C8' H8' 0.9300 . ?
C10' C11' 1.3901(10) . ?
C10' H10' 0.9300 . ?
C11' H11' 0.9300 . ?
C12 N2 1.335(7) . ?
C12 C13 1.392(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.354(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(7) . ?
C14 C17 1.496(7) . ?
C15 C16 1.385(8) . ?
C15 H15 0.9300 . ?
C16 N2 1.336(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.352(8) . ?
C17 C22 1.365(8) . ?
C18 C19 1.358(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.376(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.337(8) . ?
C20 C46 1.509(8) . ?
C21 C22 1.430(8) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 N3 1.335(7) . ?
C23 C24 1.388(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.365(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(8) . ?
C25 C28 1.469(7) . ?
C26 C27 1.401(8) . ?
C26 H26 0.9300 . ?
C27 N3 1.325(7) . ?
C27 H27 0.9300 . ?
C28 C33 1.366(8) . ?
C28 C29 1.399(7) . ?
C29 C30 1.407(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.404(8) . ?
C30 H30 0.9300 . ?
C31 C32 1.372(7) . ?
C31 C46 1.519(7) . ?
C32 C33 1.387(7) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 N4 1.345(8) . ?
C34 C35 1.409(8) . ?
C34 H34 0.9300 . ?
C35 C36 1.365(9) . ?
C35 H35 0.9300 . ?
C36 C37 1.408(8) . ?
C36 C39 1.512(8) . ?
C37 C38 1.410(8) . ?
C37 H37 0.9300 . ?
C38 N4 1.320(8) . ?
C38 H38 0.9300 . ?
C39 C44 1.342(8) . ?
C39 C40 1.367(9) . ?
C40 C41 1.368(8) . ?
C40 H40 0.9300 . ?
C41 C42 1.364(8) . ?
C41 H41 0.9300 . ?
C42 C43 1.383(8) . ?
C42 C45 1.513(8) . ?
C43 C44 1.403(8) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 C46 1.327(7) . ?
N2 Cd1 2.406(5) 4_666 ?
N3 Cd1 2.376(4) 1_556 ?
N4 Cd1 2.409(5) 4_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cd1 N1 177.53(19) 1_554 . ?
N3 Cd1 N2 91.17(18) 1_554 4_565 ?
N1 Cd1 N2 86.43(19) . 4_565 ?
N3 Cd1 N4 91.93(18) 1_554 4_655 ?
N1 Cd1 N4 90.47(18) . 4_655 ?
N2 Cd1 N4 176.83(19) 4_565 4_655 ?
N3 Cd1 Cl1 87.74(15) 1_554 . ?
N1 Cd1 Cl1 92.81(17) . . ?
N2 Cd1 Cl1 90.33(15) 4_565 . ?
N4 Cd1 Cl1 90.46(17) 4_655 . ?
N3 Cd1 Cl2 88.04(15) 1_554 . ?
N1 Cd1 Cl2 91.41(17) . . ?
N2 Cd1 Cl2 89.98(16) 4_565 . ?
N4 Cd1 Cl2 89.45(16) 4_655 . ?
Cl1 Cd1 Cl2 175.78(6) . . ?
N1 C1 C2 124.7(7) . . ?
N1 C1 H1 117.7 . . ?
C2 C1 H1 117.7 . . ?
C3 C2 C1 120.2(8) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 116.4(6) . . ?
C2 C3 C6 120.9(7) . . ?
C4 C3 C6 122.6(6) . . ?
C5 C4 C3 118.9(7) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 126.5(7) . . ?
N1 C5 H5 116.8 . . ?
C4 C5 H5 116.8 . . ?
C11' C6 C7' 118.8(6) . . ?
C7 C6 C11 120.0 . . ?
C11' C6 C3 121.6(5) . . ?
C7' C6 C3 119.5(6) . . ?
C7 C6 C3 118.8(4) . . ?
C11 C6 C3 121.2(4) . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10' C9 C8' 121.1(5) . . ?
C8 C9 C10 120.0 . . ?
C10' C9 C45 124.4(5) . . ?
C8' C9 C45 114.5(5) . . ?
C8 C9 C45 116.7(4) . . ?
C10 C9 C45 123.2(4) . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C6 120.0 . . ?
C10 C11 H11 120.0 . . ?
C6 C11 H11 120.0 . . ?
C6 C7' C8' 122.4(7) . . ?
C6 C7' H7' 118.8 . . ?
C8' C7' H7' 118.8 . . ?
C9 C8' C7' 117.6(7) . . ?
C9 C8' H8' 121.2 . . ?
C7' C8' H8' 121.2 . . ?
C9 C10' C11' 120.1(7) . . ?
C9 C10' H10' 120.0 . . ?
C11' C10' H10' 120.0 . . ?
C6 C11' C10' 119.9(7) . . ?
C6 C11' H11' 120.0 . . ?
C10' C11' H11' 120.0 . . ?
N2 C12 C13 123.1(7) . . ?
N2 C12 H12 118.4 . . ?
C13 C12 H12 118.4 . . ?
C14 C13 C12 120.5(7) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 117.2(6) . . ?
C13 C14 C17 121.4(6) . . ?
C15 C14 C17 121.4(6) . . ?
C14 C15 C16 119.6(6) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
N2 C16 C15 123.7(6) . . ?
N2 C16 H16 118.2 . . ?
C15 C16 H16 118.2 . . ?
C18 C17 C22 117.7(6) . . ?
C18 C17 C14 121.6(6) . . ?
C22 C17 C14 120.8(6) . . ?
C17 C18 C19 120.8(6) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C20 123.0(7) . . ?
C18 C19 H19 118.5 . . ?
C20 C19 H19 118.5 . . ?
C21 C20 C19 117.6(6) . . ?
C21 C20 C46 122.1(6) . . ?
C19 C20 C46 120.3(6) . . ?
C20 C21 C22 119.7(7) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C17 C22 C21 121.2(6) . . ?
C17 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
N3 C23 C24 124.9(6) . . ?
N3 C23 H23 117.6 . . ?
C24 C23 H23 117.6 . . ?
C25 C24 C23 119.5(6) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 117.7(6) . . ?
C24 C25 C28 121.8(6) . . ?
C26 C25 C28 120.5(6) . . ?
C25 C26 C27 118.1(6) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 H26 121.0 . . ?
N3 C27 C26 125.6(6) . . ?
N3 C27 H27 117.2 . . ?
C26 C27 H27 117.2 . . ?
C33 C28 C29 118.8(6) . . ?
C33 C28 C25 121.7(6) . . ?
C29 C28 C25 119.5(6) . . ?
C28 C29 C30 120.2(6) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C31 C30 C29 119.5(6) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C32 C31 C30 119.1(6) . . ?
C32 C31 C46 119.9(6) . . ?
C30 C31 C46 120.9(6) . . ?
C31 C32 C33 120.8(6) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C28 C33 C32 121.5(6) . . ?
C28 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
N4 C34 C35 123.9(7) . . ?
N4 C34 H34 118.1 . . ?
C35 C34 H34 118.1 . . ?
C36 C35 C34 119.0(7) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C35 C36 C37 118.7(7) . . ?
C35 C36 C39 121.1(7) . . ?
C37 C36 C39 120.0(8) . . ?
C36 C37 C38 117.0(7) . . ?
C36 C37 H37 121.5 . . ?
C38 C37 H37 121.5 . . ?
N4 C38 C37 125.5(6) . . ?
N4 C38 H38 117.2 . . ?
C37 C38 H38 117.2 . . ?
C44 C39 C40 119.6(6) . . ?
C44 C39 C36 120.0(7) . . ?
C40 C39 C36 120.4(7) . . ?
C39 C40 C41 119.6(7) . . ?
C39 C40 H40 120.2 . . ?
C41 C40 H40 120.2 . . ?
C42 C41 C40 121.6(7) . . ?
C42 C41 H41 119.2 . . ?
C40 C41 H41 119.2 . . ?
C41 C42 C43 119.2(6) . . ?
C41 C42 C45 120.4(6) . . ?
C43 C42 C45 120.2(7) . . ?
C42 C43 C44 118.0(7) . . ?
C42 C43 H43 121.0 . . ?
C44 C43 H43 121.0 . . ?
C39 C44 C43 121.8(7) . . ?
C39 C44 H44 119.1 . . ?
C43 C44 H44 119.1 . . ?
C46 C45 C42 121.0(5) . . ?
C46 C45 C9 123.4(5) . . ?
C42 C45 C9 115.6(5) . . ?
C45 C46 C20 124.6(5) . . ?
C45 C46 C31 122.3(5) . . ?
C20 C46 C31 113.1(5) . . ?
C1 N1 C5 113.2(6) . . ?
C1 N1 Cd1 120.8(5) . . ?
C5 N1 Cd1 125.6(5) . . ?
C12 N2 C16 115.9(6) . . ?
C12 N2 Cd1 121.5(4) . 4_666 ?
C16 N2 Cd1 122.2(5) . 4_666 ?
C27 N3 C23 114.2(5) . . ?
C27 N3 Cd1 122.4(4) . 1_556 ?
C23 N3 Cd1 123.3(5) . 1_556 ?
C38 N4 C34 115.7(6) . . ?
C38 N4 Cd1 119.8(5) . 4_556 ?
C34 N4 Cd1 124.1(5) . 4_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 4.1(16) . . . . ?
C1 C2 C3 C4 -0.7(14) . . . . ?
C1 C2 C3 C6 178.0(8) . . . . ?
C2 C3 C4 C5 -0.7(13) . . . . ?
C6 C3 C4 C5 -179.4(7) . . . . ?
C3 C4 C5 N1 -1.0(14) . . . . ?
C2 C3 C6 C11' -156.7(7) . . . . ?
C4 C3 C6 C11' 22.0(9) . . . . ?
C2 C3 C6 C7' 22.8(9) . . . . ?
C4 C3 C6 C7' -158.5(7) . . . . ?
C2 C3 C6 C7 59.3(9) . . . . ?
C4 C3 C6 C7 -122.1(7) . . . . ?
C2 C3 C6 C11 -119.4(8) . . . . ?
C4 C3 C6 C11 59.3(8) . . . . ?
C11 C6 C7 C8 0.0 . . . . ?
C3 C6 C7 C8 -178.7(5) . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C7 C8 C9 C45 176.7(4) . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C45 C9 C10 C11 -176.5(5) . . . . ?
C9 C10 C11 C6 0.0 . . . . ?
C7 C6 C11 C10 0.0 . . . . ?
C3 C6 C11 C10 178.7(5) . . . . ?
C11' C6 C7' C8' -0.7(2) . . . . ?
C3 C6 C7' C8' 179.7(5) . . . . ?
C10' C9 C8' C7' -0.7(2) . . . . ?
C45 C9 C8' C7' 179.1(5) . . . . ?
C6 C7' C8' C9 1.0(3) . . . . ?
C8' C9 C10' C11' 0.3(2) . . . . ?
C45 C9 C10' C11' -179.5(5) . . . . ?
C7' C6 C11' C10' 0.2(2) . . . . ?
C3 C6 C11' C10' 179.8(5) . . . . ?
C9 C10' C11' C6 0.0(3) . . . . ?
N2 C12 C13 C14 0.1(14) . . . . ?
C12 C13 C14 C15 -0.1(12) . . . . ?
C12 C13 C14 C17 177.6(7) . . . . ?
C13 C14 C15 C16 -0.5(11) . . . . ?
C17 C14 C15 C16 -178.2(6) . . . . ?
C14 C15 C16 N2 1.2(12) . . . . ?
C13 C14 C17 C18 -33.0(11) . . . . ?
C15 C14 C17 C18 144.7(8) . . . . ?
C13 C14 C17 C22 147.2(8) . . . . ?
C15 C14 C17 C22 -35.2(10) . . . . ?
C22 C17 C18 C19 -1.5(12) . . . . ?
C14 C17 C18 C19 178.7(7) . . . . ?
C17 C18 C19 C20 0.9(13) . . . . ?
C18 C19 C20 C21 0.1(12) . . . . ?
C18 C19 C20 C46 176.9(7) . . . . ?
C19 C20 C21 C22 -0.4(11) . . . . ?
C46 C20 C21 C22 -177.2(7) . . . . ?
C18 C17 C22 C21 1.2(12) . . . . ?
C14 C17 C22 C21 -179.0(7) . . . . ?
C20 C21 C22 C17 -0.2(12) . . . . ?
N3 C23 C24 C25 -2.9(13) . . . . ?
C23 C24 C25 C26 3.7(11) . . . . ?
C23 C24 C25 C28 -175.0(7) . . . . ?
C24 C25 C26 C27 -2.8(10) . . . . ?
C28 C25 C26 C27 176.0(6) . . . . ?
C25 C26 C27 N3 0.8(12) . . . . ?
C24 C25 C28 C33 140.8(7) . . . . ?
C26 C25 C28 C33 -38.0(10) . . . . ?
C24 C25 C28 C29 -36.3(10) . . . . ?
C26 C25 C28 C29 145.0(7) . . . . ?
C33 C28 C29 C30 0.3(10) . . . . ?
C25 C28 C29 C30 177.5(6) . . . . ?
C28 C29 C30 C31 -1.2(10) . . . . ?
C29 C30 C31 C32 -0.2(9) . . . . ?
C29 C30 C31 C46 -176.4(5) . . . . ?
C30 C31 C32 C33 2.3(9) . . . . ?
C46 C31 C32 C33 178.6(6) . . . . ?
C29 C28 C33 C32 1.8(10) . . . . ?
C25 C28 C33 C32 -175.3(6) . . . . ?
C31 C32 C33 C28 -3.2(10) . . . . ?
N4 C34 C35 C36 -1.8(12) . . . . ?
C34 C35 C36 C37 0.1(12) . . . . ?
C34 C35 C36 C39 175.6(7) . . . . ?
C35 C36 C37 C38 1.1(12) . . . . ?
C39 C36 C37 C38 -174.4(7) . . . . ?
C36 C37 C38 N4 -1.0(14) . . . . ?
C35 C36 C39 C44 152.8(8) . . . . ?
C37 C36 C39 C44 -31.8(11) . . . . ?
C35 C36 C39 C40 -29.9(11) . . . . ?
C37 C36 C39 C40 145.6(8) . . . . ?
C44 C39 C40 C41 2.8(13) . . . . ?
C36 C39 C40 C41 -174.6(7) . . . . ?
C39 C40 C41 C42 -4.5(13) . . . . ?
C40 C41 C42 C43 3.0(12) . . . . ?
C40 C41 C42 C45 178.3(7) . . . . ?
C41 C42 C43 C44 0.2(11) . . . . ?
C45 C42 C43 C44 -175.2(6) . . . . ?
C40 C39 C44 C43 0.4(13) . . . . ?
C36 C39 C44 C43 177.7(6) . . . . ?
C42 C43 C44 C39 -1.8(12) . . . . ?
C41 C42 C45 C46 114.9(8) . . . . ?
C43 C42 C45 C46 -69.8(9) . . . . ?
C41 C42 C45 C9 -64.5(9) . . . . ?
C43 C42 C45 C9 110.8(7) . . . . ?
C10' C9 C45 C46 -38.2(9) . . . . ?
C8' C9 C45 C46 142.0(6) . . . . ?
C8 C9 C45 C46 106.8(7) . . . . ?
C10 C9 C45 C46 -76.6(8) . . . . ?
C10' C9 C45 C42 141.1(6) . . . . ?
C8' C9 C45 C42 -38.7(7) . . . . ?
C8 C9 C45 C42 -73.9(7) . . . . ?
C10 C9 C45 C42 102.8(6) . . . . ?
C42 C45 C46 C20 178.5(7) . . . . ?
C9 C45 C46 C20 -2.2(10) . . . . ?
C42 C45 C46 C31 0.3(10) . . . . ?
C9 C45 C46 C31 179.6(6) . . . . ?
C21 C20 C46 C45 -66.0(10) . . . . ?
C19 C20 C46 C45 117.2(8) . . . . ?
C21 C20 C46 C31 112.4(8) . . . . ?
C19 C20 C46 C31 -64.4(8) . . . . ?
C32 C31 C46 C45 115.3(7) . . . . ?
C30 C31 C46 C45 -68.5(8) . . . . ?
C32 C31 C46 C20 -63.2(8) . . . . ?
C30 C31 C46 C20 113.0(7) . . . . ?
C2 C1 N1 C5 -5.4(14) . . . . ?
C2 C1 N1 Cd1 -178.9(8) . . . . ?
C4 C5 N1 C1 3.9(13) . . . . ?
C4 C5 N1 Cd1 177.1(7) . . . . ?
C13 C12 N2 C16 0.5(12) . . . . ?
C13 C12 N2 Cd1 -172.5(6) . . . 4_666 ?
C15 C16 N2 C12 -1.1(11) . . . . ?
C15 C16 N2 Cd1 171.8(6) . . . 4_666 ?
C26 C27 N3 C23 0.2(12) . . . . ?
C26 C27 N3 Cd1 -176.2(6) . . . 1_556 ?
C24 C23 N3 C27 0.9(12) . . . . ?
C24 C23 N3 Cd1 177.2(6) . . . 1_556 ?
C37 C38 N4 C34 -0.6(13) . . . . ?
C37 C38 N4 Cd1 173.1(7) . . . 4_556 ?
C35 C34 N4 C38 2.0(11) . . . . ?
C35 C34 N4 Cd1 -171.3(6) . . . 4_556 ?

_refine_diff_density_max         0.546
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.079
# SQUEEZE RESULTS (Version = 120716)
# 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 0.250 -0.054 -0.086 983 261 '26 H2O'
2 0.750 -0.050 0.416 981 261 '26 H2O'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains 52 H2O molecules which have been treated as a diffuse
contribution to the overall scattering and removed by SQUEEZE/PLATON.
The amount of these disordered solvent was determined by TGA, elemental analysis and SQUEEZE results.
A. L. Spek, J. Appl. Crystallogr., 2003, 36, 7-13.
A. L. Spek, Acta Crystallogr., 2009, D65, 148-155.
;


_exptl_crystal_recrystallization_method solvothermal
_chemical_properties_physical    ', Pressure-sensitive'
_exptl_crystal_preparation       ', Luminescent'
