# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_cd66z
_database_code_depnum_ccdc_archive 'CCDC 1446466'
_audit_update_record             
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 Cd N4 O2 S2'
_chemical_formula_sum            'C14 H12 Cd N4 O2 S2'
_chemical_formula_weight         444.80

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

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

_cell_length_a                   8.5167(4)
_cell_length_b                   8.9163(4)
_cell_length_c                   22.2579(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1690.22(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    2592
_cell_measurement_theta_min      3.5520
_cell_measurement_theta_max      27.7180

_exptl_crystal_description       plate
_exptl_crystal_colour            white
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;CrysAlis RED, (2005)
;
_exptl_absorpt_correction_T_min  0.65422
_exptl_absorpt_correction_T_max  1.00000

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295.0
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5938
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         25.04
_reflns_number_total             2951
_reflns_number_gt                2755
_reflns_threshold_expression     >2sigma(I)

#========================================================================== 
#
# REFINEMENT DATA

_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0264P)²+0.1455P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_number_reflns         2951
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0612
_refine_ls_wR_factor_gt          0.0592
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9240(5) 0.4976(5) 0.46987(19) 0.0401(10) Uani 1 1 d . . .
H1 H 0.9892 0.4275 0.4515 0.048 Uiso 1 1 calc R . .
C2 C 0.8564(6) 0.6063(5) 0.4349(2) 0.0486(12) Uani 1 1 d . . .
H2 H 0.8737 0.6081 0.3937 0.058 Uiso 1 1 calc R . .
C3 C 0.7634(6) 0.7118(5) 0.4614(2) 0.0540(13) Uani 1 1 d . . .
H3 H 0.7193 0.7888 0.4388 0.065 Uiso 1 1 calc R . .
C4 C 0.7361(5) 0.7021(5) 0.5223(2) 0.0496(12) Uani 1 1 d . . .
H4 H 0.6713 0.7714 0.5412 0.060 Uiso 1 1 calc R . .
C5 C 0.8051(4) 0.5894(4) 0.55458(19) 0.0329(10) Uani 1 1 d . . .
C6 C 0.7837(5) 0.5718(5) 0.6225(2) 0.0350(10) Uani 1 1 d . . .
C7 C 0.9271(5) 0.6314(4) 0.65520(18) 0.0324(9) Uani 1 1 d . . .
C8 C 0.9280(6) 0.7678(5) 0.6840(2) 0.0464(11) Uani 1 1 d . . .
H8 H 0.8392 0.8284 0.6838 0.056 Uiso 1 1 calc R . .
C9 C 1.0629(6) 0.8133(5) 0.7132(2) 0.0551(12) Uani 1 1 d . . .
H9 H 1.0658 0.9055 0.7327 0.066 Uiso 1 1 calc R . .
C10 C 1.1920(6) 0.7225(5) 0.7135(2) 0.0516(13) Uani 1 1 d . . .
H10 H 1.2830 0.7501 0.7337 0.062 Uiso 1 1 calc R . .
C11 C 1.1830(5) 0.5905(5) 0.6832(2) 0.0451(12) Uani 1 1 d . . .
H11 H 1.2714 0.5293 0.6826 0.054 Uiso 1 1 calc R . .
C12 C 0.6375(5) 0.3401(6) 0.6169(2) 0.0599(14) Uani 1 1 d . . .
H12A H 0.5472 0.3780 0.6377 0.090 Uiso 1 1 calc R . .
H12B H 0.6474 0.2344 0.6243 0.090 Uiso 1 1 calc R . .
H12C H 0.6253 0.3570 0.5745 0.090 Uiso 1 1 calc R . .
C98 C 1.2994(5) 0.1535(5) 0.6892(2) 0.0432(11) Uani 1 1 d . . .
C99 C 1.3328(5) 0.3938(5) 0.4927(2) 0.0435(11) Uani 1 1 d . . .
N1 N 0.9007(4) 0.4876(4) 0.52909(16) 0.0346(8) Uani 1 1 d . . .
N2 N 1.0542(4) 0.5431(3) 0.65408(14) 0.0340(7) Uani 1 1 d . . .
N98 N 1.2012(6) 0.2142(5) 0.6654(2) 0.0647(12) Uani 1 1 d . . .
N99 N 1.2532(5) 0.3718(4) 0.5328(2) 0.0563(11) Uani 1 1 d . . .
O1 O 0.7768(3) 0.4165(3) 0.63801(13) 0.0386(7) Uani 1 1 d . . .
O2 O 0.6480(3) 0.6479(4) 0.63915(15) 0.0507(8) Uani 1 1 d . . .
H2A H 0.5715 0.6067 0.6241 0.076 Uiso 1 1 calc R . .
S98 S 1.44007(15) 0.06287(15) 0.72396(6) 0.0573(3) Uani 1 1 d . . .
S99 S 0.94588(19) 0.06603(13) 0.56482(7) 0.0670(4) Uani 1 1 d . . .
Cd1 Cd 1.04604(4) 0.32744(3) 0.595727(14) 0.03677(10) 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
C1 N1 1.336(5) . ?
C1 C2 1.370(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.378(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.345(5) . ?
C5 C6 1.531(6) . ?
C6 O2 1.390(5) . ?
C6 O1 1.428(5) . ?
C6 C7 1.518(6) . ?
C7 N2 1.339(5) . ?
C7 C8 1.374(6) . ?
C8 C9 1.381(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.365(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.359(6) . ?
C10 H10 0.9300 . ?
C11 N2 1.342(5) . ?
C11 H11 0.9300 . ?
C12 O1 1.447(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C98 N98 1.129(6) . ?
C98 S98 1.639(5) . ?
C99 N99 1.138(6) . ?
C99 S99 1.642(5) 4_556 ?
N1 Cd1 2.402(3) . ?
N2 Cd1 2.322(3) . ?
N98 Cd1 2.273(4) . ?
N99 Cd1 2.287(4) . ?
O1 Cd1 2.603(3) . ?
O2 H2A 0.8200 . ?
S99 C99 1.642(5) 4_456 ?
S99 Cd1 2.5756(12) . ?

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 C1 C2 123.0(4) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.2(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 118.6(4) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 119.4(5) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 122.3(4) . . ?
N1 C5 C6 114.8(4) . . ?
C4 C5 C6 122.9(4) . . ?
O2 C6 O1 112.0(3) . . ?
O2 C6 C7 111.8(3) . . ?
O1 C6 C7 104.9(3) . . ?
O2 C6 C5 108.2(3) . . ?
O1 C6 C5 110.0(3) . . ?
C7 C6 C5 110.0(3) . . ?
N2 C7 C8 121.7(4) . . ?
N2 C7 C6 115.8(3) . . ?
C8 C7 C6 122.5(4) . . ?
C7 C8 C9 119.0(4) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 119.8(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C9 117.8(4) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
N2 C11 C10 123.9(4) . . ?
N2 C11 H11 118.0 . . ?
C10 C11 H11 118.0 . . ?
O1 C12 H12A 109.5 . . ?
O1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N98 C98 S98 179.0(5) . . ?
N99 C99 S99 177.3(4) . 4_556 ?
C1 N1 C5 117.5(3) . . ?
C1 N1 Cd1 124.9(3) . . ?
C5 N1 Cd1 116.9(3) . . ?
C7 N2 C11 117.8(3) . . ?
C7 N2 Cd1 118.3(3) . . ?
C11 N2 Cd1 123.7(3) . . ?
C98 N98 Cd1 164.7(4) . . ?
C99 N99 Cd1 165.9(4) . . ?
C6 O1 C12 114.3(3) . . ?
C6 O1 Cd1 99.9(2) . . ?
C12 O1 Cd1 117.5(3) . . ?
C6 O2 H2A 109.5 . . ?
C99 S99 Cd1 101.84(16) 4_456 . ?
N98 Cd1 N99 92.64(16) . . ?
N98 Cd1 N2 88.22(13) . . ?
N99 Cd1 N2 100.15(13) . . ?
N98 Cd1 N1 169.88(14) . . ?
N99 Cd1 N1 85.21(13) . . ?
N2 Cd1 N1 82.44(11) . . ?
N98 Cd1 S99 88.44(12) . . ?
N99 Cd1 S99 104.39(11) . . ?
N2 Cd1 S99 155.35(9) . . ?
N1 Cd1 S99 101.67(9) . . ?
N98 Cd1 O1 113.65(14) . . ?
N99 Cd1 O1 148.02(12) . . ?
N2 Cd1 O1 64.62(10) . . ?
N1 Cd1 O1 65.67(10) . . ?
S99 Cd1 O1 94.64(7) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.072
####################################################################### 
# 
# 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_cd111d
_database_code_depnum_ccdc_archive 'CCDC 1446467'
_audit_update_record             
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H24 Cd2 N8 O4 S4'
_chemical_formula_sum            'C28 H24 Cd2 N8 O4 S4'
_chemical_formula_weight         889.59

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5984(6)
_cell_length_b                   9.9463(7)
_cell_length_c                   10.6576(6)
_cell_angle_alpha                100.460(5)
_cell_angle_beta                 108.911(5)
_cell_angle_gamma                92.653(5)
_cell_volume                     842.50(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    3246
_cell_measurement_theta_min      4.1810
_cell_measurement_theta_max      28.6920

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.76
_exptl_crystal_size_min          0.54
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             440
_exptl_absorpt_coefficient_mu    1.556
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;CrysAlis RED, (2005)
;
_exptl_absorpt_correction_T_min  0.83837
_exptl_absorpt_correction_T_max  1.00000

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295.0
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7106
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         25.04
_reflns_number_total             2968
_reflns_number_gt                2463
_reflns_threshold_expression     >2sigma(I)

#========================================================================== 
#
# REFINEMENT DATA

_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0569P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2968
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1010
_refine_ls_wR_factor_gt          0.0962
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1139(6) 0.5300(6) 0.1394(6) 0.0561(14) Uani 1 1 d . . .
H1 H -0.1043 0.4543 0.1803 0.067 Uiso 1 1 calc R . .
C2 C -0.2369(7) 0.5213(8) 0.0160(6) 0.0674(17) Uani 1 1 d . . .
H2 H -0.3116 0.4424 -0.0245 0.081 Uiso 1 1 calc R . .
C3 C -0.2460(7) 0.6318(8) -0.0455(6) 0.0680(19) Uani 1 1 d . . .
H3 H -0.3274 0.6283 -0.1289 0.082 Uiso 1 1 calc R . .
C4 C -0.1353(6) 0.7474(7) 0.0157(5) 0.0531(14) Uani 1 1 d . . .
H4 H -0.1389 0.8220 -0.0262 0.064 Uiso 1 1 calc R . .
C5 C -0.0177(5) 0.7505(5) 0.1413(4) 0.0373(11) Uani 1 1 d . . .
C6 C 0.1097(5) 0.8742(5) 0.2186(4) 0.0372(11) Uani 1 1 d . . .
C7 C 0.2798(5) 0.8384(5) 0.2187(4) 0.0359(10) Uani 1 1 d . . .
C8 C 0.3544(6) 0.8809(6) 0.1332(5) 0.0503(13) Uani 1 1 d . . .
H8 H 0.3026 0.9358 0.0736 0.060 Uiso 1 1 calc R . .
C9 C 0.5064(6) 0.8405(6) 0.1380(6) 0.0576(15) Uani 1 1 d . . .
H9 H 0.5578 0.8667 0.0803 0.069 Uiso 1 1 calc R . .
C10 C 0.5820(6) 0.7620(6) 0.2276(6) 0.0544(14) Uani 1 1 d . . .
H10 H 0.6864 0.7365 0.2337 0.065 Uiso 1 1 calc R . .
C11 C 0.5004(5) 0.7208(6) 0.3093(5) 0.0437(12) Uani 1 1 d . . .
H11 H 0.5509 0.6660 0.3694 0.052 Uiso 1 1 calc R . .
C12 C 0.2054(8) 1.0180(6) 0.4444(6) 0.0610(15) Uani 1 1 d . . .
H12A H 0.3199 1.0081 0.4578 0.091 Uiso 1 1 calc R . .
H12B H 0.1878 1.0301 0.5300 0.091 Uiso 1 1 calc R . .
H12C H 0.1759 1.0968 0.4052 0.091 Uiso 1 1 calc R . .
C98 C 0.2740(7) 0.8407(7) 0.7421(5) 0.0549(15) Uani 1 1 d . . .
C99 C 0.1248(6) 0.3728(5) 0.4599(5) 0.0358(10) Uani 1 1 d . . .
N1 N -0.0082(4) 0.6434(4) 0.2020(4) 0.0384(9) Uani 1 1 d . . .
N2 N 0.3511(4) 0.7576(4) 0.3046(4) 0.0351(9) Uani 1 1 d . . .
N98 N 0.1919(6) 0.8954(6) 0.7957(5) 0.0711(15) Uani 1 1 d . . .
N99 N 0.0360(5) 0.3375(5) 0.5109(5) 0.0524(11) Uani 1 1 d . . .
O2 O 0.0791(4) 0.9891(4) 0.1632(4) 0.0544(10) Uani 1 1 d . . .
H2A H -0.0101 1.0130 0.1657 0.082 Uiso 1 1 calc R . .
O4 O 0.1048(4) 0.8969(3) 0.3547(3) 0.0377(7) Uani 1 1 d . . .
S98 S 0.39940(19) 0.7652(2) 0.66791(15) 0.0752(5) Uani 1 1 d . . .
S99 S 0.25499(18) 0.41990(15) 0.38809(15) 0.0561(4) Uani 1 1 d . . .
Cd1 Cd 0.18975(4) 0.67735(4) 0.42468(3) 0.03720(15) 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
C1 N1 1.335(7) . ?
C1 C2 1.380(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.371(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.370(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.336(6) . ?
C5 C6 1.521(7) . ?
C6 O2 1.377(5) . ?
C6 O4 1.441(5) . ?
C6 C7 1.521(6) . ?
C7 N2 1.345(5) . ?
C7 C8 1.383(6) . ?
C8 C9 1.373(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.364(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.384(7) . ?
C10 H10 0.9300 . ?
C11 N2 1.339(6) . ?
C11 H11 0.9300 . ?
C12 O4 1.437(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C98 N98 1.142(7) . ?
C98 S98 1.663(6) . ?
C99 N99 1.148(6) . ?
C99 S99 1.641(5) . ?
N1 Cd1 2.383(3) . ?
N2 Cd1 2.370(4) . ?
N99 Cd1 2.265(4) 2_566 ?
O2 H2A 0.8200 . ?
O4 Cd1 2.498(3) . ?
S98 Cd1 2.5953(15) . ?
S99 Cd1 2.6336(14) . ?
Cd1 N99 2.265(4) 2_566 ?

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 C1 C2 122.2(6) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 118.3(6) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C4 C3 C2 120.1(5) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 118.5(6) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 121.7(5) . . ?
N1 C5 C6 115.5(3) . . ?
C4 C5 C6 122.8(5) . . ?
O2 C6 O4 112.0(4) . . ?
O2 C6 C5 113.3(4) . . ?
O4 C6 C5 104.7(3) . . ?
O2 C6 C7 107.6(4) . . ?
O4 C6 C7 110.0(3) . . ?
C5 C6 C7 109.2(4) . . ?
N2 C7 C8 121.9(4) . . ?
N2 C7 C6 115.2(4) . . ?
C8 C7 C6 122.8(4) . . ?
C9 C8 C7 118.7(5) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
C10 C9 C8 119.9(5) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 118.9(5) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
N2 C11 C10 122.1(4) . . ?
N2 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
O4 C12 H12A 109.5 . . ?
O4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N98 C98 S98 177.9(6) . . ?
N99 C99 S99 178.4(4) . . ?
C1 N1 C5 119.1(4) . . ?
C1 N1 Cd1 124.8(3) . . ?
C5 N1 Cd1 116.0(3) . . ?
C11 N2 C7 118.6(4) . . ?
C11 N2 Cd1 125.0(3) . . ?
C7 N2 Cd1 116.3(3) . . ?
C99 N99 Cd1 159.9(4) . 2_566 ?
C6 O2 H2A 109.5 . . ?
C12 O4 C6 114.7(4) . . ?
C12 O4 Cd1 114.0(3) . . ?
C6 O4 Cd1 102.2(2) . . ?
C98 S98 Cd1 99.45(18) . . ?
C99 S99 Cd1 92.58(17) . . ?
N99 Cd1 N2 154.69(15) 2_566 . ?
N99 Cd1 N1 84.19(15) 2_566 . ?
N2 Cd1 N1 78.58(12) . . ?
N99 Cd1 O4 88.22(13) 2_566 . ?
N2 Cd1 O4 68.00(11) . . ?
N1 Cd1 O4 66.67(12) . . ?
N99 Cd1 S98 95.54(13) 2_566 . ?
N2 Cd1 S98 97.78(9) . . ?
N1 Cd1 S98 168.73(11) . . ?
O4 Cd1 S98 102.06(8) . . ?
N99 Cd1 S99 102.25(12) 2_566 . ?
N2 Cd1 S99 96.92(10) . . ?
N1 Cd1 S99 92.45(11) . . ?
O4 Cd1 S99 155.80(8) . . ?
S98 Cd1 S99 98.60(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.121
####################################################################### 
# 
# 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_cd126
_database_code_depnum_ccdc_archive 'CCDC 1446468'
_audit_update_record             
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H44 Cd4 N20 O8'
_chemical_formula_sum            'C48 H44 Cd4 N20 O8'
_chemical_formula_weight         1478.63

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I41/acd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'y+3/4, x+1/4, -z+1/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'y+5/4, x+3/4, -z+3/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'x-1/2, -y, z'
'-y-3/4, -x-1/4, z-1/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-y-1/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   18.4180(5)
_cell_length_b                   18.4180(5)
_cell_length_c                   30.698(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10413.6(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    4764
_cell_measurement_theta_min      3.7310
_cell_measurement_theta_max      29.0740

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.6
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5824
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;CrysAlis RED, (2005)
;
_exptl_absorpt_correction_T_min  0.65568
_exptl_absorpt_correction_T_max  1.00000

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295.0
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12961
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         25.04
_reflns_number_total             2298
_reflns_number_gt                1616
_reflns_threshold_expression     >2sigma(I)

#========================================================================== 
#
# REFINEMENT DATA

_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0415P)²+55.7509P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2298
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0953
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5478(3) 0.3306(3) -0.0201(2) 0.0350(14) Uani 1 1 d . . .
H1 H 0.5154 0.3693 -0.0208 0.042 Uiso 1 1 calc R . .
C2 C 0.5735(3) 0.3042(4) -0.0590(2) 0.0406(16) Uani 1 1 d . . .
H2 H 0.5579 0.3236 -0.0854 0.049 Uiso 1 1 calc R . .
C3 C 0.6228(4) 0.2485(4) -0.0579(2) 0.0440(17) Uani 1 1 d . . .
H3 H 0.6414 0.2296 -0.0836 0.053 Uiso 1 1 calc R . .
C4 C 0.6443(3) 0.2209(3) -0.0186(2) 0.0369(15) Uani 1 1 d . . .
H4 H 0.6781 0.1834 -0.0176 0.044 Uiso 1 1 calc R . .
C5 C 0.6157(3) 0.2491(3) 0.0196(2) 0.0333(14) Uani 1 1 d . . .
C6 C 0.6368(3) 0.2213(3) 0.06514(19) 0.0252(13) Uani 1 1 d . . .
C7 C 0.3499(3) 0.3616(3) 0.06326(19) 0.0293(13) Uani 1 1 d . . .
C8 C 0.2824(3) 0.3940(3) 0.0675(2) 0.0364(15) Uani 1 1 d . . .
H8 H 0.2414 0.3666 0.0741 0.044 Uiso 1 1 calc R . .
C9 C 0.2775(4) 0.4681(3) 0.0617(3) 0.0522(19) Uani 1 1 d . . .
H9 H 0.2331 0.4915 0.0651 0.063 Uiso 1 1 calc R . .
C10 C 0.3381(4) 0.5068(4) 0.0510(3) 0.065(2) Uani 1 1 d . . .
H10 H 0.3350 0.5562 0.0453 0.078 Uiso 1 1 calc R . .
C11 C 0.4032(4) 0.4716(3) 0.0490(3) 0.052(2) Uani 1 1 d . . .
H11 H 0.4446 0.4988 0.0429 0.063 Uiso 1 1 calc R . .
C12 C 0.7114(3) 0.3257(3) 0.0790(2) 0.0454(17) Uani 1 1 d . . .
H12A H 0.7142 0.3435 0.0497 0.068 Uiso 1 1 calc R . .
H12B H 0.7545 0.3394 0.0946 0.068 Uiso 1 1 calc R . .
H12C H 0.6696 0.3462 0.0931 0.068 Uiso 1 1 calc R . .
N1 N 0.5669(2) 0.3034(2) 0.01872(16) 0.0290(11) Uani 1 1 d . . .
N2 N 0.4105(3) 0.4002(2) 0.05519(18) 0.0376(13) Uani 1 1 d . . .
N97 N 0.5615(5) 0.5700(3) 0.0883(2) 0.082(2) Uani 1 1 d . . .
N98 N 0.5711(3) 0.5099(3) 0.08057(18) 0.0450(14) Uani 1 1 d . . .
N99 N 0.5830(3) 0.4494(3) 0.0717(2) 0.0544(17) Uani 1 1 d . . .
O1 O 0.58278(19) 0.23619(19) 0.09476(12) 0.0266(9) Uani 1 1 d . . .
O2 O 0.7054(2) 0.2495(2) 0.07848(14) 0.0352(10) Uani 1 1 d . . .
Cd1 Cd 0.51870(2) 0.34733(2) 0.082667(14) 0.02593(16) 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
C1 N1 1.341(7) . ?
C1 C2 1.372(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.369(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.366(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(8) . ?
C4 H4 0.9300 . ?
C5 N1 1.344(7) . ?
C5 C6 1.539(9) . ?
C6 O1 1.376(6) . ?
C6 O2 1.425(6) . ?
C6 C7 1.547(7) 3_655 ?
C7 N2 1.346(7) . ?
C7 C8 1.386(8) . ?
C7 C6 1.547(7) 3_655 ?
C8 C9 1.379(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.363(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.365(9) . ?
C10 H10 0.9300 . ?
C11 N2 1.336(7) . ?
C11 H11 0.9300 . ?
C12 O2 1.409(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N1 Cd1 2.301(5) . ?
N2 Cd1 2.373(5) . ?
N97 N98 1.146(8) . ?
N98 N99 1.167(7) . ?
N99 Cd1 2.247(5) . ?
O1 Cd1 2.246(4) 26_565 ?
O1 Cd1 2.392(3) . ?
O1 Cd1 2.449(4) 3_655 ?
Cd1 O1 2.246(4) 20_656 ?
Cd1 O1 2.449(4) 3_655 ?

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 C1 C2 123.4(6) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 118.2(6) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C4 C3 C2 119.6(6) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.7(6) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 121.0(6) . . ?
N1 C5 C6 115.8(5) . . ?
C4 C5 C6 123.2(5) . . ?
O1 C6 O2 112.2(4) . . ?
O1 C6 C5 110.5(4) . . ?
O2 C6 C5 111.4(4) . . ?
O1 C6 C7 109.6(4) . 3_655 ?
O2 C6 C7 103.3(4) . 3_655 ?
C5 C6 C7 109.5(5) . 3_655 ?
N2 C7 C8 122.3(5) . . ?
N2 C7 C6 113.4(5) . 3_655 ?
C8 C7 C6 124.3(5) . 3_655 ?
C9 C8 C7 118.2(6) . . ?
C9 C8 H8 120.9 . . ?
C7 C8 H8 120.9 . . ?
C10 C9 C8 119.7(6) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 118.9(6) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
N2 C11 C10 123.2(6) . . ?
N2 C11 H11 118.4 . . ?
C10 C11 H11 118.4 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 N1 C5 118.1(5) . . ?
C1 N1 Cd1 121.8(4) . . ?
C5 N1 Cd1 120.1(4) . . ?
C11 N2 C7 117.6(5) . . ?
C11 N2 Cd1 122.6(4) . . ?
C7 N2 Cd1 114.5(4) . . ?
N97 N98 N99 177.5(8) . . ?
N98 N99 Cd1 131.6(5) . . ?
C6 O1 Cd1 124.2(3) . 26_565 ?
C6 O1 Cd1 115.1(3) . . ?
Cd1 O1 Cd1 104.31(14) 26_565 . ?
C6 O1 Cd1 109.1(3) . 3_655 ?
Cd1 O1 Cd1 102.49(14) 26_565 3_655 ?
Cd1 O1 Cd1 97.90(13) . 3_655 ?
C12 O2 C6 115.8(4) . . ?
O1 Cd1 N99 105.6(2) 20_656 . ?
O1 Cd1 N1 145.06(14) 20_656 . ?
N99 Cd1 N1 87.87(19) . . ?
O1 Cd1 N2 111.59(16) 20_656 . ?
N99 Cd1 N2 92.64(19) . . ?
N1 Cd1 N2 99.51(18) . . ?
O1 Cd1 O1 76.33(14) 20_656 . ?
N99 Cd1 O1 118.63(17) . . ?
N1 Cd1 O1 68.98(14) . . ?
N2 Cd1 O1 145.16(14) . . ?
O1 Cd1 O1 75.17(13) 20_656 3_655 ?
N99 Cd1 O1 161.88(16) . 3_655 ?
N1 Cd1 O1 101.74(14) . 3_655 ?
N2 Cd1 O1 70.78(14) . 3_655 ?
O1 Cd1 O1 79.37(13) . 3_655 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.132
####################################################################### 
# 
# 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_cd79
_database_code_depnum_ccdc_archive 'CCDC 1446469'
_audit_update_record             
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H40 Cd4 N20 O8'
_chemical_formula_sum            'C46 H40 Cd4 N20 O8'
_chemical_formula_weight         1450.58

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   13.4980(5)
_cell_length_b                   12.6484(6)
_cell_length_c                   15.9441(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.628(4)
_cell_angle_gamma                90.00
_cell_volume                     2594.29(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    3806
_cell_measurement_theta_min      3.8500
_cell_measurement_theta_max      27.4800

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;CrysAlis RED, (2005)
;
_exptl_absorpt_correction_T_min  0.85469
_exptl_absorpt_correction_T_max  1.00000

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295.0
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10617
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.44
_diffrn_reflns_theta_max         25.05
_reflns_number_total             4578
_reflns_number_gt                3518
_reflns_threshold_expression     >2sigma(I)

#========================================================================== 
#
# REFINEMENT DATA

_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0301P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4578
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0649
_refine_ls_wR_factor_gt          0.0596
_refine_ls_goodness_of_fit_ref   0.978
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2453(3) 0.7519(4) 0.4726(3) 0.0515(11) Uani 1 1 d . . .
H1 H 0.1880 0.7966 0.4561 0.062 Uiso 1 1 calc R . .
C2 C 0.3431(4) 0.7964(4) 0.4998(3) 0.0662(13) Uani 1 1 d . . .
H2 H 0.3522 0.8693 0.5016 0.079 Uiso 1 1 calc R . .
C3 C 0.4254(4) 0.7297(4) 0.5240(4) 0.0797(16) Uani 1 1 d . . .
H3 H 0.4926 0.7568 0.5422 0.096 Uiso 1 1 calc R . .
C4 C 0.4104(3) 0.6224(4) 0.5218(3) 0.0653(13) Uani 1 1 d . . .
H4 H 0.4671 0.5768 0.5383 0.078 Uiso 1 1 calc R . .
C5 C 0.3109(3) 0.5827(3) 0.4950(2) 0.0428(10) Uani 1 1 d . . .
C6 C 0.2851(3) 0.4650(3) 0.4934(2) 0.0401(9) Uani 1 1 d . . .
C7 C 0.2737(3) 0.4146(3) 0.4024(2) 0.0425(10) Uani 1 1 d . . .
C8 C 0.3283(3) 0.4481(4) 0.3474(3) 0.0640(13) Uani 1 1 d . . .
H8 H 0.3723 0.5062 0.3625 0.077 Uiso 1 1 calc R . .
C9 C 0.3172(4) 0.3946(6) 0.2690(3) 0.0852(18) Uani 1 1 d . . .
H9 H 0.3537 0.4155 0.2308 0.102 Uiso 1 1 calc R . .
C10 C 0.2501(5) 0.3091(5) 0.2496(3) 0.0842(18) Uani 1 1 d . . .
H10 H 0.2413 0.2709 0.1980 0.101 Uiso 1 1 calc R . .
C11 C 0.1971(4) 0.2814(4) 0.3062(3) 0.0662(13) Uani 1 1 d . . .
H11 H 0.1519 0.2242 0.2922 0.079 Uiso 1 1 calc R . .
C12 C 0.3905(3) 0.4177(4) 0.6399(3) 0.0676(14) Uani 1 1 d . . .
H12A H 0.3334 0.3852 0.6541 0.101 Uiso 1 1 calc R . .
H12B H 0.3946 0.4910 0.6564 0.101 Uiso 1 1 calc R . .
H12C H 0.4540 0.3828 0.6713 0.101 Uiso 1 1 calc R . .
C13 C 0.0653(3) 0.5340(4) 0.2313(3) 0.0550(11) Uani 1 1 d . . .
H13 H 0.1149 0.5875 0.2438 0.066 Uiso 1 1 calc R . .
C14 C 0.0347(4) 0.4907(4) 0.1478(3) 0.0675(14) Uani 1 1 d . . .
H14 H 0.0646 0.5127 0.1053 0.081 Uiso 1 1 calc R . .
C15 C -0.0403(4) 0.4151(4) 0.1295(3) 0.0691(14) Uani 1 1 d . . .
H15 H -0.0634 0.3855 0.0735 0.083 Uiso 1 1 calc R . .
C16 C -0.0817(3) 0.3824(4) 0.1935(2) 0.0511(11) Uani 1 1 d . . .
H16 H -0.1334 0.3309 0.1812 0.061 Uiso 1 1 calc R . .
C17 C -0.0459(3) 0.4268(3) 0.2769(2) 0.0365(9) Uani 1 1 d . . .
C18 C -0.0926(2) 0.3977(3) 0.3499(2) 0.0349(9) Uani 1 1 d . . .
C19 C -0.1191(3) 0.2802(3) 0.3474(2) 0.0379(9) Uani 1 1 d . . .
C20 C -0.2194(3) 0.2431(4) 0.3133(3) 0.0543(11) Uani 1 1 d . . .
H20 H -0.2736 0.2899 0.2888 0.065 Uiso 1 1 calc R . .
C21 C -0.2386(4) 0.1369(4) 0.3159(3) 0.0709(14) Uani 1 1 d . . .
H21 H -0.3060 0.1110 0.2936 0.085 Uiso 1 1 calc R . .
C22 C -0.1576(4) 0.0695(4) 0.3518(3) 0.0726(15) Uani 1 1 d . . .
H22 H -0.1685 -0.0029 0.3537 0.087 Uiso 1 1 calc R . .
C23 C -0.0604(4) 0.1113(4) 0.3847(3) 0.0626(13) Uani 1 1 d . . .
H23 H -0.0054 0.0655 0.4093 0.075 Uiso 1 1 calc R . .
N1 N 0.2290(2) 0.6480(3) 0.46865(19) 0.0405(8) Uani 1 1 d . . .
N2 N 0.2076(2) 0.3334(3) 0.3816(2) 0.0492(9) Uani 1 1 d . . .
N3 N 0.0263(2) 0.5019(3) 0.29498(18) 0.0409(8) Uani 1 1 d . . .
N4 N -0.0399(2) 0.2153(3) 0.3834(2) 0.0475(8) Uani 1 1 d . . .
N94 N 0.2607(5) 0.0417(5) 0.4299(4) 0.158(3) Uani 1 1 d . . .
N95 N 0.2282(3) 0.0934(4) 0.4744(3) 0.0782(13) Uani 1 1 d . . .
N96 N 0.1965(3) 0.1430(3) 0.5215(3) 0.0732(12) Uani 1 1 d . . .
N97 N -0.0261(4) 0.8438(5) 0.3122(4) 0.122(2) Uani 1 1 d . . .
N98 N -0.0321(3) 0.7765(3) 0.3573(3) 0.0571(10) Uani 1 1 d . . .
N99 N -0.0411(3) 0.7079(3) 0.4037(2) 0.0502(9) Uani 1 1 d . . .
O1 O 0.19872(16) 0.44926(19) 0.51914(15) 0.0355(6) Uani 1 1 d . . .
O2 O 0.37495(18) 0.4093(2) 0.54787(17) 0.0488(7) Uani 1 1 d . . .
O3 O -0.02450(16) 0.42079(18) 0.43213(13) 0.0307(5) Uani 1 1 d . . .
O4 O -0.18448(17) 0.4587(2) 0.33098(15) 0.0437(7) Uani 1 1 d . . .
H4A H -0.1921 0.4806 0.3770 0.066 Uiso 1 1 calc R . .
Cd2 Cd 0.111730(19) 0.29311(2) 0.480373(17) 0.03763(10) Uani 1 1 d . . .
Cd1 Cd 0.069483(18) 0.56844(2) 0.438817(16) 0.03417(9) 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
C1 N1 1.331(5) . ?
C1 C2 1.379(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.356(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.370(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(5) . ?
C4 H4 0.9300 . ?
C5 N1 1.341(5) . ?
C5 C6 1.528(5) . ?
C6 O1 1.363(4) . ?
C6 O2 1.443(4) . ?
C6 C7 1.549(5) . ?
C7 N2 1.335(5) . ?
C7 C8 1.371(6) . ?
C8 C9 1.390(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.384(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.356(7) . ?
C10 H10 0.9300 . ?
C11 N2 1.340(5) . ?
C11 H11 0.9300 . ?
C12 O2 1.422(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N3 1.341(5) . ?
C13 C14 1.382(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.358(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.367(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.389(5) . ?
C16 H16 0.9300 . ?
C17 N3 1.328(5) . ?
C17 C18 1.527(5) . ?
C18 O3 1.385(4) . ?
C18 O4 1.414(4) . ?
C18 C19 1.526(5) . ?
C19 N4 1.331(5) . ?
C19 C20 1.380(5) . ?
C20 C21 1.371(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.367(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.363(6) . ?
C22 H22 0.9300 . ?
C23 N4 1.346(5) . ?
C23 H23 0.9300 . ?
N1 Cd1 2.291(3) . ?
N2 Cd2 2.376(3) . ?
N3 Cd1 2.345(3) . ?
N4 Cd2 2.373(3) . ?
N94 N95 1.146(6) . ?
N95 N96 1.156(5) . ?
N96 Cd2 2.211(4) . ?
N97 N98 1.133(5) . ?
N98 N99 1.170(5) . ?
N99 Cd1 2.269(3) . ?
N99 Cd2 2.322(3) 3_566 ?
O1 Cd2 2.285(2) . ?
O1 Cd1 2.367(2) . ?
O3 Cd1 2.242(2) . ?
O3 Cd1 2.319(2) 3_566 ?
O3 Cd2 2.393(2) . ?
O4 H4A 0.8200 . ?
Cd2 N99 2.322(3) 3_566 ?
Cd1 O3 2.319(2) 3_566 ?

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 C1 C2 123.2(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 117.4(4) . . ?
C3 C2 H2 121.3 . . ?
C1 C2 H2 121.3 . . ?
C2 C3 C4 120.5(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 119.5(4) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 120.5(4) . . ?
N1 C5 C6 115.6(3) . . ?
C4 C5 C6 123.8(4) . . ?
O1 C6 O2 112.8(3) . . ?
O1 C6 C5 110.4(3) . . ?
O2 C6 C5 108.7(3) . . ?
O1 C6 C7 111.8(3) . . ?
O2 C6 C7 101.0(3) . . ?
C5 C6 C7 112.0(3) . . ?
N2 C7 C8 121.8(4) . . ?
N2 C7 C6 114.7(3) . . ?
C8 C7 C6 123.5(4) . . ?
C7 C8 C9 119.5(5) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C10 C9 C8 117.8(5) . . ?
C10 C9 H9 121.1 . . ?
C8 C9 H9 121.1 . . ?
C11 C10 C9 119.6(5) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
N2 C11 C10 122.5(5) . . ?
N2 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 122.5(4) . . ?
N3 C13 H13 118.7 . . ?
C14 C13 H13 118.7 . . ?
C15 C14 C13 118.2(4) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C14 C15 C16 119.9(4) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 119.3(4) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
N3 C17 C16 121.2(4) . . ?
N3 C17 C18 116.9(3) . . ?
C16 C17 C18 121.8(3) . . ?
O3 C18 O4 112.0(3) . . ?
O3 C18 C19 108.3(3) . . ?
O4 C18 C19 110.0(3) . . ?
O3 C18 C17 111.2(3) . . ?
O4 C18 C17 104.1(3) . . ?
C19 C18 C17 111.2(3) . . ?
N4 C19 C20 121.6(4) . . ?
N4 C19 C18 116.0(3) . . ?
C20 C19 C18 122.3(4) . . ?
C21 C20 C19 119.5(4) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C22 C21 C20 119.3(4) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C23 C22 C21 118.3(5) . . ?
C23 C22 H22 120.9 . . ?
C21 C22 H22 120.9 . . ?
N4 C23 C22 123.4(4) . . ?
N4 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
C1 N1 C5 118.9(3) . . ?
C1 N1 Cd1 125.1(3) . . ?
C5 N1 Cd1 115.4(2) . . ?
C7 N2 C11 118.7(4) . . ?
C7 N2 Cd2 117.3(2) . . ?
C11 N2 Cd2 124.0(3) . . ?
C17 N3 C13 118.9(3) . . ?
C17 N3 Cd1 114.7(2) . . ?
C13 N3 Cd1 126.4(3) . . ?
C19 N4 C23 117.9(4) . . ?
C19 N4 Cd2 116.6(2) . . ?
C23 N4 Cd2 122.4(3) . . ?
N94 N95 N96 177.7(6) . . ?
N95 N96 Cd2 122.2(3) . . ?
N97 N98 N99 178.1(5) . . ?
N98 N99 Cd1 123.1(3) . . ?
N98 N99 Cd2 130.8(3) . 3_566 ?
Cd1 N99 Cd2 101.37(13) . 3_566 ?
C6 O1 Cd2 117.4(2) . . ?
C6 O1 Cd1 107.56(19) . . ?
Cd2 O1 Cd1 99.79(8) . . ?
C12 O2 C6 114.8(3) . . ?
C18 O3 Cd1 115.1(2) . . ?
C18 O3 Cd1 125.12(19) . 3_566 ?
Cd1 O3 Cd1 101.84(8) . 3_566 ?
C18 O3 Cd2 112.75(19) . . ?
Cd1 O3 Cd2 100.27(8) . . ?
Cd1 O3 Cd2 97.85(8) 3_566 . ?
C18 O4 H4A 109.5 . . ?
N96 Cd2 O1 118.99(13) . . ?
N96 Cd2 N99 93.39(14) . 3_566 ?
O1 Cd2 N99 95.21(11) . 3_566 ?
N96 Cd2 N4 95.97(14) . . ?
O1 Cd2 N4 143.68(10) . . ?
N99 Cd2 N4 92.01(12) 3_566 . ?
N96 Cd2 N2 92.54(14) . . ?
O1 Cd2 N2 69.85(10) . . ?
N99 Cd2 N2 164.96(13) 3_566 . ?
N4 Cd2 N2 101.11(11) . . ?
N96 Cd2 O3 162.38(13) . . ?
O1 Cd2 O3 77.61(7) . . ?
N99 Cd2 O3 78.40(9) 3_566 . ?
N4 Cd2 O3 69.08(9) . . ?
N2 Cd2 O3 99.31(9) . . ?
O3 Cd1 N99 108.39(11) . . ?
O3 Cd1 N1 149.08(10) . . ?
N99 Cd1 N1 102.49(12) . . ?
O3 Cd1 O3 78.16(8) . 3_566 ?
N99 Cd1 O3 81.02(10) . 3_566 ?
N1 Cd1 O3 105.78(9) . 3_566 ?
O3 Cd1 N3 71.63(10) . . ?
N99 Cd1 N3 95.02(11) . . ?
N1 Cd1 N3 107.48(11) . . ?
O3 Cd1 N3 146.56(9) 3_566 . ?
O3 Cd1 O1 78.98(8) . . ?
N99 Cd1 O1 161.94(10) . . ?
N1 Cd1 O1 71.05(10) . . ?
O3 Cd1 O1 84.57(8) 3_566 . ?
N3 Cd1 O1 102.99(9) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.084
####################################################################### 
# 
# 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_cd129
_database_code_depnum_ccdc_archive 'CCDC 1446470'
_audit_update_record             
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H44 Cd4 N12 O12'
_chemical_formula_sum            'C52 H44 Cd4 N12 O12'
_chemical_formula_weight         1478.59

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

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I41/acd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'y+3/4, x+1/4, -z+1/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'y+5/4, x+3/4, -z+3/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'x-1/2, -y, z'
'-y-3/4, -x-1/4, z-1/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-y-1/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   18.4690(7)
_cell_length_b                   18.4690(7)
_cell_length_c                   30.558(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10423.4(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    2164
_cell_measurement_theta_min      3.7140
_cell_measurement_theta_max      26.4060

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5824
_exptl_absorpt_coefficient_mu    1.686
__exptl_absorpt_correction_type  empirical
_exptl_absorpt_process_details   
;CrysAlis RED, (2005)
;
_exptl_absorpt_correction_T_min  0.37536
_exptl_absorpt_correction_T_max  1.00000

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295.0
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13401
_diffrn_reflns_av_R_equivalents  0.1223
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         25.05
_reflns_number_total             2299
_reflns_number_gt                1659
_reflns_threshold_expression     >2sigma(I)

#========================================================================== 
#
# REFINEMENT DATA

_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0814P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2299
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1500
_refine_ls_wR_factor_gt          0.1339
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5979(5) 0.4684(5) 0.5493(3) 0.060(3) Uani 1 1 d . . .
H1 H 0.5565 0.4958 0.5440 0.072 Uiso 1 1 calc R . .
C2 C 0.6633(5) 0.5037(5) 0.5504(4) 0.069(3) Uani 1 1 d . . .
H2 H 0.6666 0.5530 0.5443 0.083 Uiso 1 1 calc R . .
C3 C 0.7233(5) 0.4642(4) 0.5608(3) 0.061(2) Uani 1 1 d . . .
H3 H 0.7680 0.4869 0.5642 0.073 Uiso 1 1 calc R . .
C4 C 0.7171(4) 0.3896(4) 0.5664(3) 0.0424(19) Uani 1 1 d . . .
H4 H 0.7576 0.3616 0.5727 0.051 Uiso 1 1 calc R . .
C5 C 0.6500(4) 0.3584(4) 0.5623(2) 0.0358(17) Uani 1 1 d . . .
C6 C 0.6360(4) 0.2776(4) 0.5642(2) 0.0309(16) Uani 1 1 d . . .
C7 C 0.3860(4) 0.2512(4) 0.5186(3) 0.0390(19) Uani 1 1 d . . .
C8 C 0.3564(4) 0.2237(5) 0.4806(2) 0.0440(19) Uani 1 1 d . . .
H8 H 0.3219 0.1870 0.4816 0.053 Uiso 1 1 calc R . .
C9 C 0.3787(5) 0.2514(5) 0.4415(3) 0.053(2) Uani 1 1 d . . .
H9 H 0.3606 0.2327 0.4155 0.064 Uiso 1 1 calc R . .
C10 C 0.4274(5) 0.3063(5) 0.4406(3) 0.051(2) Uani 1 1 d . . .
H10 H 0.4418 0.3265 0.4141 0.061 Uiso 1 1 calc R . .
C11 C 0.4548(5) 0.3316(4) 0.4790(3) 0.0449(19) Uani 1 1 d . . .
H11 H 0.4887 0.3688 0.4783 0.054 Uiso 1 1 calc R . .
C12 C 0.7090(5) 0.1700(4) 0.5776(3) 0.055(2) Uani 1 1 d . . .
H12A H 0.7073 0.1512 0.5484 0.082 Uiso 1 1 calc R . .
H12B H 0.6691 0.1509 0.5942 0.082 Uiso 1 1 calc R . .
H12C H 0.7537 0.1560 0.5912 0.082 Uiso 1 1 calc R . .
C99 C 0.4250(5) 0.5106(5) 0.5798(3) 0.053(2) Uani 1 1 d . . .
N1 N 0.5900(3) 0.3977(3) 0.5551(2) 0.0470(18) Uani 1 1 d . . .
N2 N 0.4345(3) 0.3044(3) 0.51737(19) 0.0352(14) Uani 1 1 d . . .
N99 N 0.4230(4) 0.4505(4) 0.5750(2) 0.0558(19) Uani 1 1 d . . .
O1 O 0.5831(3) 0.2612(2) 0.59421(17) 0.0332(12) Uani 1 1 d . . .
O2 O 0.7042(3) 0.2467(2) 0.57636(16) 0.0397(12) Uani 1 1 d . . .
O99 O 0.4279(6) 0.5748(4) 0.5852(3) 0.126(4) Uani 1 1 d . . .
Cd1 Cd 0.48187(3) 0.34742(3) 0.582855(18) 0.0324(3) 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
C1 N1 1.326(10) . ?
C1 C2 1.373(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.365(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(10) . ?
C4 H4 0.9300 . ?
C5 N1 1.343(10) . ?
C5 C6 1.514(10) . ?
C6 O1 1.375(9) . ?
C6 O2 1.432(8) . ?
C6 C7 1.545(11) 3_655 ?
C7 N2 1.330(9) . ?
C7 C8 1.380(11) . ?
C7 C6 1.545(11) 3_655 ?
C8 C9 1.365(11) . ?
C8 H8 0.9300 . ?
C9 C10 1.355(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.360(11) . ?
C10 H10 0.9300 . ?
C11 N2 1.330(9) . ?
C11 H11 0.9300 . ?
C12 O2 1.421(9) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C99 N99 1.120(11) . ?
C99 O99 1.200(11) . ?
N1 Cd1 2.360(6) . ?
N2 Cd1 2.324(6) . ?
N99 Cd1 2.205(7) . ?
O1 Cd1 2.248(5) 26_566 ?
O1 Cd1 2.363(5) 3_655 ?
O1 Cd1 2.481(5) . ?
Cd1 O1 2.248(5) 20_657 ?
Cd1 O1 2.363(5) 3_655 ?

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 C1 C2 124.1(8) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C3 C2 C1 117.8(8) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C4 119.4(8) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 118.7(7) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N1 C5 C4 122.2(7) . . ?
N1 C5 C6 113.4(6) . . ?
C4 C5 C6 124.4(7) . . ?
O1 C6 O2 111.2(6) . . ?
O1 C6 C5 111.3(5) . . ?
O2 C6 C5 104.6(6) . . ?
O1 C6 C7 109.8(6) . 3_655 ?
O2 C6 C7 109.2(5) . 3_655 ?
C5 C6 C7 110.5(6) . 3_655 ?
N2 C7 C8 121.1(8) . . ?
N2 C7 C6 117.2(7) . 3_655 ?
C8 C7 C6 121.8(6) . 3_655 ?
C9 C8 C7 118.5(8) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C10 C9 C8 120.0(8) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 119.1(8) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
N2 C11 C10 121.8(8) . . ?
N2 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N99 C99 O99 179.3(14) . . ?
C1 N1 C5 117.6(7) . . ?
C1 N1 Cd1 121.9(5) . . ?
C5 N1 Cd1 115.3(5) . . ?
C11 N2 C7 119.5(7) . . ?
C11 N2 Cd1 121.6(5) . . ?
C7 N2 Cd1 118.8(5) . . ?
C99 N99 Cd1 145.5(8) . . ?
C6 O1 Cd1 124.5(4) . 26_566 ?
C6 O1 Cd1 116.8(4) . 3_655 ?
Cd1 O1 Cd1 104.69(19) 26_566 3_655 ?
C6 O1 Cd1 107.5(4) . . ?
Cd1 O1 Cd1 100.98(19) 26_566 . ?
Cd1 O1 Cd1 98.12(17) 3_655 . ?
C12 O2 C6 117.4(6) . . ?
N99 Cd1 O1 103.7(2) . 20_657 ?
N99 Cd1 N2 90.9(2) . . ?
O1 Cd1 N2 146.63(19) 20_657 . ?
N99 Cd1 N1 92.2(3) . . ?
O1 Cd1 N1 110.7(2) 20_657 . ?
N2 Cd1 N1 98.3(2) . . ?
N99 Cd1 O1 119.9(2) . 3_655 ?
O1 Cd1 O1 77.52(19) 20_657 3_655 ?
N2 Cd1 O1 69.21(19) . 3_655 ?
N1 Cd1 O1 144.73(19) . 3_655 ?
N99 Cd1 O1 160.2(2) . . ?
O1 Cd1 O1 75.11(18) 20_657 . ?
N2 Cd1 O1 100.65(19) . . ?
N1 Cd1 O1 70.40(19) . . ?
O1 Cd1 O1 79.50(18) 3_655 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.178
####################################################################### 
# 
# 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_cd131
_database_code_depnum_ccdc_archive 'CCDC 1446471'
_audit_update_record             
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H40 Cd4 N12 O12'
_chemical_formula_sum            'C50 H40 Cd4 N12 O12'
_chemical_formula_weight         1450.54

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   13.4790(9)
_cell_length_b                   12.6998(6)
_cell_length_c                   15.9841(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.524(8)
_cell_angle_gamma                90.00
_cell_volume                     2623.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    3120
_cell_measurement_theta_min      3.4460
_cell_measurement_theta_max      28.8110

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;CrysAlis RED, (2005)
;
_exptl_absorpt_correction_T_min  0.64733
_exptl_absorpt_correction_T_max  1.00000

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295.0
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11587
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         25.05
_reflns_number_total             4626
_reflns_number_gt                3393
_reflns_threshold_expression     >2sigma(I)

#========================================================================== 
#
# REFINEMENT DATA

_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0903P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4626
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1556
_refine_ls_wR_factor_gt          0.1395
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2532(6) 0.7515(6) 0.0244(6) 0.052(2) Uani 1 1 d . . .
H1 H 0.3095 0.7971 0.0393 0.063 Uiso 1 1 calc R . .
C2 C 0.1549(8) 0.7929(8) -0.0024(7) 0.072(3) Uani 1 1 d . . .
H2 H 0.1444 0.8654 -0.0050 0.086 Uiso 1 1 calc R . .
C3 C 0.0719(7) 0.7240(7) -0.0254(8) 0.071(3) Uani 1 1 d . . .
H3 H 0.0046 0.7498 -0.0435 0.085 Uiso 1 1 calc R . .
C4 C 0.0893(6) 0.6185(7) -0.0214(7) 0.063(3) Uani 1 1 d . . .
H4 H 0.0340 0.5717 -0.0364 0.076 Uiso 1 1 calc R . .
C5 C 0.1900(6) 0.5810(6) 0.0051(5) 0.0417(18) Uani 1 1 d . . .
C6 C 0.2170(5) 0.4631(6) 0.0097(5) 0.0401(18) Uani 1 1 d . . .
C7 C 0.2275(6) 0.4165(6) 0.0996(5) 0.0433(19) Uani 1 1 d . . .
C8 C 0.1691(7) 0.4494(9) 0.1560(6) 0.069(3) Uani 1 1 d . . .
H8 H 0.1223 0.5048 0.1400 0.083 Uiso 1 1 calc R . .
C9 C 0.1817(10) 0.3993(12) 0.2340(7) 0.089(4) Uani 1 1 d . . .
H9 H 0.1453 0.4215 0.2723 0.107 Uiso 1 1 calc R . .
C10 C 0.2489(11) 0.3159(12) 0.2551(7) 0.096(4) Uani 1 1 d . . .
H10 H 0.2574 0.2801 0.3074 0.116 Uiso 1 1 calc R . .
C11 C 0.3042(9) 0.2852(7) 0.1982(6) 0.071(3) Uani 1 1 d . . .
H11 H 0.3490 0.2281 0.2124 0.085 Uiso 1 1 calc R . .
C12 C 0.1134(7) 0.4080(8) -0.1338(6) 0.064(3) Uani 1 1 d . . .
H12A H 0.0521 0.3692 -0.1627 0.096 Uiso 1 1 calc R . .
H12B H 0.1722 0.3765 -0.1467 0.096 Uiso 1 1 calc R . .
H12C H 0.1062 0.4795 -0.1540 0.096 Uiso 1 1 calc R . .
C13 C 0.4313(7) 0.5407(7) 0.2677(6) 0.056(2) Uani 1 1 d . . .
H13 H 0.3819 0.5939 0.2547 0.068 Uiso 1 1 calc R . .
C14 C 0.4612(8) 0.4996(9) 0.3500(6) 0.070(3) Uani 1 1 d . . .
H14 H 0.4308 0.5232 0.3920 0.084 Uiso 1 1 calc R . .
C15 C 0.5348(9) 0.4246(8) 0.3701(6) 0.071(3) Uani 1 1 d . . .
H15 H 0.5555 0.3961 0.4259 0.085 Uiso 1 1 calc R . .
C16 C 0.5789(7) 0.3909(7) 0.3077(5) 0.054(2) Uani 1 1 d . . .
H16 H 0.6314 0.3408 0.3211 0.064 Uiso 1 1 calc R . .
C17 C 0.5441(5) 0.4327(5) 0.2231(5) 0.0350(16) Uani 1 1 d . . .
C18 C 0.5921(5) 0.4020(5) 0.1497(4) 0.0323(16) Uani 1 1 d . . .
C19 C 0.6216(6) 0.2849(5) 0.1557(5) 0.0390(17) Uani 1 1 d . . .
C20 C 0.7209(6) 0.2496(6) 0.1899(5) 0.051(2) Uani 1 1 d . . .
H20 H 0.7744 0.2967 0.2135 0.061 Uiso 1 1 calc R . .
C21 C 0.7405(7) 0.1421(7) 0.1890(6) 0.061(2) Uani 1 1 d . . .
H21 H 0.8075 0.1167 0.2118 0.073 Uiso 1 1 calc R . .
C22 C 0.6613(8) 0.0739(6) 0.1545(6) 0.065(3) Uani 1 1 d . . .
H22 H 0.6729 0.0017 0.1540 0.078 Uiso 1 1 calc R . .
C23 C 0.5631(7) 0.1152(6) 0.1202(6) 0.053(2) Uani 1 1 d . . .
H23 H 0.5088 0.0694 0.0955 0.063 Uiso 1 1 calc R . .
C96 C 0.2751(9) 0.0852(8) 0.0274(7) 0.074(3) Uani 1 1 d . . .
C99 C 0.5313(6) 0.7811(7) 0.1400(7) 0.058(2) Uani 1 1 d . . .
N1 N 0.2702(5) 0.6481(5) 0.0296(4) 0.0416(15) Uani 1 1 d . . .
N2 N 0.2939(5) 0.3364(5) 0.1236(4) 0.0518(18) Uani 1 1 d . . .
N3 N 0.4717(5) 0.5059(5) 0.2050(4) 0.0396(14) Uani 1 1 d . . .
N4 N 0.5427(5) 0.2197(5) 0.1212(5) 0.0492(17) Uani 1 1 d . . .
N96 N 0.3030(6) 0.1463(6) -0.0126(6) 0.072(2) Uani 1 1 d . . .
N99 N 0.5347(5) 0.7126(5) 0.0931(5) 0.0478(17) Uani 1 1 d . . .
O1 O 0.3034(3) 0.4472(4) -0.0159(3) 0.0364(11) Uani 1 1 d . . .
O2 O 0.1277(4) 0.4060(4) -0.0431(3) 0.0470(13) Uani 1 1 d . . .
O3 O 0.5245(3) 0.4230(3) 0.0688(3) 0.0274(10) Uani 1 1 d . . .
O4 O 0.6834(4) 0.4630(4) 0.1681(3) 0.0418(12) Uani 1 1 d . . .
H4A H 0.6920 0.4847 0.1223 0.063 Uiso 1 1 calc R . .
O96 O 0.2411(10) 0.0223(10) 0.0641(8) 0.177(6) Uani 1 1 d . . .
O99 O 0.5296(7) 0.8498(7) 0.1909(7) 0.125(4) Uani 1 1 d . . .
Cd1 Cd 0.43051(4) 0.57022(4) 0.06020(3) 0.0327(2) Uani 1 1 d . . .
Cd2 Cd 0.39085(4) 0.29222(4) 0.02249(4) 0.0389(2) 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
C1 N1 1.332(10) . ?
C1 C2 1.376(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.385(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.359(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(11) . ?
C4 H4 0.9300 . ?
C5 N1 1.343(9) . ?
C5 C6 1.538(10) . ?
C6 O1 1.356(8) . ?
C6 O2 1.452(8) . ?
C6 C7 1.523(11) . ?
C7 N2 1.336(10) . ?
C7 C8 1.418(12) . ?
C8 C9 1.366(15) . ?
C8 H8 0.9300 . ?
C9 C10 1.372(16) . ?
C9 H9 0.9300 . ?
C10 C11 1.384(15) . ?
C10 H10 0.9300 . ?
C11 N2 1.331(11) . ?
C11 H11 0.9300 . ?
C12 O2 1.408(10) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N3 1.345(10) . ?
C13 C14 1.366(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.346(14) . ?
C14 H14 0.9300 . ?
C15 C16 1.367(13) . ?
C15 H15 0.9300 . ?
C16 C17 1.403(11) . ?
C16 H16 0.9300 . ?
C17 N3 1.319(9) . ?
C17 C18 1.543(10) . ?
C18 O3 1.380(8) . ?
C18 O4 1.412(8) . ?
C18 C19 1.535(9) . ?
C19 N4 1.337(9) . ?
C19 C20 1.370(10) . ?
C20 C21 1.392(11) . ?
C20 H20 0.9300 . ?
C21 C22 1.363(13) . ?
C21 H21 0.9300 . ?
C22 C23 1.384(12) . ?
C22 H22 0.9300 . ?
C23 N4 1.356(9) . ?
C23 H23 0.9300 . ?
C96 N96 1.135(12) . ?
C96 O96 1.161(14) . ?
C99 N99 1.159(11) . ?
C99 O99 1.197(12) . ?
N1 Cd1 2.299(6) . ?
N2 Cd2 2.415(7) . ?
N3 Cd1 2.366(6) . ?
N4 Cd2 2.385(6) . ?
N96 Cd2 2.184(7) . ?
N99 Cd1 2.258(6) . ?
N99 Cd2 2.341(7) 3_665 ?
O1 Cd2 2.287(5) . ?
O1 Cd1 2.381(5) . ?
O3 Cd1 2.241(4) . ?
O3 Cd1 2.310(5) 3_665 ?
O3 Cd2 2.408(4) . ?
O4 H4A 0.8200 . ?
Cd1 O3 2.310(5) 3_665 ?
Cd2 N99 2.341(7) 3_665 ?

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 C1 C2 122.0(8) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C1 C2 C3 118.3(9) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 119.7(8) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.6(8) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 120.5(7) . . ?
N1 C5 C6 116.3(6) . . ?
C4 C5 C6 123.1(7) . . ?
O1 C6 O2 113.0(6) . . ?
O1 C6 C7 111.7(6) . . ?
O2 C6 C7 101.2(5) . . ?
O1 C6 C5 110.0(6) . . ?
O2 C6 C5 108.2(6) . . ?
C7 C6 C5 112.4(6) . . ?
N2 C7 C8 119.3(8) . . ?
N2 C7 C6 116.2(7) . . ?
C8 C7 C6 124.4(8) . . ?
C9 C8 C7 119.7(11) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 119.0(11) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C9 C10 C11 119.9(11) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
N2 C11 C10 120.8(11) . . ?
N2 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 121.4(9) . . ?
N3 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 119.7(9) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 119.5(9) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C15 C16 C17 119.3(9) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
N3 C17 C16 120.2(7) . . ?
N3 C17 C18 117.1(6) . . ?
C16 C17 C18 122.6(7) . . ?
O3 C18 O4 113.1(5) . . ?
O3 C18 C19 109.6(5) . . ?
O4 C18 C19 108.9(6) . . ?
O3 C18 C17 110.8(5) . . ?
O4 C18 C17 103.4(5) . . ?
C19 C18 C17 110.8(5) . . ?
N4 C19 C20 122.4(7) . . ?
N4 C19 C18 114.4(6) . . ?
C20 C19 C18 123.2(7) . . ?
C19 C20 C21 118.9(8) . . ?
C19 C20 H20 120.6 . . ?
C21 C20 H20 120.6 . . ?
C22 C21 C20 119.9(8) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 118.0(7) . . ?
C21 C22 H22 121.0 . . ?
C23 C22 H22 121.0 . . ?
N4 C23 C22 122.7(8) . . ?
N4 C23 H23 118.6 . . ?
C22 C23 H23 118.6 . . ?
N96 C96 O96 175.8(13) . . ?
N99 C99 O99 177.6(12) . . ?
C1 N1 C5 119.8(7) . . ?
C1 N1 Cd1 124.9(5) . . ?
C5 N1 Cd1 114.8(5) . . ?
C11 N2 C7 121.3(8) . . ?
C11 N2 Cd2 123.2(7) . . ?
C7 N2 Cd2 115.5(5) . . ?
C17 N3 C13 120.0(7) . . ?
C17 N3 Cd1 114.3(5) . . ?
C13 N3 Cd1 125.7(5) . . ?
C19 N4 C23 118.1(7) . . ?
C19 N4 Cd2 117.8(5) . . ?
C23 N4 Cd2 120.6(5) . . ?
C96 N96 Cd2 132.7(8) . . ?
C99 N99 Cd1 128.0(7) . . ?
C99 N99 Cd2 129.4(6) . 3_665 ?
Cd1 N99 Cd2 100.0(3) . 3_665 ?
C6 O1 Cd2 117.9(4) . . ?
C6 O1 Cd1 107.6(4) . . ?
Cd2 O1 Cd1 100.74(17) . . ?
C12 O2 C6 116.0(6) . . ?
C18 O3 Cd1 115.5(4) . . ?
C18 O3 Cd1 124.9(4) . 3_665 ?
Cd1 O3 Cd1 101.63(16) . 3_665 ?
C18 O3 Cd2 113.0(4) . . ?
Cd1 O3 Cd2 101.30(17) . . ?
Cd1 O3 Cd2 96.58(15) 3_665 . ?
C18 O4 H4A 109.5 . . ?
O3 Cd1 N99 110.5(2) . . ?
O3 Cd1 N1 148.53(19) . . ?
N99 Cd1 N1 101.0(2) . . ?
O3 Cd1 O3 78.37(16) . 3_665 ?
N99 Cd1 O3 82.8(2) . 3_665 ?
N1 Cd1 O3 105.28(18) . 3_665 ?
O3 Cd1 N3 71.37(18) . . ?
N99 Cd1 N3 95.2(2) . . ?
N1 Cd1 N3 107.5(2) . . ?
O3 Cd1 N3 146.86(18) 3_665 . ?
O3 Cd1 O1 78.25(15) . . ?
N99 Cd1 O1 162.5(2) . . ?
N1 Cd1 O1 71.16(19) . . ?
O3 Cd1 O1 84.34(15) 3_665 . ?
N3 Cd1 O1 102.01(19) . . ?
N96 Cd2 O1 117.5(3) . . ?
N96 Cd2 N99 95.6(3) . 3_665 ?
O1 Cd2 N99 96.6(2) . 3_665 ?
N96 Cd2 N4 98.2(3) . . ?
O1 Cd2 N4 142.16(19) . . ?
N99 Cd2 N4 91.9(2) 3_665 . ?
N96 Cd2 O3 165.4(3) . . ?
O1 Cd2 O3 76.83(15) . . ?
N99 Cd2 O3 79.01(19) 3_665 . ?
N4 Cd2 O3 68.70(17) . . ?
N96 Cd2 N2 90.7(3) . . ?
O1 Cd2 N2 69.1(2) . . ?
N99 Cd2 N2 165.7(2) 3_665 . ?
N4 Cd2 N2 100.0(2) . . ?
O3 Cd2 N2 97.71(18) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.377
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.163
####################################################################### 
# 
# 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_cd135
_database_code_depnum_ccdc_archive 'CCDC 1446472'
_audit_update_record             
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H40 Cd4 N16 O14'
_chemical_formula_sum            'C46 H40 Cd4 N16 O14'
_chemical_formula_weight         1490.54

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   13.4664(6)
_cell_length_b                   12.4449(5)
_cell_length_c                   16.1614(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.398(5)
_cell_angle_gamma                90.00
_cell_volume                     2664.00(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    4439
_cell_measurement_theta_min      3.9030
_cell_measurement_theta_max      28.3500

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;CrysAlis RED, (2005)
;
_exptl_absorpt_correction_T_min  0.12453
_exptl_absorpt_correction_T_max  1.00000

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295.0
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13051
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4731
_reflns_number_gt                3736
_reflns_threshold_expression     >2sigma(I)

#========================================================================== 
#
# REFINEMENT DATA

_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0399P)²+1.8030P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4731
_refine_ls_number_parameters     363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2442(4) -0.2538(5) 0.5094(3) 0.0574(13) Uani 1 1 d . . .
H1 H 0.2973 -0.3025 0.5203 0.069 Uiso 1 1 calc R . .
C2 C 0.1493(5) -0.2920(5) 0.4806(5) 0.085(2) Uani 1 1 d . . .
H2 H 0.1374 -0.3652 0.4722 0.102 Uiso 1 1 calc R . .
C3 C 0.0724(5) -0.2195(7) 0.4646(5) 0.105(3) Uani 1 1 d . . .
H3 H 0.0067 -0.2429 0.4454 0.126 Uiso 1 1 calc R . .
C4 C 0.0918(4) -0.1126(6) 0.4766(5) 0.0809(19) Uani 1 1 d . . .
H4 H 0.0395 -0.0629 0.4651 0.097 Uiso 1 1 calc R . .
C5 C 0.1880(4) -0.0786(4) 0.5056(3) 0.0502(13) Uani 1 1 d . . .
C6 C 0.2181(3) 0.0402(4) 0.5191(3) 0.0437(11) Uani 1 1 d . . .
C7 C 0.2227(4) 0.0726(4) 0.6130(4) 0.0547(14) Uani 1 1 d . . .
C8 C 0.1600(4) 0.0296(6) 0.6628(4) 0.0751(18) Uani 1 1 d . . .
H8 H 0.1133 -0.0232 0.6419 0.090 Uiso 1 1 calc R . .
C9 C 0.1673(7) 0.0655(8) 0.7433(5) 0.104(3) Uani 1 1 d . . .
H9 H 0.1259 0.0372 0.7781 0.125 Uiso 1 1 calc R . .
C10 C 0.2356(7) 0.1430(8) 0.7722(4) 0.107(3) Uani 1 1 d . . .
H10 H 0.2420 0.1675 0.8273 0.129 Uiso 1 1 calc R . .
C11 C 0.2950(5) 0.1849(6) 0.7199(4) 0.084(2) Uani 1 1 d . . .
H11 H 0.3406 0.2393 0.7395 0.101 Uiso 1 1 calc R . .
C12 C 0.1323(5) 0.1170(6) 0.3914(4) 0.083(2) Uani 1 1 d . . .
H12A H 0.1275 0.0472 0.3656 0.124 Uiso 1 1 calc R . .
H12B H 0.1920 0.1526 0.3808 0.124 Uiso 1 1 calc R . .
H12C H 0.0739 0.1587 0.3683 0.124 Uiso 1 1 calc R . .
C13 C 0.4079(5) -0.0803(5) 0.7568(4) 0.0759(19) Uani 1 1 d . . .
H13 H 0.3586 -0.1323 0.7406 0.091 Uiso 1 1 calc R . .
C14 C 0.4292(6) -0.0501(7) 0.8396(4) 0.091(2) Uani 1 1 d . . .
H14 H 0.3949 -0.0804 0.8788 0.109 Uiso 1 1 calc R . .
C15 C 0.5011(6) 0.0248(7) 0.8626(4) 0.091(2) Uani 1 1 d . . .
H15 H 0.5164 0.0469 0.9185 0.109 Uiso 1 1 calc R . .
C16 C 0.5520(5) 0.0687(5) 0.8049(3) 0.0682(17) Uani 1 1 d . . .
H16 H 0.6026 0.1193 0.8210 0.082 Uiso 1 1 calc R . .
C17 C 0.5262(4) 0.0360(4) 0.7209(3) 0.0488(12) Uani 1 1 d . . .
C18 C 0.5823(3) 0.0764(4) 0.6520(3) 0.0410(11) Uani 1 1 d . . .
C19 C 0.6149(4) 0.1942(4) 0.6659(3) 0.0475(12) Uani 1 1 d . . .
C20 C 0.7122(4) 0.2227(5) 0.7002(3) 0.0627(15) Uani 1 1 d . . .
H20 H 0.7606 0.1703 0.7182 0.075 Uiso 1 1 calc R . .
C21 C 0.7369(5) 0.3295(6) 0.7075(4) 0.0805(18) Uani 1 1 d . . .
H21 H 0.8026 0.3501 0.7300 0.097 Uiso 1 1 calc R . .
C22 C 0.6654(5) 0.4054(5) 0.6817(4) 0.0815(19) Uani 1 1 d . . .
H22 H 0.6812 0.4782 0.6865 0.098 Uiso 1 1 calc R . .
C23 C 0.5689(5) 0.3716(5) 0.6483(4) 0.0701(16) Uani 1 1 d . . .
H23 H 0.5196 0.4230 0.6303 0.084 Uiso 1 1 calc R . .
N1 N 0.2639(3) -0.1497(3) 0.5227(2) 0.0471(10) Uani 1 1 d . . .
N2 N 0.2885(3) 0.1487(4) 0.6401(3) 0.0588(12) Uani 1 1 d . . .
N3 N 0.4556(3) -0.0377(4) 0.6977(2) 0.0532(11) Uani 1 1 d . . .
N4 N 0.5436(3) 0.2672(3) 0.6410(2) 0.0535(11) Uani 1 1 d . . .
N5 N 0.2688(5) 0.3988(5) 0.5186(4) 0.0830(17) Uani 1 1 d . . .
N97 N 0.5502(5) -0.3405(6) 0.6809(4) 0.111(2) Uani 1 1 d . . .
N98 N 0.5344(3) -0.2860(4) 0.6225(3) 0.0602(12) Uani 1 1 d . . .
N99 N 0.5176(3) -0.2302(4) 0.5630(3) 0.0569(11) Uani 1 1 d . . .
O1 O 0.3078(2) 0.0587(2) 0.49455(18) 0.0393(7) Uani 1 1 d . . .
O2 O 0.1374(2) 0.1059(3) 0.4779(2) 0.0569(9) Uani 1 1 d . . .
O3 O 0.5212(2) 0.0686(2) 0.57369(17) 0.0340(7) Uani 1 1 d . . .
O4 O 0.6685(2) 0.0109(3) 0.65970(19) 0.0503(9) Uani 1 1 d . . .
H4A H 0.6741 -0.0122 0.6133 0.076 Uiso 1 1 calc R . .
O5 O 0.3350(5) 0.3842(5) 0.5795(4) 0.1200(19) Uani 1 1 d . . .
O6 O 0.2676(5) 0.3293(5) 0.4652(4) 0.128(2) Uani 1 1 d . . .
O7 O 0.2131(6) 0.4715(6) 0.5107(4) 0.173(3) Uani 1 1 d . . .
Cd1 Cd 0.42325(2) -0.07830(3) 0.55349(2) 0.03811(12) Uani 1 1 d . . .
Cd2 Cd 0.39638(3) 0.20845(3) 0.54745(2) 0.04532(13) 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
C1 N1 1.332(7) . ?
C1 C2 1.364(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.363(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.363(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.343(6) . ?
C5 C6 1.538(7) . ?
C6 O1 1.358(5) . ?
C6 O2 1.425(5) . ?
C6 C7 1.560(7) . ?
C7 N2 1.316(7) . ?
C7 C8 1.376(7) . ?
C8 C9 1.362(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.356(11) . ?
C9 H9 0.9300 . ?
C10 C11 1.368(10) . ?
C10 H10 0.9300 . ?
C11 N2 1.355(7) . ?
C11 H11 0.9300 . ?
C12 O2 1.393(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N3 1.351(7) . ?
C13 C14 1.370(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.347(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.367(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.399(7) . ?
C16 H16 0.9300 . ?
C17 N3 1.326(7) . ?
C17 C18 1.540(7) . ?
C18 O3 1.382(5) . ?
C18 O4 1.406(5) . ?
C18 C19 1.535(7) . ?
C19 N4 1.330(6) . ?
C19 C20 1.375(7) . ?
C20 C21 1.371(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.359(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.380(9) . ?
C22 H22 0.9300 . ?
C23 N4 1.344(7) . ?
C23 H23 0.9300 . ?
N1 Cd1 2.293(4) . ?
N2 Cd2 2.385(4) . ?
N3 Cd1 2.347(4) . ?
N4 Cd2 2.381(4) . ?
N5 O7 1.167(7) . ?
N5 O5 1.216(7) . ?
N5 O6 1.220(7) . ?
N97 N98 1.151(7) . ?
N98 N99 1.174(6) . ?
N99 Cd1 2.268(4) . ?
N99 Cd2 2.313(4) 3_656 ?
O1 Cd2 2.293(3) . ?
O1 Cd1 2.386(3) . ?
O3 Cd1 2.243(3) . ?
O3 Cd1 2.314(3) 3_656 ?
O3 Cd2 2.404(3) . ?
O4 H4A 0.8200 . ?
O5 Cd2 2.427(5) . ?
O6 Cd2 2.491(6) . ?
Cd1 O3 2.314(3) 3_656 ?
Cd2 N99 2.313(4) 3_656 ?

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 C1 C2 122.8(5) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 117.8(6) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C4 120.0(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 119.8(6) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 120.5(5) . . ?
N1 C5 C6 115.7(4) . . ?
C4 C5 C6 123.8(5) . . ?
O1 C6 O2 114.1(4) . . ?
O1 C6 C5 110.3(4) . . ?
O2 C6 C5 109.0(4) . . ?
O1 C6 C7 111.0(4) . . ?
O2 C6 C7 101.6(3) . . ?
C5 C6 C7 110.5(4) . . ?
N2 C7 C8 122.2(6) . . ?
N2 C7 C6 114.6(4) . . ?
C8 C7 C6 123.2(6) . . ?
C9 C8 C7 119.0(7) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C10 C9 C8 119.4(7) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 119.6(7) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
N2 C11 C10 121.2(8) . . ?
N2 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 122.7(7) . . ?
N3 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C15 C14 C13 118.3(6) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C14 C15 C16 120.7(6) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C17 118.6(7) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
N3 C17 C16 121.1(5) . . ?
N3 C17 C18 116.2(4) . . ?
C16 C17 C18 122.6(5) . . ?
O3 C18 O4 112.7(3) . . ?
O3 C18 C19 108.0(4) . . ?
O4 C18 C19 109.4(4) . . ?
O3 C18 C17 110.5(4) . . ?
O4 C18 C17 104.5(4) . . ?
C19 C18 C17 111.8(4) . . ?
N4 C19 C20 122.0(5) . . ?
N4 C19 C18 115.9(4) . . ?
C20 C19 C18 122.1(5) . . ?
C21 C20 C19 118.9(6) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
C22 C21 C20 120.0(6) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 118.2(6) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 H22 120.9 . . ?
N4 C23 C22 122.4(6) . . ?
N4 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C1 N1 C5 119.0(4) . . ?
C1 N1 Cd1 124.3(3) . . ?
C5 N1 Cd1 115.9(3) . . ?
C7 N2 C11 118.7(5) . . ?
C7 N2 Cd2 117.7(3) . . ?
C11 N2 Cd2 123.5(5) . . ?
C17 N3 C13 118.6(5) . . ?
C17 N3 Cd1 115.2(3) . . ?
C13 N3 Cd1 126.2(4) . . ?
C19 N4 C23 118.4(5) . . ?
C19 N4 Cd2 117.1(3) . . ?
C23 N4 Cd2 121.5(4) . . ?
O7 N5 O5 124.6(8) . . ?
O7 N5 O6 123.0(8) . . ?
O5 N5 O6 112.4(6) . . ?
N97 N98 N99 179.5(6) . . ?
N98 N99 Cd1 124.8(4) . . ?
N98 N99 Cd2 130.7(4) . 3_656 ?
Cd1 N99 Cd2 101.69(17) . 3_656 ?
C6 O1 Cd2 117.3(3) . . ?
C6 O1 Cd1 108.2(3) . . ?
Cd2 O1 Cd1 100.04(11) . . ?
C12 O2 C6 115.0(4) . . ?
C18 O3 Cd1 115.3(3) . . ?
C18 O3 Cd1 125.1(3) . 3_656 ?
Cd1 O3 Cd1 100.91(10) . 3_656 ?
C18 O3 Cd2 113.1(2) . . ?
Cd1 O3 Cd2 100.95(10) . . ?
Cd1 O3 Cd2 97.66(10) 3_656 . ?
C18 O4 H4A 109.5 . . ?
N5 O5 Cd2 101.0(4) . . ?
N5 O6 Cd2 97.5(4) . . ?
O3 Cd1 N99 111.23(14) . . ?
O3 Cd1 N1 148.25(12) . . ?
N99 Cd1 N1 100.49(16) . . ?
O3 Cd1 O3 79.09(10) . 3_656 ?
N99 Cd1 O3 80.61(13) . 3_656 ?
N1 Cd1 O3 105.49(12) . 3_656 ?
O3 Cd1 N3 71.43(13) . . ?
N99 Cd1 N3 96.38(15) . . ?
N1 Cd1 N3 107.31(14) . . ?
O3 Cd1 N3 147.05(13) 3_656 . ?
O3 Cd1 O1 78.44(10) . . ?
N99 Cd1 O1 159.91(14) . . ?
N1 Cd1 O1 70.96(12) . . ?
O3 Cd1 O1 84.24(9) 3_656 . ?
N3 Cd1 O1 103.49(12) . . ?
O1 Cd2 N99 96.14(13) . 3_656 ?
O1 Cd2 N4 143.48(13) . . ?
N99 Cd2 N4 88.75(15) 3_656 . ?
O1 Cd2 N2 69.26(14) . . ?
N99 Cd2 N2 165.39(16) 3_656 . ?
N4 Cd2 N2 103.22(15) . . ?
O1 Cd2 O3 77.13(10) . . ?
N99 Cd2 O3 77.82(12) 3_656 . ?
N4 Cd2 O3 68.57(12) . . ?
N2 Cd2 O3 98.57(12) . . ?
O1 Cd2 O5 129.64(17) . . ?
N99 Cd2 O5 107.24(19) 3_656 . ?
N4 Cd2 O5 82.20(18) . . ?
N2 Cd2 O5 82.98(19) . . ?
O3 Cd2 O5 150.36(17) . . ?
O1 Cd2 O6 91.52(18) . . ?
N99 Cd2 O6 85.14(18) 3_656 . ?
N4 Cd2 O6 125.0(2) . . ?
N2 Cd2 O6 94.52(18) . . ?
O3 Cd2 O6 158.25(17) . . ?
O5 Cd2 O6 48.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.096
####################################################################### 
# 
# 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_cd136f
_database_code_depnum_ccdc_archive 'CCDC 1446473'
_audit_update_record             
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H40 Cd4 N12 O16'
_chemical_formula_weight         1490.52

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   13.3914(6)
_cell_length_b                   12.5725(5)
_cell_length_c                   16.1350(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.274(4)
_cell_angle_gamma                90.00
_cell_volume                     2664.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293.0(2)
_cell_measurement_reflns_used    4342
_cell_measurement_theta_min      3.9110
_cell_measurement_theta_max      28.5690

_exptl_crystal_description       'triangle plate'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;CrysAlis RED, (2005)
;
_exptl_absorpt_correction_T_min  0.55234
_exptl_absorpt_correction_T_max  1.00000

_exptl_special_details           
; 
 ? 
;


_diffrn_ambient_temperature      293.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11503
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4731
_reflns_number_gt                3685
_reflns_threshold_expression     >2sigma(I)

#========================================================================== 
#
# REFINEMENT DATA

_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0994P)²+0.0696P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4731
_refine_ls_number_parameters     363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1677
_refine_ls_wR_factor_gt          0.1523
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2537(6) 0.2442(7) 0.4890(5) 0.0632(19) Uani 1 1 d . . .
H1 H 0.2003 0.1958 0.4771 0.076 Uiso 1 1 calc R . .
C2 C 0.3505(7) 0.2080(7) 0.5191(7) 0.085(3) Uani 1 1 d . . .
H2 H 0.3624 0.1357 0.5285 0.102 Uiso 1 1 calc R . .
C3 C 0.4298(7) 0.2793(8) 0.5354(7) 0.092(3) Uani 1 1 d . . .
H3 H 0.4962 0.2558 0.5540 0.111 Uiso 1 1 calc R . .
C4 C 0.4090(5) 0.3854(7) 0.5238(6) 0.079(3) Uani 1 1 d . . .
H4 H 0.4615 0.4347 0.5366 0.095 Uiso 1 1 calc R . .
C5 C 0.3117(5) 0.4197(5) 0.4936(5) 0.0512(16) Uani 1 1 d . . .
C6 C 0.2818(4) 0.5366(6) 0.4800(4) 0.0482(15) Uani 1 1 d . . .
C7 C 0.2767(5) 0.5718(5) 0.3882(5) 0.0587(19) Uani 1 1 d . . .
C8 C 0.3416(6) 0.5277(8) 0.3378(6) 0.076(2) Uani 1 1 d . . .
H8 H 0.3885 0.4746 0.3579 0.091 Uiso 1 1 calc R . .
C9 C 0.3310(9) 0.5684(9) 0.2559(7) 0.099(4) Uani 1 1 d . . .
H9 H 0.3711 0.5420 0.2197 0.119 Uiso 1 1 calc R . .
C10 C 0.2619(10) 0.6468(11) 0.2293(7) 0.106(3) Uani 1 1 d . . .
H10 H 0.2555 0.6744 0.1751 0.127 Uiso 1 1 calc R . .
C11 C 0.2032(8) 0.6841(7) 0.2810(6) 0.086(3) Uani 1 1 d . . .
H11 H 0.1564 0.7374 0.2612 0.103 Uiso 1 1 calc R . .
C12 C 0.3694(6) 0.6136(8) 0.6113(6) 0.080(2) Uani 1 1 d . . .
H12A H 0.3129 0.6556 0.6208 0.121 Uiso 1 1 calc R . .
H12B H 0.4319 0.6483 0.6362 0.121 Uiso 1 1 calc R . .
H12C H 0.3668 0.5448 0.6366 0.121 Uiso 1 1 calc R . .
C13 C 0.0890(6) 0.4236(7) 0.2424(6) 0.074(2) Uani 1 1 d . . .
H13 H 0.1391 0.3725 0.2589 0.089 Uiso 1 1 calc R . .
C14 C 0.0668(8) 0.4552(9) 0.1584(6) 0.092(3) Uani 1 1 d . . .
H14 H 0.1011 0.4261 0.1190 0.111 Uiso 1 1 calc R . .
C15 C -0.0055(9) 0.5288(9) 0.1362(6) 0.094(3) Uani 1 1 d . . .
H15 H -0.0216 0.5513 0.0803 0.113 Uiso 1 1 calc R . .
C16 C -0.0566(7) 0.5721(6) 0.1947(5) 0.075(2) Uani 1 1 d . . .
H16 H -0.1074 0.6227 0.1786 0.090 Uiso 1 1 calc R . .
C17 C -0.0304(5) 0.5382(6) 0.2783(4) 0.0508(15) Uani 1 1 d . . .
C18 C -0.0851(5) 0.5770(5) 0.3476(4) 0.0478(16) Uani 1 1 d . . .
C19 C -0.1185(5) 0.6936(5) 0.3343(4) 0.0533(16) Uani 1 1 d . . .
C20 C -0.2174(5) 0.7225(6) 0.2997(5) 0.0630(19) Uani 1 1 d . . .
H20 H -0.2664 0.6708 0.2814 0.076 Uiso 1 1 calc R . .
C21 C -0.2421(7) 0.8285(7) 0.2926(6) 0.079(2) Uani 1 1 d . . .
H21 H -0.3084 0.8494 0.2695 0.095 Uiso 1 1 calc R . .
C22 C -0.1692(7) 0.9028(7) 0.3196(6) 0.077(2) Uani 1 1 d . . .
H22 H -0.1847 0.9749 0.3159 0.092 Uiso 1 1 calc R . .
C23 C -0.0716(6) 0.8684(6) 0.3526(5) 0.073(2) Uani 1 1 d . . .
H23 H -0.0212 0.9191 0.3700 0.087 Uiso 1 1 calc R . .
C99 C -0.0345(6) 0.2089(6) 0.3808(6) 0.067(2) Uani 1 1 d . . .
N1 N 0.2346(4) 0.3495(4) 0.4763(4) 0.0531(13) Uani 1 1 d . . .
N2 N 0.2086(4) 0.6483(5) 0.3602(4) 0.0615(15) Uani 1 1 d . . .
N3 N 0.0406(4) 0.4641(5) 0.3007(4) 0.0595(15) Uani 1 1 d . . .
N4 N -0.0464(5) 0.7658(5) 0.3607(4) 0.0630(16) Uani 1 1 d . . .
N5 N 0.2305(7) 0.8977(8) 0.4782(6) 0.095(3) Uani 1 1 d . . .
N99 N -0.0233(5) 0.2712(5) 0.4323(4) 0.0608(15) Uani 1 1 d . . .
O1 O 0.1926(3) 0.5561(3) 0.5057(3) 0.0471(10) Uani 1 1 d . . .
O2 O 0.3645(3) 0.6017(4) 0.5225(3) 0.0605(12) Uani 1 1 d . . .
O3 O -0.0221(3) 0.5680(3) 0.4255(3) 0.0430(10) Uani 1 1 d . . .
O4 O -0.1719(3) 0.5120(4) 0.3394(3) 0.0549(11) Uani 1 1 d . . .
H4A H -0.1746 0.4854 0.3853 0.082 Uiso 1 1 calc R . .
O5 O 0.1602(7) 0.8807(6) 0.4192(6) 0.136(3) Uani 1 1 d . . .
O6 O 0.2365(7) 0.8258(7) 0.5318(7) 0.139(3) Uani 1 1 d . . .
O7 O 0.2844(8) 0.9722(8) 0.4850(7) 0.171(5) Uani 1 1 d . . .
O99 O -0.0459(6) 0.1438(7) 0.3254(6) 0.132(3) Uani 1 1 d . . .
Cd1 Cd 0.07387(3) 0.42078(3) 0.44543(3) 0.0446(2) Uani 1 1 d . . .
Cd2 Cd 0.10364(4) 0.70580(4) 0.45353(3) 0.0510(2) 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
C1 N1 1.357(10) . ?
C1 C2 1.369(11) . ?
C1 H1 0.9300 . ?
C2 C3 1.375(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.368(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(10) . ?
C4 H4 0.9300 . ?
C5 N1 1.345(8) . ?
C5 C6 1.529(9) . ?
C6 O1 1.360(8) . ?
C6 O2 1.438(8) . ?
C6 C7 1.534(11) . ?
C7 N2 1.342(9) . ?
C7 C8 1.415(10) . ?
C8 C9 1.397(14) . ?
C8 H8 0.9300 . ?
C9 C10 1.363(15) . ?
C9 H9 0.9300 . ?
C10 C11 1.338(14) . ?
C10 H10 0.9300 . ?
C11 N2 1.344(10) . ?
C11 H11 0.9300 . ?
C12 O2 1.429(10) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N3 1.342(10) . ?
C13 C14 1.387(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.337(14) . ?
C14 H14 0.9300 . ?
C15 C16 1.382(13) . ?
C15 H15 0.9300 . ?
C16 C17 1.393(10) . ?
C16 H16 0.9300 . ?
C17 N3 1.330(9) . ?
C17 C18 1.532(10) . ?
C18 O3 1.375(7) . ?
C18 O4 1.406(7) . ?
C18 C19 1.536(9) . ?
C19 N4 1.333(9) . ?
C19 C20 1.381(10) . ?
C20 C21 1.373(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.360(12) . ?
C21 H21 0.9300 . ?
C22 C23 1.381(11) . ?
C22 H22 0.9300 . ?
C23 N4 1.333(10) . ?
C23 H23 0.9300 . ?
C99 N99 1.130(9) . ?
C99 O99 1.199(10) . ?
N1 Cd1 2.295(5) . ?
N2 Cd2 2.364(6) . ?
N3 Cd1 2.355(6) . ?
N4 Cd2 2.382(6) . ?
N5 O7 1.174(10) . ?
N5 O5 1.220(11) . ?
N5 O6 1.242(12) . ?
N99 Cd1 2.274(6) . ?
N99 Cd2 2.326(6) 3_566 ?
O1 Cd2 2.297(4) . ?
O1 Cd1 2.401(4) . ?
O3 Cd1 2.240(4) . ?
O3 Cd1 2.324(4) 3_566 ?
O3 Cd2 2.397(4) . ?
O4 H4A 0.8200 . ?
O5 Cd2 2.425(8) . ?
O6 Cd2 2.482(9) . ?
Cd1 O3 2.324(4) 3_566 ?
Cd2 N99 2.326(6) 3_566 ?

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 C1 C2 121.0(7) . . ?
N1 C1 H1 119.5 . . ?
C2 C1 H1 119.5 . . ?
C1 C2 C3 119.5(8) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 118.7(8) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 120.6(8) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
N1 C5 C4 120.4(6) . . ?
N1 C5 C6 115.6(5) . . ?
C4 C5 C6 124.0(6) . . ?
O1 C6 O2 113.1(5) . . ?
O1 C6 C5 110.6(5) . . ?
O2 C6 C5 108.8(5) . . ?
O1 C6 C7 111.5(5) . . ?
O2 C6 C7 100.4(5) . . ?
C5 C6 C7 112.0(6) . . ?
N2 C7 C8 122.7(8) . . ?
N2 C7 C6 115.5(6) . . ?
C8 C7 C6 121.8(7) . . ?
C9 C8 C7 116.1(9) . . ?
C9 C8 H8 121.9 . . ?
C7 C8 H8 121.9 . . ?
C10 C9 C8 120.0(9) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 120.2(10) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 N2 123.2(10) . . ?
C10 C11 H11 118.4 . . ?
N2 C11 H11 118.4 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 122.4(9) . . ?
N3 C13 H13 118.8 . . ?
C14 C13 H13 118.8 . . ?
C15 C14 C13 117.8(9) . . ?
C15 C14 H14 121.1 . . ?
C13 C14 H14 121.1 . . ?
C14 C15 C16 121.3(9) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C15 C16 C17 118.4(9) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N3 C17 C16 120.6(7) . . ?
N3 C17 C18 116.3(6) . . ?
C16 C17 C18 122.9(7) . . ?
O3 C18 O4 112.7(5) . . ?
O3 C18 C17 110.3(5) . . ?
O4 C18 C17 104.5(5) . . ?
O3 C18 C19 108.5(5) . . ?
O4 C18 C19 109.2(5) . . ?
C17 C18 C19 111.7(5) . . ?
N4 C19 C20 121.9(6) . . ?
N4 C19 C18 115.6(6) . . ?
C20 C19 C18 122.5(6) . . ?
C21 C20 C19 119.0(7) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
C22 C21 C20 119.6(8) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C23 118.4(7) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
N4 C23 C22 122.9(8) . . ?
N4 C23 H23 118.6 . . ?
C22 C23 H23 118.6 . . ?
N99 C99 O99 179.1(11) . . ?
C5 N1 C1 119.6(6) . . ?
C5 N1 Cd1 116.0(4) . . ?
C1 N1 Cd1 123.7(5) . . ?
C7 N2 C11 117.8(7) . . ?
C7 N2 Cd2 117.0(5) . . ?
C11 N2 Cd2 125.1(6) . . ?
C17 N3 C13 119.5(7) . . ?
C17 N3 Cd1 114.7(4) . . ?
C13 N3 Cd1 125.7(6) . . ?
C19 N4 C23 118.3(6) . . ?
C19 N4 Cd2 117.0(4) . . ?
C23 N4 Cd2 122.3(5) . . ?
O7 N5 O5 125.4(12) . . ?
O7 N5 O6 124.1(11) . . ?
O5 N5 O6 110.5(9) . . ?
C99 N99 Cd1 129.2(6) . . ?
C99 N99 Cd2 130.8(6) . 3_566 ?
Cd1 N99 Cd2 99.7(2) . 3_566 ?
C6 O1 Cd2 117.4(4) . . ?
C6 O1 Cd1 107.5(4) . . ?
Cd2 O1 Cd1 100.21(16) . . ?
C12 O2 C6 114.7(5) . . ?
C18 O3 Cd1 115.6(4) . . ?
C18 O3 Cd1 125.3(4) . 3_566 ?
Cd1 O3 Cd1 100.67(16) . 3_566 ?
C18 O3 Cd2 113.3(3) . . ?
Cd1 O3 Cd2 101.99(16) . . ?
Cd1 O3 Cd2 96.23(15) 3_566 . ?
C18 O4 H4A 109.5 . . ?
N5 O5 Cd2 102.0(7) . . ?
N5 O6 Cd2 98.4(7) . . ?
O3 Cd1 N99 111.59(19) . . ?
O3 Cd1 N1 147.28(18) . . ?
N99 Cd1 N1 101.1(2) . . ?
O3 Cd1 O3 79.33(16) . 3_566 ?
N99 Cd1 O3 82.45(19) . 3_566 ?
N1 Cd1 O3 105.10(18) . 3_566 ?
O3 Cd1 N3 71.02(19) . . ?
N99 Cd1 N3 96.0(2) . . ?
N1 Cd1 N3 107.0(2) . . ?
O3 Cd1 N3 147.48(18) 3_566 . ?
O3 Cd1 O1 77.81(14) . . ?
N99 Cd1 O1 161.1(2) . . ?
N1 Cd1 O1 70.71(17) . . ?
O3 Cd1 O1 83.34(14) 3_566 . ?
N3 Cd1 O1 102.67(18) . . ?
O1 Cd2 N99 95.68(19) . 3_566 ?
O1 Cd2 N2 69.67(18) . . ?
N99 Cd2 N2 165.2(2) 3_566 . ?
O1 Cd2 N4 143.43(18) . . ?
N99 Cd2 N4 89.7(2) 3_566 . ?
N2 Cd2 N4 103.3(2) . . ?
O1 Cd2 O3 76.80(14) . . ?
N99 Cd2 O3 79.79(19) 3_566 . ?
N2 Cd2 O3 98.17(18) . . ?
N4 Cd2 O3 68.61(17) . . ?
O1 Cd2 O5 131.6(2) . . ?
N99 Cd2 O5 106.3(3) 3_566 . ?
N2 Cd2 O5 83.2(3) . . ?
N4 Cd2 O5 80.3(3) . . ?
O3 Cd2 O5 148.4(2) . . ?
O1 Cd2 O6 92.5(3) . . ?
N99 Cd2 O6 85.3(3) 3_566 . ?
N2 Cd2 O6 93.1(3) . . ?
N4 Cd2 O6 124.1(3) . . ?
O3 Cd2 O6 160.5(3) . . ?
O5 Cd2 O6 48.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.546
_refine_diff_density_min         -1.565
_refine_diff_density_rms         0.149
####################################################################### 
# 
# 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_cd134
_database_code_depnum_ccdc_archive 'CCDC 1446474'
_audit_update_record             
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H40 Cd4 N12 O16'
_chemical_formula_sum            'C48 H40 Cd4 N12 O16'
_chemical_formula_weight         1490.52

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   12.5084(5)
_cell_length_b                   19.1468(9)
_cell_length_c                   22.4328(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5372.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295.0
_cell_measurement_reflns_used    5258
_cell_measurement_theta_min      3.8040
_cell_measurement_theta_max      28.6310

_exptl_crystal_description       plate
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2928
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;CrysAlis RED, (2005)
;
_exptl_absorpt_correction_T_min  0.55865
_exptl_absorpt_correction_T_max  1.00000

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295.0
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17425
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4775
_reflns_number_gt                2978
_reflns_threshold_expression     >2sigma(I)

#========================================================================== 
#
# REFINEMENT DATA

_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0197P)²+21.8358P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4775
_refine_ls_number_parameters     363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.57165(4) 0.49383(3) 0.43342(2) 0.02709(15) Uani 1 1 d . . .
Cd2 Cd 0.71715(4) 0.49091(3) 0.56832(2) 0.03310(16) Uani 1 1 d . . .
O1 O 0.5691(4) 0.4278(2) 0.59403(19) 0.0291(11) Uani 1 1 d . . .
N1 N 0.6348(5) 0.5686(3) 0.3627(3) 0.0338(15) Uani 1 1 d . . .
O3 O 0.4281(3) 0.4453(2) 0.47834(19) 0.0222(10) Uani 1 1 d . . .
C5 C 0.5614(6) 0.6063(4) 0.3342(3) 0.0357(19) Uani 1 1 d . . .
N4 N 0.7727(5) 0.6035(3) 0.5404(3) 0.0384(16) Uani 1 1 d . . .
N3 N 0.5244(5) 0.3903(3) 0.3834(3) 0.0353(15) Uani 1 1 d . . .
C8 C 0.5521(8) 0.4867(5) 0.7490(4) 0.058(3) Uani 1 1 d . . .
H8 H 0.5012 0.4567 0.7651 0.069 Uiso 1 1 calc R . .
C18 C 0.4180(6) 0.3733(3) 0.4736(3) 0.0263(16) Uani 1 1 d . . .
N2 N 0.6689(5) 0.5152(3) 0.6688(3) 0.0445(17) Uani 1 1 d . . .
C19 C 0.7003(6) 0.6474(4) 0.5166(3) 0.0316(17) Uani 1 1 d . . .
N5 N 0.9129(7) 0.4262(4) 0.6114(4) 0.058(2) Uani 1 1 d . . .
O4 O 0.4821(4) 0.3376(2) 0.5149(2) 0.0374(13) Uani 1 1 d . . .
H4 H 0.5062 0.3654 0.5392 0.056 Uiso 1 1 calc R . .
N99 N 0.7262(5) 0.4495(3) 0.4711(3) 0.0380(16) Uani 1 1 d . . .
O2 O 0.3756(4) 0.6431(3) 0.3268(2) 0.0430(13) Uani 1 1 d . . .
C99 C 0.7860(7) 0.4118(5) 0.4474(4) 0.054(2) Uani 1 1 d . . .
C20 C 0.7288(7) 0.7062(4) 0.4853(4) 0.044(2) Uani 1 1 d . . .
H20 H 0.6764 0.7347 0.4687 0.053 Uiso 1 1 calc R . .
C17 C 0.4565(6) 0.3486(4) 0.4122(3) 0.0336(18) Uani 1 1 d . . .
C23 C 0.8762(7) 0.6216(4) 0.5331(4) 0.054(2) Uani 1 1 d . . .
H23 H 0.9279 0.5925 0.5496 0.064 Uiso 1 1 calc R . .
C21 C 0.8349(7) 0.7225(5) 0.4786(4) 0.059(3) Uani 1 1 d . . .
H21 H 0.8549 0.7623 0.4577 0.071 Uiso 1 1 calc R . .
C6 C 0.4421(5) 0.5868(4) 0.3470(3) 0.0304(17) Uani 1 1 d . . .
C13 C 0.5663(7) 0.3687(4) 0.3320(4) 0.048(2) Uani 1 1 d . . .
H13 H 0.6126 0.3983 0.3117 0.057 Uiso 1 1 calc R . .
C7 C 0.5911(6) 0.4758(4) 0.6927(3) 0.0354(19) Uani 1 1 d . . .
C4 C 0.7372(6) 0.5834(4) 0.3544(4) 0.043(2) Uani 1 1 d . . .
H4A H 0.7879 0.5578 0.3754 0.051 Uiso 1 1 calc R . .
O5 O 0.8967(6) 0.4892(4) 0.6102(4) 0.098(3) Uani 1 1 d . . .
O99 O 0.8449(7) 0.3723(4) 0.4234(4) 0.111(3) Uani 1 1 d . . .
O7 O 0.9954(6) 0.4004(4) 0.6303(3) 0.093(3) Uani 1 1 d . . .
C1 C 0.7723(7) 0.6348(5) 0.3164(4) 0.061(3) Uani 1 1 d . . .
H1 H 0.8447 0.6439 0.3111 0.074 Uiso 1 1 calc R . .
C15 C 0.4753(8) 0.2622(4) 0.3375(4) 0.060(3) Uani 1 1 d . . .
H15 H 0.4585 0.2186 0.3218 0.072 Uiso 1 1 calc R . .
C12 C 0.7047(8) 0.5686(5) 0.7013(4) 0.060(3) Uani 1 1 d . . .
H12 H 0.7581 0.5966 0.6852 0.072 Uiso 1 1 calc R . .
C16 C 0.4311(7) 0.2836(4) 0.3904(4) 0.047(2) Uani 1 1 d . . .
H16 H 0.3847 0.2546 0.4112 0.056 Uiso 1 1 calc R . .
C22 C 0.9108(7) 0.6800(5) 0.5029(4) 0.063(3) Uani 1 1 d . . .
H22 H 0.9832 0.6901 0.4992 0.076 Uiso 1 1 calc R . .
C14 C 0.5887(7) 0.6580(5) 0.2952(4) 0.066(3) Uani 1 1 d . . .
H14 H 0.5366 0.6832 0.2750 0.079 Uiso 1 1 calc R . .
O6 O 0.8399(6) 0.3910(4) 0.5897(3) 0.095(2) Uani 1 1 d . . .
C2 C 0.3703(8) 0.7010(4) 0.3663(4) 0.059(3) Uani 1 1 d . . .
H2A H 0.3283 0.7374 0.3485 0.089 Uiso 1 1 calc R . .
H2B H 0.4412 0.7180 0.3740 0.089 Uiso 1 1 calc R . .
H2C H 0.3379 0.6867 0.4031 0.089 Uiso 1 1 calc R . .
C3 C 0.5438(8) 0.3051(5) 0.3081(4) 0.063(3) Uani 1 1 d . . .
H3 H 0.5748 0.2912 0.2723 0.076 Uiso 1 1 calc R . .
C1A C 0.6678(8) 0.5846(6) 0.7569(4) 0.068(3) Uani 1 1 d . . .
H1A H 0.6946 0.6227 0.7777 0.082 Uiso 1 1 calc R . .
C1D C 0.5894(9) 0.5426(6) 0.7813(4) 0.069(3) Uani 1 1 d . . .
H1D H 0.5623 0.5521 0.8191 0.083 Uiso 1 1 calc R . .
C1F C 0.6961(9) 0.6716(6) 0.2868(5) 0.084(4) Uani 1 1 d . . .
H1F H 0.7166 0.7066 0.2604 0.100 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O3 2.259(4) . ?
Cd1 N99 2.274(6) . ?
Cd1 N1 2.278(6) . ?
Cd1 O3 2.297(4) 5_666 ?
Cd1 N3 2.354(6) . ?
Cd1 O1 2.394(4) 5_666 ?
Cd2 O1 2.286(4) . ?
Cd2 N99 2.324(6) . ?
Cd2 N4 2.349(6) . ?
Cd2 N2 2.380(6) . ?
Cd2 O3 2.426(4) 5_666 ?
Cd2 O5 2.435(8) . ?
Cd2 O6 2.500(7) . ?
O1 C6 1.359(8) 5_666 ?
O1 Cd1 2.394(4) 5_666 ?
N1 C4 1.325(9) . ?
N1 C5 1.331(9) . ?
O3 C18 1.389(7) . ?
O3 Cd1 2.297(4) 5_666 ?
O3 Cd2 2.426(4) 5_666 ?
C5 C14 1.364(11) . ?
C5 C6 1.565(10) . ?
N4 C19 1.346(9) . ?
N4 C23 1.350(10) . ?
N3 C13 1.332(9) . ?
N3 C17 1.332(9) . ?
C8 C7 1.369(10) . ?
C8 C1D 1.376(12) . ?
C8 H8 0.9300 . ?
C18 O4 1.402(7) . ?
C18 C17 1.535(10) . ?
C18 C19 1.548(9) 5_666 ?
N2 C12 1.334(10) . ?
N2 C7 1.343(9) . ?
C19 C20 1.374(10) . ?
C19 C18 1.548(9) 5_666 ?
N5 O7 1.220(9) . ?
N5 O5 1.224(9) . ?
N5 O6 1.236(9) . ?
O4 H4 0.8200 . ?
N99 C99 1.168(10) . ?
O2 C2 1.421(9) . ?
O2 C6 1.435(8) . ?
C99 O99 1.186(10) . ?
C20 C21 1.372(11) . ?
C20 H20 0.9300 . ?
C17 C16 1.374(9) . ?
C23 C22 1.378(11) . ?
C23 H23 0.9300 . ?
C21 C22 1.364(12) . ?
C21 H21 0.9300 . ?
C6 O1 1.359(8) 5_666 ?
C6 C7 1.550(10) 5_666 ?
C13 C3 1.360(11) . ?
C13 H13 0.9300 . ?
C7 C6 1.550(10) 5_666 ?
C4 C1 1.374(11) . ?
C4 H4A 0.9300 . ?
C1 C1F 1.359(12) . ?
C1 H1 0.9300 . ?
C15 C3 1.357(12) . ?
C15 C16 1.372(11) . ?
C15 H15 0.9300 . ?
C12 C1A 1.364(12) . ?
C12 H12 0.9300 . ?
C16 H16 0.9300 . ?
C22 H22 0.9300 . ?
C14 C1F 1.382(12) . ?
C14 H14 0.9300 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3 0.9300 . ?
C1A C1D 1.380(13) . ?
C1A H1A 0.9300 . ?
C1D H1D 0.9300 . ?
C1F H1F 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
O3 Cd1 N99 110.88(19) . . ?
O3 Cd1 N1 147.65(19) . . ?
N99 Cd1 N1 101.4(2) . . ?
O3 Cd1 O3 79.96(16) . 5_666 ?
N99 Cd1 O3 82.41(19) . 5_666 ?
N1 Cd1 O3 106.29(18) . 5_666 ?
O3 Cd1 N3 70.52(19) . . ?
N99 Cd1 N3 94.4(2) . . ?
N1 Cd1 N3 106.5(2) . . ?
O3 Cd1 N3 147.00(18) 5_666 . ?
O3 Cd1 O1 77.76(15) . 5_666 ?
N99 Cd1 O1 162.70(19) . 5_666 ?
N1 Cd1 O1 71.46(18) . 5_666 ?
O3 Cd1 O1 84.53(15) 5_666 5_666 ?
N3 Cd1 O1 102.75(18) . 5_666 ?
O1 Cd2 N99 95.50(19) . . ?
O1 Cd2 N4 142.39(19) . . ?
N99 Cd2 N4 92.8(2) . . ?
O1 Cd2 N2 70.04(19) . . ?
N99 Cd2 N2 165.5(2) . . ?
N4 Cd2 N2 98.5(2) . . ?
O1 Cd2 O3 76.62(15) . 5_666 ?
N99 Cd2 O3 78.66(18) . 5_666 ?
N4 Cd2 O3 69.19(18) . 5_666 ?
N2 Cd2 O3 96.93(18) . 5_666 ?
O1 Cd2 O5 130.0(2) . . ?
N99 Cd2 O5 108.2(3) . . ?
N4 Cd2 O5 80.9(2) . . ?
N2 Cd2 O5 82.6(3) . . ?
O3 Cd2 O5 149.7(2) 5_666 . ?
O1 Cd2 O6 92.5(2) . . ?
N99 Cd2 O6 83.6(2) . . ?
N4 Cd2 O6 124.9(3) . . ?
N2 Cd2 O6 97.1(2) . . ?
O3 Cd2 O6 158.1(2) 5_666 . ?
O5 Cd2 O6 49.4(2) . . ?
C6 O1 Cd2 115.9(4) 5_666 . ?
C6 O1 Cd1 107.7(4) 5_666 5_666 ?
Cd2 O1 Cd1 101.50(16) . 5_666 ?
C4 N1 C5 118.9(6) . . ?
C4 N1 Cd1 124.6(5) . . ?
C5 N1 Cd1 115.8(5) . . ?
C18 O3 Cd1 116.5(4) . . ?
C18 O3 Cd1 124.7(4) . 5_666 ?
Cd1 O3 Cd1 100.04(16) . 5_666 ?
C18 O3 Cd2 113.5(4) . 5_666 ?
Cd1 O3 Cd2 101.28(16) . 5_666 ?
Cd1 O3 Cd2 96.74(15) 5_666 5_666 ?
N1 C5 C14 121.9(7) . . ?
N1 C5 C6 116.1(6) . . ?
C14 C5 C6 122.0(7) . . ?
C19 N4 C23 115.9(7) . . ?
C19 N4 Cd2 118.7(5) . . ?
C23 N4 Cd2 123.5(5) . . ?
C13 N3 C17 119.0(6) . . ?
C13 N3 Cd1 125.1(5) . . ?
C17 N3 Cd1 115.7(5) . . ?
C7 C8 C1D 118.9(9) . . ?
C7 C8 H8 120.5 . . ?
C1D C8 H8 120.5 . . ?
O3 C18 O4 112.5(5) . . ?
O3 C18 C17 110.2(5) . . ?
O4 C18 C17 105.3(5) . . ?
O3 C18 C19 109.2(5) . 5_666 ?
O4 C18 C19 109.2(6) . 5_666 ?
C17 C18 C19 110.4(6) . 5_666 ?
C12 N2 C7 117.1(7) . . ?
C12 N2 Cd2 125.6(6) . . ?
C7 N2 Cd2 116.9(5) . . ?
N4 C19 C20 122.7(7) . . ?
N4 C19 C18 115.3(6) . 5_666 ?
C20 C19 C18 121.9(7) . 5_666 ?
O7 N5 O5 123.1(9) . . ?
O7 N5 O6 122.7(8) . . ?
O5 N5 O6 114.1(8) . . ?
C18 O4 H4 109.5 . . ?
C99 N99 Cd1 127.3(6) . . ?
C99 N99 Cd2 132.1(6) . . ?
Cd1 N99 Cd2 100.4(2) . . ?
C2 O2 C6 114.6(6) . . ?
N99 C99 O99 178.4(11) . . ?
C21 C20 C19 119.5(8) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
N3 C17 C16 121.1(7) . . ?
N3 C17 C18 116.9(6) . . ?
C16 C17 C18 121.7(7) . . ?
N4 C23 C22 124.7(8) . . ?
N4 C23 H23 117.6 . . ?
C22 C23 H23 117.6 . . ?
C22 C21 C20 119.7(8) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
O1 C6 O2 113.8(6) 5_666 . ?
O1 C6 C7 112.0(6) 5_666 5_666 ?
O2 C6 C7 104.1(5) . 5_666 ?
O1 C6 C5 109.0(6) 5_666 . ?
O2 C6 C5 108.3(6) . . ?
C7 C6 C5 109.5(6) 5_666 . ?
N3 C13 C3 122.5(8) . . ?
N3 C13 H13 118.8 . . ?
C3 C13 H13 118.8 . . ?
N2 C7 C8 122.8(8) . . ?
N2 C7 C6 113.4(6) . 5_666 ?
C8 C7 C6 123.6(7) . 5_666 ?
N1 C4 C1 123.3(8) . . ?
N1 C4 H4A 118.3 . . ?
C1 C4 H4A 118.3 . . ?
N5 O5 Cd2 100.0(6) . . ?
C1F C1 C4 116.8(8) . . ?
C1F C1 H1 121.6 . . ?
C4 C1 H1 121.6 . . ?
C3 C15 C16 119.6(8) . . ?
C3 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
N2 C12 C1A 123.9(9) . . ?
N2 C12 H12 118.1 . . ?
C1A C12 H12 118.1 . . ?
C15 C16 C17 119.0(8) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C21 C22 C23 117.5(8) . . ?
C21 C22 H22 121.2 . . ?
C23 C22 H22 121.2 . . ?
C5 C14 C1F 117.9(8) . . ?
C5 C14 H14 121.0 . . ?
C1F C14 H14 121.0 . . ?
N5 O6 Cd2 96.4(6) . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C15 C3 C13 118.8(8) . . ?
C15 C3 H3 120.6 . . ?
C13 C3 H3 120.6 . . ?
C12 C1A C1D 118.2(9) . . ?
C12 C1A H1A 120.9 . . ?
C1D C1A H1A 120.9 . . ?
C8 C1D C1A 119.0(10) . . ?
C8 C1D H1D 120.5 . . ?
C1A C1D H1D 120.5 . . ?
C1 C1F C14 121.1(8) . . ?
C1 C1F H1F 119.5 . . ?
C14 C1F H1F 119.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.924
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.127
