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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex6
_database_code_depnum_ccdc_archive 'CCDC 1519712'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_publ_requested_journal_name     'Eur. J. Inorg. Chem.'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C44 H54 Cs N24 O13, 4(C7 H5 O3), 3(H3 O), 7(H2 O)'
_chemical_formula_sum            'C72 H97 Cs N24 O35'
_chemical_formula_weight         1991.65

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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   36.424(5)
_cell_length_b                   17.532(2)
_cell_length_c                   13.6510(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.591(4)
_cell_angle_gamma                90.00
_cell_volume                     8700.3(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4128
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9157
_exptl_absorpt_correction_T_max  0.9394
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36820
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.29
_diffrn_reflns_theta_max         25.10
_reflns_number_total             7706
_reflns_number_gt                5091
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.2000P)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     SHELXL
_refine_ls_extinction_coef       0.0019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7706
_refine_ls_number_parameters     560
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_gt           0.1238
_refine_ls_wR_factor_ref         0.4098
_refine_ls_wR_factor_gt          0.3970
_refine_ls_goodness_of_fit_ref   1.539
_refine_ls_restrained_S_all      1.539
_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
Cs1 Cs 0.74372(3) 0.30868(6) 0.81282(10) 0.0743(5) Uani 0.50 1 d P . .
O1W O 0.7532(8) 0.3116(11) 0.6635(11) 0.162(11) Uani 0.50 1 d P . .
C23 C 0.5754(3) 0.2675(6) 1.3766(7) 0.078(3) Uani 1 1 d . . .
C24 C 0.5383(3) 0.2750(7) 1.3640(8) 0.090(3) Uani 1 1 d . . .
H24 H 0.5232 0.2316 1.3565 0.108 Uiso 1 1 calc R . .
C25 C 0.5231(3) 0.3462(6) 1.3623(7) 0.077(3) Uani 1 1 d . . .
H25 H 0.4975 0.3511 1.3498 0.092 Uiso 1 1 calc R . .
C26 C 0.5439(2) 0.4106(6) 1.3784(6) 0.070(2) Uani 1 1 d . . .
C27 C 0.5823(3) 0.4012(6) 1.3927(7) 0.075(3) Uani 1 1 d . . .
H27 H 0.5977 0.4439 1.4022 0.091 Uiso 1 1 calc R . .
C28 C 0.5972(3) 0.3283(7) 1.3926(7) 0.078(3) Uani 1 1 d . . .
H28 H 0.6228 0.3217 1.4039 0.094 Uiso 1 1 calc R . .
C29 C 0.5270(3) 0.4861(7) 1.3760(7) 0.079(3) Uani 1 1 d . . .
C30 C 0.5719(3) 0.0976(8) 0.6413(7) 0.086(3) Uani 1 1 d . . .
C31 C 0.5346(3) 0.1058(8) 0.6439(9) 0.096(3) Uani 1 1 d . . .
H31 H 0.5196 0.0624 0.6479 0.115 Uiso 1 1 calc R . .
C32 C 0.5190(3) 0.1770(7) 0.6405(10) 0.097(3) Uani 1 1 d . . .
H32 H 0.4933 0.1810 0.6423 0.116 Uiso 1 1 calc R . .
C33 C 0.5393(2) 0.2425(6) 0.6347(7) 0.072(3) Uani 1 1 d . . .
C34 C 0.5772(3) 0.2359(7) 0.6313(7) 0.077(3) Uani 1 1 d . . .
H34 H 0.5922 0.2795 0.6284 0.093 Uiso 1 1 calc R . .
C35 C 0.5928(3) 0.1619(8) 0.6324(7) 0.085(3) Uani 1 1 d . . .
H35 H 0.6183 0.1568 0.6269 0.102 Uiso 1 1 calc R . .
C36 C 0.5211(2) 0.3156(6) 0.6328(7) 0.075(3) Uani 1 1 d . . .
O7 O 0.5890(2) 0.1934(5) 1.3773(6) 0.104(2) Uani 1 1 d . . .
H7 H 0.6114 0.1940 1.3925 0.156 Uiso 1 1 calc R . .
O8 O 0.49267(18) 0.4919(4) 1.3692(7) 0.094(2) Uani 1 1 d . . .
O9 O 0.54800(18) 0.5450(4) 1.3819(5) 0.0858(19) Uani 1 1 d . . .
O10 O 0.5889(2) 0.0287(5) 0.6449(6) 0.109(3) Uani 1 1 d . . .
H10 H 0.5734 -0.0054 0.6517 0.164 Uiso 1 1 calc R . .
O11 O 0.48639(16) 0.3249(4) 0.6273(6) 0.089(2) Uani 1 1 d . . .
O12 O 0.54262(17) 0.3760(5) 0.6365(5) 0.090(2) Uani 1 1 d . . .
C1 C 0.84166(19) 0.1948(4) 0.8031(5) 0.0453(16) Uani 1 1 d . . .
C2 C 0.88713(16) 0.1603(4) 0.9240(5) 0.0399(15) Uani 1 1 d . . .
C3 C 0.86439(18) 0.0879(4) 0.8894(5) 0.0444(16) Uani 1 1 d . . .
C4 C 0.8566(2) 0.1080(4) 1.0579(5) 0.0477(17) Uani 1 1 d . . .
C5 C 0.81165(19) 0.0763(4) 0.7528(5) 0.0503(17) Uani 1 1 d . . .
H5A H 0.8223 0.0267 0.7375 0.060 Uiso 1 1 calc R . .
H5B H 0.8068 0.1038 0.6909 0.060 Uiso 1 1 calc R . .
C6 C 0.82404(19) -0.0028(4) 0.9899(6) 0.0525(18) Uani 1 1 d . . .
H6A H 0.8260 -0.0180 1.0592 0.063 Uiso 1 1 calc R . .
H6B H 0.8338 -0.0447 0.9518 0.063 Uiso 1 1 calc R . .
C7 C 0.74450(18) 0.0950(4) 0.7599(5) 0.0419(15) Uani 1 1 d . . .
C8 C 0.77056(19) -0.0009(4) 0.8583(5) 0.0487(17) Uani 1 1 d . . .
H8 H 0.7792 -0.0487 0.8288 0.058 Uiso 1 1 calc R . .
C9 C 0.72872(18) -0.0015(4) 0.8678(5) 0.0439(15) Uani 1 1 d . . .
H9 H 0.7176 -0.0509 0.8472 0.053 Uiso 1 1 calc R . .
C10 C 0.75887(18) 0.0149(4) 1.0235(6) 0.0448(16) Uani 1 1 d . . .
C11 C 0.67818(19) 0.0737(4) 0.7751(5) 0.0511(18) Uani 1 1 d . . .
H11A H 0.6664 0.0247 0.7591 0.061 Uiso 1 1 calc R . .
H11B H 0.6766 0.1048 0.7154 0.061 Uiso 1 1 calc R . .
C12 C 0.6919(2) -0.0032(4) 1.0172(6) 0.0521(18) Uani 1 1 d . . .
H12A H 0.6981 -0.0160 1.0861 0.063 Uiso 1 1 calc R . .
H12B H 0.6802 -0.0481 0.9859 0.063 Uiso 1 1 calc R . .
C13 C 0.64979(18) 0.1871(4) 0.8397(5) 0.0439(16) Uani 1 1 d . . .
C14 C 0.64015(19) 0.0742(4) 0.9274(5) 0.0477(17) Uani 1 1 d . . .
C15 C 0.61552(18) 0.1414(4) 0.9674(5) 0.0493(17) Uani 1 1 d . . .
C16 C 0.65883(18) 0.1014(4) 1.0947(5) 0.0479(17) Uani 1 1 d . . .
C17 C 0.6062(2) 0.2790(4) 0.9026(5) 0.0506(17) Uani 1 1 d . . .
H17A H 0.6073 0.2990 0.8358 0.061 Uiso 1 1 calc R . .
H17B H 0.5802 0.2702 0.9141 0.061 Uiso 1 1 calc R . .
C18 C 0.6174(2) 0.2019(4) 1.1406(5) 0.0485(17) Uani 1 1 d . . .
H18A H 0.6243 0.1828 1.2066 0.058 Uiso 1 1 calc R . .
H18B H 0.5904 0.2033 1.1334 0.058 Uiso 1 1 calc R . .
C19 C 0.9280(2) 0.1565(5) 0.9083(6) 0.064(2) Uani 1 1 d . . .
H19A H 0.9316 0.1550 0.8385 0.096 Uiso 1 1 calc R . .
H19B H 0.9384 0.1109 0.9393 0.096 Uiso 1 1 calc R . .
H19C H 0.9401 0.2011 0.9371 0.096 Uiso 1 1 calc R . .
C20 C 0.8870(2) 0.0224(5) 0.8493(7) 0.067(2) Uani 1 1 d . . .
H20A H 0.8988 0.0396 0.7915 0.101 Uiso 1 1 calc R . .
H20B H 0.8709 -0.0202 0.8319 0.101 Uiso 1 1 calc R . .
H20C H 0.9056 0.0064 0.8990 0.101 Uiso 1 1 calc R . .
C21 C 0.6186(2) 0.0045(6) 0.8947(8) 0.074(2) Uani 1 1 d . . .
H21A H 0.6019 0.0174 0.8389 0.111 Uiso 1 1 calc R . .
H21B H 0.6046 -0.0137 0.9481 0.111 Uiso 1 1 calc R . .
H21C H 0.6353 -0.0351 0.8758 0.111 Uiso 1 1 calc R . .
C22 C 0.5746(2) 0.1255(6) 0.9619(7) 0.076(3) Uani 1 1 d . . .
H22A H 0.5658 0.1190 0.8938 0.114 Uiso 1 1 calc R . .
H22B H 0.5618 0.1680 0.9901 0.114 Uiso 1 1 calc R . .
H22C H 0.5699 0.0794 0.9982 0.114 Uiso 1 1 calc R . .
N1 N 0.86911(15) 0.2213(3) 0.8669(4) 0.0471(14) Uani 1 1 d . . .
N2 N 0.83787(15) 0.1184(3) 0.8136(4) 0.0441(13) Uani 1 1 d . . .
N3 N 0.87968(16) 0.1641(4) 1.0297(4) 0.0488(14) Uani 1 1 d . . .
N4 N 0.84677(16) 0.0644(4) 0.9780(4) 0.0493(14) Uani 1 1 d . . .
N5 N 0.77718(15) 0.0641(3) 0.7980(4) 0.0428(13) Uani 1 1 d . . .
N6 N 0.71642(14) 0.0601(3) 0.8029(4) 0.0462(14) Uani 1 1 d . . .
N7 N 0.78505(15) 0.0079(4) 0.9592(4) 0.0489(14) Uani 1 1 d . . .
N8 N 0.72504(15) 0.0132(3) 0.9704(4) 0.0491(14) Uani 1 1 d . . .
N9 N 0.65758(16) 0.1115(3) 0.8486(4) 0.0478(14) Uani 1 1 d . . .
N10 N 0.62519(16) 0.2064(3) 0.9080(4) 0.0475(14) Uani 1 1 d . . .
N11 N 0.66550(16) 0.0592(4) 1.0132(4) 0.0507(15) Uani 1 1 d . . .
N12 N 0.63023(16) 0.1487(3) 1.0704(4) 0.0487(14) Uani 1 1 d . . .
O1 O 0.82314(16) 0.2335(3) 0.7432(4) 0.0625(14) Uani 1 1 d . . .
O2 O 0.74174(15) 0.1460(3) 0.6978(4) 0.0564(13) Uani 1 1 d . . .
O3 O 0.66165(14) 0.2301(3) 0.7807(4) 0.0570(13) Uani 1 1 d . . .
O4 O 0.84717(16) 0.0974(3) 1.1408(4) 0.0622(14) Uani 1 1 d . . .
O5 O 0.76354(15) 0.0221(3) 1.1124(4) 0.0600(14) Uani 1 1 d . . .
O6 O 0.67581(16) 0.0966(3) 1.1740(4) 0.0616(14) 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
Cs1 O1W 2.089(13) . ?
Cs1 O5 3.154(6) 7_657 ?
Cs1 O2 3.255(5) . ?
Cs1 O3 3.296(5) . ?
Cs1 O6 3.363(6) 7_657 ?
Cs1 O1 3.370(6) . ?
Cs1 O4 3.786(6) 7_657 ?
Cs1 C7 3.815(7) . ?
Cs1 C10 3.819(7) 7_657 ?
Cs1 Cs1 5.501(3) 7_657 ?
C23 C28 1.341(15) . ?
C23 C24 1.359(15) . ?
C23 O7 1.390(12) . ?
C24 C25 1.365(16) . ?
C24 H24 0.9400 . ?
C25 C26 1.370(13) . ?
C25 H25 0.9400 . ?
C26 C27 1.410(13) . ?
C26 C29 1.459(14) . ?
C27 C28 1.388(14) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 O8 1.251(11) . ?
C29 O9 1.285(12) . ?
C30 O10 1.357(14) . ?
C30 C31 1.368(15) . ?
C30 C35 1.370(16) . ?
C31 C32 1.371(16) . ?
C31 H31 0.9400 . ?
C32 C33 1.372(15) . ?
C32 H32 0.9400 . ?
C33 C34 1.389(13) . ?
C33 C36 1.443(14) . ?
C34 C35 1.416(16) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 O11 1.273(11) . ?
C36 O12 1.315(12) . ?
O7 H7 0.8300 . ?
O10 H10 0.8300 . ?
C1 O1 1.230(9) . ?
C1 N2 1.354(9) . ?
C1 N1 1.366(9) . ?
C2 N1 1.454(9) . ?
C2 N3 1.486(9) . ?
C2 C19 1.518(9) . ?
C2 C3 1.573(10) . ?
C3 N4 1.463(9) . ?
C3 N2 1.472(9) . ?
C3 C20 1.534(10) . ?
C4 O4 1.218(8) . ?
C4 N4 1.360(10) . ?
C4 N3 1.364(10) . ?
C5 N2 1.431(9) . ?
C5 N5 1.449(9) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.456(10) . ?
C6 N7 1.468(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.232(8) . ?
C7 N6 1.356(9) . ?
C7 N5 1.380(9) . ?
C8 N5 1.434(9) . ?
C8 N7 1.451(10) . ?
C8 C9 1.538(10) . ?
C8 H8 0.9900 . ?
C9 N8 1.437(9) . ?
C9 N6 1.450(9) . ?
C9 H9 0.9900 . ?
C10 O5 1.221(9) . ?
C10 N7 1.342(9) . ?
C10 N8 1.391(9) . ?
C10 Cs1 3.819(7) 7_657 ?
C11 N6 1.440(9) . ?
C11 N9 1.449(9) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N8 1.431(9) . ?
C12 N11 1.455(9) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.204(8) . ?
C13 N9 1.360(9) . ?
C13 N10 1.375(9) . ?
C14 N9 1.440(9) . ?
C14 N11 1.469(10) . ?
C14 C21 1.505(11) . ?
C14 C15 1.598(10) . ?
C15 N10 1.455(9) . ?
C15 N12 1.479(10) . ?
C15 C22 1.515(11) . ?
C16 O6 1.216(9) . ?
C16 N12 1.357(9) . ?
C16 N11 1.370(10) . ?
C17 N3 1.434(10) 7_657 ?
C17 N10 1.448(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N12 1.437(9) . ?
C18 N1 1.439(9) 7_657 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
N1 C18 1.439(9) 7_657 ?
N3 C17 1.434(10) 7_657 ?
O4 Cs1 3.786(6) 7_657 ?
O5 Cs1 3.154(6) 7_657 ?
O6 Cs1 3.363(6) 7_657 ?

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
O1W Cs1 O5 108.4(5) . 7_657 ?
O1W Cs1 O2 63.3(6) . . ?
O5 Cs1 O2 168.73(14) 7_657 . ?
O1W Cs1 O3 94.9(9) . . ?
O5 Cs1 O3 110.04(14) 7_657 . ?
O2 Cs1 O3 64.97(13) . . ?
O1W Cs1 O6 81.0(8) . 7_657 ?
O5 Cs1 O6 66.97(14) 7_657 7_657 ?
O2 Cs1 O6 116.82(14) . 7_657 ?
O3 Cs1 O6 173.47(14) . 7_657 ?
O1W Cs1 O1 62.4(7) . . ?
O5 Cs1 O1 123.37(14) 7_657 . ?
O2 Cs1 O1 60.95(13) . . ?
O3 Cs1 O1 125.90(13) . . ?
O6 Cs1 O1 56.47(13) 7_657 . ?
O1W Cs1 O4 110.7(7) . 7_657 ?
O5 Cs1 O4 56.28(13) 7_657 7_657 ?
O2 Cs1 O4 117.95(13) . 7_657 ?
O3 Cs1 O4 53.76(12) . 7_657 ?
O6 Cs1 O4 122.99(13) 7_657 7_657 ?
O1 Cs1 O4 172.95(13) . 7_657 ?
O1W Cs1 C7 80.5(6) . . ?
O5 Cs1 C7 170.61(14) 7_657 . ?
O2 Cs1 C7 17.91(12) . . ?
O3 Cs1 C7 65.28(14) . . ?
O6 Cs1 C7 118.55(14) 7_657 . ?
O1 Cs1 C7 62.98(14) . . ?
O4 Cs1 C7 118.40(13) 7_657 . ?
O1W Cs1 C10 124.2(6) . 7_657 ?
O5 Cs1 C10 16.97(14) 7_657 7_657 ?
O2 Cs1 C10 172.37(14) . 7_657 ?
O3 Cs1 C10 111.16(14) . 7_657 ?
O6 Cs1 C10 67.82(14) 7_657 7_657 ?
O1 Cs1 C10 122.33(14) . 7_657 ?
O4 Cs1 C10 59.75(13) 7_657 7_657 ?
C7 Cs1 C10 155.01(15) . 7_657 ?
O1W Cs1 Cs1 154.9(5) . 7_657 ?
O5 Cs1 Cs1 93.16(10) 7_657 7_657 ?
O2 Cs1 Cs1 96.80(9) . 7_657 ?
O3 Cs1 Cs1 89.39(10) . 7_657 ?
O6 Cs1 Cs1 96.51(9) 7_657 7_657 ?
O1 Cs1 Cs1 95.31(10) . 7_657 ?
O4 Cs1 Cs1 91.73(8) 7_657 7_657 ?
C7 Cs1 Cs1 78.90(10) . 7_657 ?
C10 Cs1 Cs1 76.30(11) 7_657 7_657 ?
C28 C23 C24 121.2(11) . . ?
C28 C23 O7 122.4(10) . . ?
C24 C23 O7 116.3(11) . . ?
C23 C24 C25 119.4(11) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C24 C25 C26 122.1(9) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C25 C26 C27 117.3(10) . . ?
C25 C26 C29 121.1(9) . . ?
C27 C26 C29 121.5(9) . . ?
C28 C27 C26 119.6(9) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C23 C28 C27 120.3(9) . . ?
C23 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
O8 C29 O9 121.8(10) . . ?
O8 C29 C26 119.6(9) . . ?
O9 C29 C26 118.6(8) . . ?
O10 C30 C31 122.9(12) . . ?
O10 C30 C35 118.8(10) . . ?
C31 C30 C35 118.3(12) . . ?
C30 C31 C32 120.3(12) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C33 122.7(9) . . ?
C31 C32 H32 118.7 . . ?
C33 C32 H32 118.7 . . ?
C32 C33 C34 118.3(10) . . ?
C32 C33 C36 119.8(8) . . ?
C34 C33 C36 122.0(9) . . ?
C33 C34 C35 118.3(10) . . ?
C33 C34 H34 120.9 . . ?
C35 C34 H34 120.9 . . ?
C30 C35 C34 122.1(9) . . ?
C30 C35 H35 119.0 . . ?
C34 C35 H35 119.0 . . ?
O11 C36 O12 119.1(10) . . ?
O11 C36 C33 124.6(9) . . ?
O12 C36 C33 116.3(8) . . ?
C23 O7 H7 109.5 . . ?
C30 O10 H10 109.5 . . ?
O1 C1 N2 124.1(7) . . ?
O1 C1 N1 125.8(7) . . ?
N2 C1 N1 110.1(6) . . ?
N1 C2 N3 112.6(5) . . ?
N1 C2 C19 111.8(6) . . ?
N3 C2 C19 112.3(6) . . ?
N1 C2 C3 102.8(5) . . ?
N3 C2 C3 101.6(5) . . ?
C19 C2 C3 115.1(6) . . ?
N4 C3 N2 112.4(5) . . ?
N4 C3 C20 111.0(6) . . ?
N2 C3 C20 111.4(6) . . ?
N4 C3 C2 103.2(5) . . ?
N2 C3 C2 103.1(5) . . ?
C20 C3 C2 115.3(6) . . ?
O4 C4 N4 125.7(7) . . ?
O4 C4 N3 126.0(7) . . ?
N4 C4 N3 108.3(6) . . ?
N2 C5 N5 113.2(6) . . ?
N2 C5 H5A 108.9 . . ?
N5 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
N5 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
N4 C6 N7 114.3(6) . . ?
N4 C6 H6A 108.7 . . ?
N7 C6 H6A 108.7 . . ?
N4 C6 H6B 108.7 . . ?
N7 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
O2 C7 N6 126.4(6) . . ?
O2 C7 N5 125.2(6) . . ?
N6 C7 N5 108.4(6) . . ?
O2 C7 Cs1 54.4(3) . . ?
N6 C7 Cs1 110.3(4) . . ?
N5 C7 Cs1 109.3(4) . . ?
N5 C8 N7 113.4(6) . . ?
N5 C8 C9 104.9(5) . . ?
N7 C8 C9 102.9(6) . . ?
N5 C8 H8 111.7 . . ?
N7 C8 H8 111.7 . . ?
C9 C8 H8 111.7 . . ?
N8 C9 N6 114.8(6) . . ?
N8 C9 C8 103.6(6) . . ?
N6 C9 C8 102.3(5) . . ?
N8 C9 H9 111.8 . . ?
N6 C9 H9 111.8 . . ?
C8 C9 H9 111.8 . . ?
O5 C10 N7 126.9(6) . . ?
O5 C10 N8 125.8(6) . . ?
N7 C10 N8 107.4(6) . . ?
O5 C10 Cs1 48.9(4) . 7_657 ?
N7 C10 Cs1 120.1(4) . 7_657 ?
N8 C10 Cs1 105.7(4) . 7_657 ?
N6 C11 N9 115.4(6) . . ?
N6 C11 H11A 108.4 . . ?
N9 C11 H11A 108.4 . . ?
N6 C11 H11B 108.4 . . ?
N9 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
N8 C12 N11 113.9(6) . . ?
N8 C12 H12A 108.8 . . ?
N11 C12 H12A 108.8 . . ?
N8 C12 H12B 108.8 . . ?
N11 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
O3 C13 N9 126.0(6) . . ?
O3 C13 N10 125.2(7) . . ?
N9 C13 N10 108.8(6) . . ?
N9 C14 N11 113.1(6) . . ?
N9 C14 C21 113.2(6) . . ?
N11 C14 C21 112.5(7) . . ?
N9 C14 C15 101.8(6) . . ?
N11 C14 C15 101.4(5) . . ?
C21 C14 C15 113.9(6) . . ?
N10 C15 N12 112.1(6) . . ?
N10 C15 C22 112.9(7) . . ?
N12 C15 C22 111.1(6) . . ?
N10 C15 C14 103.1(5) . . ?
N12 C15 C14 102.2(5) . . ?
C22 C15 C14 114.8(7) . . ?
O6 C16 N12 126.8(7) . . ?
O6 C16 N11 125.5(7) . . ?
N12 C16 N11 107.7(6) . . ?
N3 C17 N10 115.3(6) 7_657 . ?
N3 C17 H17A 108.5 7_657 . ?
N10 C17 H17A 108.5 . . ?
N3 C17 H17B 108.5 7_657 . ?
N10 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
N12 C18 N1 115.6(5) . 7_657 ?
N12 C18 H18A 108.4 . . ?
N1 C18 H18A 108.4 7_657 . ?
N12 C18 H18B 108.4 . . ?
N1 C18 H18B 108.4 7_657 . ?
H18A C18 H18B 107.4 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 H20A 109.5 . . ?
C3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C14 C21 H21A 109.5 . . ?
C14 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C14 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C18 120.9(6) . 7_657 ?
C1 N1 C2 112.3(6) . . ?
C18 N1 C2 125.5(6) 7_657 . ?
C1 N2 C5 121.2(6) . . ?
C1 N2 C3 111.6(6) . . ?
C5 N2 C3 127.2(6) . . ?
C4 N3 C17 121.5(6) . 7_657 ?
C4 N3 C2 113.3(6) . . ?
C17 N3 C2 125.2(6) 7_657 . ?
C4 N4 C6 119.3(6) . . ?
C4 N4 C3 113.4(6) . . ?
C6 N4 C3 127.0(6) . . ?
C7 N5 C8 110.9(5) . . ?
C7 N5 C5 122.1(6) . . ?
C8 N5 C5 122.9(6) . . ?
C7 N6 C11 123.7(6) . . ?
C7 N6 C9 112.8(5) . . ?
C11 N6 C9 122.8(6) . . ?
C10 N7 C8 113.6(6) . . ?
C10 N7 C6 122.6(6) . . ?
C8 N7 C6 123.1(6) . . ?
C10 N8 C12 121.1(6) . . ?
C10 N8 C9 112.2(5) . . ?
C12 N8 C9 122.1(6) . . ?
C13 N9 C14 114.2(6) . . ?
C13 N9 C11 119.9(6) . . ?
C14 N9 C11 125.5(6) . . ?
C13 N10 C17 120.8(6) . . ?
C13 N10 C15 112.1(6) . . ?
C17 N10 C15 125.8(6) . . ?
C16 N11 C12 121.7(6) . . ?
C16 N11 C14 114.6(6) . . ?
C12 N11 C14 123.0(6) . . ?
C16 N12 C18 120.8(6) . . ?
C16 N12 C15 114.0(6) . . ?
C18 N12 C15 125.2(6) . . ?
C1 O1 Cs1 118.2(5) . . ?
C7 O2 Cs1 107.7(4) . . ?
C13 O3 Cs1 122.2(5) . . ?
C4 O4 Cs1 112.9(4) . 7_657 ?
C10 O5 Cs1 114.1(4) . 7_657 ?
C16 O6 Cs1 114.0(4) . 7_657 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.444
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.144

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.250 0.000 162 58 ' '
2 0.750 0.750 0.000 162 58 ' '
3 0.000 0.580 0.250 120 41 ' '
4 0.500 0.080 0.250 120 41 ' '
5 0.250 0.750 0.500 162 58 ' '
6 0.750 0.250 0.500 162 58 ' '
7 0.000 0.419 0.750 117 40 ' '
8 0.500 0.919 0.750 117 40 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex4
_database_code_depnum_ccdc_archive 'CCDC 1519710'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_publ_requested_journal_name     'Eur. J. Inorg. Chem.'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 Cs N24 O12, Cd2 Cl7, 2(H3 O), 5(H2 O)'
_chemical_formula_sum            'C44 H68 Cd2 Cl7 Cs N24 O19'
_chemical_formula_weight         1843.08

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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   21.382(3)
_cell_length_b                   13.150(2)
_cell_length_c                   26.066(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.422(3)
_cell_angle_gamma                90.00
_cell_volume                     7030.0(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3688
_exptl_absorpt_coefficient_mu    1.464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6597
_exptl_absorpt_correction_T_max  0.7202
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19435
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.10
_reflns_number_total             6257
_reflns_number_gt                4591
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.1039P)²+2.2176P] 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         6257
_refine_ls_number_parameters     411
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1855
_refine_ls_wR_factor_gt          0.1731
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_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
Cs1 Cs 0.61304(11) 0.60182(15) 0.46003(8) 0.1669(8) Uani 0.50 1 d P . .
Cd1 Cd 0.40214(2) 0.01307(3) 0.252906(17) 0.05308(19) Uani 1 1 d . . .
Cl1 Cl 0.39703(9) 0.17684(13) 0.20886(6) 0.0694(5) Uani 1 1 d . . .
Cl2 Cl 0.31940(7) -0.10919(13) 0.20742(7) 0.0739(5) Uani 1 1 d . . .
Cl3 Cl 0.40411(14) 0.02716(15) 0.34517(8) 0.1019(8) Uani 1 1 d . . .
Cl4 Cl 0.5000 -0.0904(2) 0.2500 0.0988(10) Uani 1 2 d S . .
C1 C 0.6835(2) 0.3146(4) 0.5234(2) 0.0464(12) Uani 1 1 d . . .
C2 C 0.6634(2) 0.2019(4) 0.5872(2) 0.0499(13) Uani 1 1 d . . .
C3 C 0.6342(2) 0.1564(4) 0.5295(2) 0.0492(13) Uani 1 1 d . . .
C4 C 0.5500(2) 0.1871(4) 0.5689(2) 0.0458(12) Uani 1 1 d . . .
C5 C 0.6406(2) 0.2284(5) 0.4378(2) 0.0513(13) Uani 1 1 d . . .
H5A H 0.6744 0.2685 0.4284 0.062 Uiso 1 1 calc R . .
H5B H 0.6451 0.1578 0.4274 0.062 Uiso 1 1 calc R . .
C6 C 0.5135(3) 0.1165(4) 0.4790(2) 0.0520(14) Uani 1 1 d . . .
H6A H 0.5304 0.0575 0.4642 0.062 Uiso 1 1 calc R . .
H6B H 0.4766 0.0933 0.4913 0.062 Uiso 1 1 calc R . .
C7 C 0.5681(3) 0.3553(4) 0.3795(2) 0.0466(12) Uani 1 1 d . . .
C8 C 0.5209(2) 0.2026(4) 0.3941(2) 0.0455(12) Uani 1 1 d . . .
H8 H 0.5291 0.1363 0.3792 0.055 Uiso 1 1 calc R . .
C9 C 0.4711(2) 0.2662(4) 0.3532(2) 0.0435(12) Uani 1 1 d . . .
H9 H 0.4580 0.2324 0.3179 0.052 Uiso 1 1 calc R . .
C10 C 0.4281(3) 0.2250(4) 0.4231(2) 0.0451(12) Uani 1 1 d . . .
C11 C 0.4806(3) 0.4320(5) 0.3086(2) 0.0511(13) Uani 1 1 d . . .
H11A H 0.4615 0.3947 0.2753 0.061 Uiso 1 1 calc R . .
H11B H 0.5176 0.4711 0.3040 0.061 Uiso 1 1 calc R . .
C12 C 0.3530(2) 0.3070(4) 0.3448(2) 0.0511(13) Uani 1 1 d . . .
H12A H 0.3439 0.2795 0.3085 0.061 Uiso 1 1 calc R . .
H12B H 0.3205 0.2790 0.3609 0.061 Uiso 1 1 calc R . .
C13 C 0.4476(2) 0.6003(4) 0.3305(2) 0.0476(13) Uani 1 1 d . . .
C14 C 0.3625(3) 0.4813(4) 0.3033(2) 0.0484(13) Uani 1 1 d . . .
C15 C 0.3347(2) 0.5883(4) 0.3146(2) 0.0480(13) Uani 1 1 d . . .
C16 C 0.3188(2) 0.4638(4) 0.3753(2) 0.0480(13) Uani 1 1 d . . .
C17 C 0.3937(3) 0.7590(4) 0.3401(2) 0.0498(13) Uani 1 1 d . . .
H17A H 0.3555 0.7906 0.3153 0.060 Uiso 1 1 calc R . .
H17B H 0.4326 0.7889 0.3332 0.060 Uiso 1 1 calc R . .
C18 C 0.2726(2) 0.6322(5) 0.3841(2) 0.0529(14) Uani 1 1 d . . .
H18A H 0.2439 0.6717 0.3549 0.064 Uiso 1 1 calc R . .
H18B H 0.2449 0.5904 0.3999 0.064 Uiso 1 1 calc R . .
C19 C 0.7165(3) 0.1372(5) 0.6246(3) 0.0696(18) Uani 1 1 d . . .
H19A H 0.7534 0.1313 0.6100 0.104 Uiso 1 1 calc R . .
H19B H 0.6994 0.0700 0.6280 0.104 Uiso 1 1 calc R . .
H19C H 0.7305 0.1692 0.6595 0.104 Uiso 1 1 calc R . .
C20 C 0.6580(3) 0.0521(5) 0.5202(3) 0.0717(18) Uani 1 1 d . . .
H20A H 0.6458 0.0036 0.5437 0.108 Uiso 1 1 calc R . .
H20B H 0.7051 0.0531 0.5276 0.108 Uiso 1 1 calc R . .
H20C H 0.6384 0.0323 0.4833 0.108 Uiso 1 1 calc R . .
C21 C 0.3358(3) 0.4421(5) 0.2460(2) 0.0683(17) Uani 1 1 d . . .
H21A H 0.3475 0.4890 0.2215 0.102 Uiso 1 1 calc R . .
H21B H 0.2887 0.4367 0.2371 0.102 Uiso 1 1 calc R . .
H21C H 0.3542 0.3757 0.2430 0.102 Uiso 1 1 calc R . .
C22 C 0.2822(3) 0.6332(5) 0.2692(2) 0.0642(16) Uani 1 1 d . . .
H22A H 0.2996 0.6462 0.2392 0.096 Uiso 1 1 calc R . .
H22B H 0.2671 0.6965 0.2807 0.096 Uiso 1 1 calc R . .
H22C H 0.2461 0.5859 0.2583 0.096 Uiso 1 1 calc R . .
N1 N 0.6910(2) 0.2992(4) 0.57634(18) 0.0482(11) Uani 1 1 d . . .
N2 N 0.6512(2) 0.2329(3) 0.49518(17) 0.0470(11) Uani 1 1 d . . .
N3 N 0.60605(19) 0.2160(3) 0.60584(16) 0.0444(10) Uani 1 1 d . . .
N4 N 0.56427(19) 0.1553(4) 0.52450(18) 0.0495(11) Uani 1 1 d . . .
N5 N 0.5777(2) 0.2657(3) 0.40764(17) 0.0453(10) Uani 1 1 d . . .
N6 N 0.5045(2) 0.3595(4) 0.35102(18) 0.0484(11) Uani 1 1 d . . .
N7 N 0.4905(2) 0.1908(3) 0.43725(17) 0.0437(10) Uani 1 1 d . . .
N8 N 0.4167(2) 0.2745(3) 0.37547(16) 0.0449(10) Uani 1 1 d . . .
N9 N 0.4326(2) 0.5019(4) 0.3170(2) 0.0528(12) Uani 1 1 d . . .
N10 N 0.39275(19) 0.6519(3) 0.32879(17) 0.0470(11) Uani 1 1 d . . .
N11 N 0.3462(2) 0.4148(3) 0.34176(17) 0.0452(10) Uani 1 1 d . . .
N12 N 0.3127(2) 0.5654(4) 0.36189(17) 0.0482(11) Uani 1 1 d . . .
O1 O 0.7038(2) 0.3875(3) 0.50412(17) 0.0639(11) Uani 1 1 d . . .
O2 O 0.60943(19) 0.4176(3) 0.37942(17) 0.0628(11) Uani 1 1 d . . .
O3 O 0.50230(18) 0.6356(4) 0.34086(19) 0.0671(12) Uani 1 1 d . . .
O4 O 0.49570(18) 0.1879(4) 0.57511(16) 0.0652(12) Uani 1 1 d . . .
O5 O 0.38932(18) 0.2138(3) 0.44903(16) 0.0603(11) Uani 1 1 d . . .
O6 O 0.30171(18) 0.4258(3) 0.41223(15) 0.0592(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
Cs1 O2 3.194(5) . ?
Cs1 O6 3.333(4) 5_666 ?
Cs1 O3 3.361(5) . ?
Cs1 O5 3.401(5) 5_666 ?
Cs1 O1 3.430(5) . ?
Cs1 O4 3.561(5) 5_666 ?
Cs1 C7 3.833(6) . ?
Cd1 Cl3 2.4006(19) . ?
Cd1 Cl1 2.4283(17) . ?
Cd1 Cl2 2.4361(16) . ?
Cd1 Cl4 2.5146(16) . ?
Cl4 Cd1 2.5146(16) 2_655 ?
C1 O1 1.218(6) . ?
C1 N1 1.359(7) . ?
C1 N2 1.372(7) . ?
C2 N3 1.453(7) . ?
C2 N1 1.468(7) . ?
C2 C19 1.530(7) . ?
C2 C3 1.575(8) . ?
C3 N2 1.459(7) . ?
C3 N4 1.464(6) . ?
C3 C20 1.506(8) . ?
C4 O4 1.217(6) . ?
C4 N4 1.344(7) . ?
C4 N3 1.363(7) . ?
C5 N5 1.439(7) . ?
C5 N2 1.450(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N7 1.441(7) . ?
C6 N4 1.456(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.206(6) . ?
C7 N6 1.354(7) . ?
C7 N5 1.372(7) . ?
C8 N5 1.431(7) . ?
C8 N7 1.458(7) . ?
C8 C9 1.525(7) . ?
C8 H8 0.9900 . ?
C9 N6 1.428(7) . ?
C9 N8 1.442(7) . ?
C9 H9 0.9900 . ?
C10 O5 1.219(6) . ?
C10 N7 1.355(7) . ?
C10 N8 1.361(7) . ?
C11 N6 1.439(7) . ?
C11 N9 1.439(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.424(7) . ?
C12 N8 1.437(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.215(6) . ?
C13 N10 1.345(7) . ?
C13 N9 1.356(7) . ?
C14 N11 1.445(7) . ?
C14 N9 1.466(7) . ?
C14 C21 1.531(8) . ?
C14 C15 1.587(8) . ?
C15 N10 1.455(7) . ?
C15 N12 1.470(7) . ?
C15 C22 1.503(7) . ?
C16 O6 1.229(6) . ?
C16 N11 1.347(8) . ?
C16 N12 1.377(7) . ?
C17 N10 1.439(7) . ?
C17 N3 1.445(7) 5_666 ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N1 1.426(7) 5_666 ?
C18 N12 1.457(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
N1 C18 1.426(7) 5_666 ?
N3 C17 1.445(7) 5_666 ?
O4 Cs1 3.561(5) 5_666 ?
O5 Cs1 3.401(5) 5_666 ?
O6 Cs1 3.333(4) 5_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cs1 O6 118.64(13) . 5_666 ?
O2 Cs1 O3 67.19(12) . . ?
O6 Cs1 O3 168.87(13) 5_666 . ?
O2 Cs1 O5 175.56(12) . 5_666 ?
O6 Cs1 O5 59.53(11) 5_666 5_666 ?
O3 Cs1 O5 113.87(12) . 5_666 ?
O2 Cs1 O1 60.22(11) . . ?
O6 Cs1 O1 58.54(11) 5_666 . ?
O3 Cs1 O1 127.03(12) . . ?
O5 Cs1 O1 118.06(11) 5_666 . ?
O2 Cs1 O4 121.81(12) . 5_666 ?
O6 Cs1 O4 118.31(12) 5_666 5_666 ?
O3 Cs1 O4 54.66(11) . 5_666 ?
O5 Cs1 O4 59.25(10) 5_666 5_666 ?
O1 Cs1 O4 171.98(12) . 5_666 ?
O2 Cs1 C7 16.80(10) . . ?
O6 Cs1 C7 115.89(13) 5_666 . ?
O3 Cs1 C7 66.64(12) . . ?
O5 Cs1 C7 158.98(12) 5_666 . ?
O1 Cs1 C7 61.27(11) . . ?
O4 Cs1 C7 118.11(12) 5_666 . ?
Cl3 Cd1 Cl1 113.01(7) . . ?
Cl3 Cd1 Cl2 110.07(7) . . ?
Cl1 Cd1 Cl2 115.20(6) . . ?
Cl3 Cd1 Cl4 107.03(7) . . ?
Cl1 Cd1 Cl4 113.08(7) . . ?
Cl2 Cd1 Cl4 97.14(6) . . ?
Cd1 Cl4 Cd1 114.51(11) . 2_655 ?
O1 C1 N1 125.6(5) . . ?
O1 C1 N2 125.4(5) . . ?
N1 C1 N2 108.9(5) . . ?
N3 C2 N1 112.1(4) . . ?
N3 C2 C19 113.7(5) . . ?
N1 C2 C19 110.0(5) . . ?
N3 C2 C3 102.9(4) . . ?
N1 C2 C3 102.7(4) . . ?
C19 C2 C3 114.8(5) . . ?
N2 C3 N4 112.2(4) . . ?
N2 C3 C20 112.1(5) . . ?
N4 C3 C20 111.0(5) . . ?
N2 C3 C2 102.9(4) . . ?
N4 C3 C2 102.0(4) . . ?
C20 C3 C2 116.1(5) . . ?
O4 C4 N4 125.1(5) . . ?
O4 C4 N3 125.8(5) . . ?
N4 C4 N3 109.1(4) . . ?
N5 C5 N2 113.5(4) . . ?
N5 C5 H5A 108.9 . . ?
N2 C5 H5A 108.9 . . ?
N5 C5 H5B 108.9 . . ?
N2 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
N7 C6 N4 113.2(4) . . ?
N7 C6 H6A 108.9 . . ?
N4 C6 H6A 108.9 . . ?
N7 C6 H6B 108.9 . . ?
N4 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
O2 C7 N6 126.5(5) . . ?
O2 C7 N5 125.8(5) . . ?
N6 C7 N5 107.7(5) . . ?
O2 C7 Cs1 50.0(3) . . ?
N6 C7 Cs1 108.9(3) . . ?
N5 C7 Cs1 117.2(3) . . ?
N5 C8 N7 113.8(4) . . ?
N5 C8 C9 103.3(4) . . ?
N7 C8 C9 102.8(4) . . ?
N5 C8 H8 112.1 . . ?
N7 C8 H8 112.1 . . ?
C9 C8 H8 112.1 . . ?
N6 C9 N8 114.8(4) . . ?
N6 C9 C8 104.0(4) . . ?
N8 C9 C8 104.0(4) . . ?
N6 C9 H9 111.2 . . ?
N8 C9 H9 111.2 . . ?
C8 C9 H9 111.2 . . ?
O5 C10 N7 125.5(5) . . ?
O5 C10 N8 126.1(5) . . ?
N7 C10 N8 108.4(4) . . ?
N6 C11 N9 114.8(4) . . ?
N6 C11 H11A 108.6 . . ?
N9 C11 H11A 108.6 . . ?
N6 C11 H11B 108.6 . . ?
N9 C11 H11B 108.6 . . ?
H11A C11 H11B 107.5 . . ?
N11 C12 N8 113.1(4) . . ?
N11 C12 H12A 109.0 . . ?
N8 C12 H12A 109.0 . . ?
N11 C12 H12B 109.0 . . ?
N8 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O3 C13 N10 126.2(6) . . ?
O3 C13 N9 124.4(5) . . ?
N10 C13 N9 109.4(4) . . ?
N11 C14 N9 111.9(4) . . ?
N11 C14 C21 112.2(5) . . ?
N9 C14 C21 111.9(5) . . ?
N11 C14 C15 103.4(4) . . ?
N9 C14 C15 101.7(4) . . ?
C21 C14 C15 115.1(5) . . ?
N10 C15 N12 110.9(4) . . ?
N10 C15 C22 111.6(5) . . ?
N12 C15 C22 113.4(5) . . ?
N10 C15 C14 102.7(4) . . ?
N12 C15 C14 101.5(4) . . ?
C22 C15 C14 116.0(5) . . ?
O6 C16 N11 126.4(5) . . ?
O6 C16 N12 124.4(6) . . ?
N11 C16 N12 109.1(5) . . ?
N10 C17 N3 114.7(4) . 5_666 ?
N10 C17 H17A 108.6 . . ?
N3 C17 H17A 108.6 5_666 . ?
N10 C17 H17B 108.6 . . ?
N3 C17 H17B 108.6 5_666 . ?
H17A C17 H17B 107.6 . . ?
N1 C18 N12 114.0(4) 5_666 . ?
N1 C18 H18A 108.8 5_666 . ?
N12 C18 H18A 108.8 . . ?
N1 C18 H18B 108.8 5_666 . ?
N12 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 H20A 109.5 . . ?
C3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C14 C21 H21A 109.5 . . ?
C14 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C14 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C18 121.6(5) . 5_666 ?
C1 N1 C2 112.8(5) . . ?
C18 N1 C2 125.3(5) 5_666 . ?
C1 N2 C5 119.5(4) . . ?
C1 N2 C3 112.7(4) . . ?
C5 N2 C3 127.7(5) . . ?
C4 N3 C17 120.8(4) . 5_666 ?
C4 N3 C2 112.6(4) . . ?
C17 N3 C2 125.8(4) 5_666 . ?
C4 N4 C6 120.8(4) . . ?
C4 N4 C3 113.3(4) . . ?
C6 N4 C3 125.7(5) . . ?
C7 N5 C8 112.2(4) . . ?
C7 N5 C5 124.1(4) . . ?
C8 N5 C5 122.3(5) . . ?
C7 N6 C9 112.2(4) . . ?
C7 N6 C11 122.1(5) . . ?
C9 N6 C11 121.8(5) . . ?
C10 N7 C6 122.0(4) . . ?
C10 N7 C8 111.9(4) . . ?
C6 N7 C8 121.5(4) . . ?
C10 N8 C12 123.2(4) . . ?
C10 N8 C9 111.9(4) . . ?
C12 N8 C9 123.0(4) . . ?
C13 N9 C11 121.5(5) . . ?
C13 N9 C14 113.0(5) . . ?
C11 N9 C14 124.7(5) . . ?
C13 N10 C17 121.7(4) . . ?
C13 N10 C15 113.1(5) . . ?
C17 N10 C15 125.2(4) . . ?
C16 N11 C12 119.8(5) . . ?
C16 N11 C14 113.2(5) . . ?
C12 N11 C14 126.9(5) . . ?
C16 N12 C18 120.6(5) . . ?
C16 N12 C15 112.4(5) . . ?
C18 N12 C15 124.9(5) . . ?
C1 O1 Cs1 123.5(3) . . ?
C7 O2 Cs1 113.2(3) . . ?
C13 O3 Cs1 122.5(4) . . ?
C4 O4 Cs1 123.4(4) . 5_666 ?
C10 O5 Cs1 116.6(3) . 5_666 ?
C16 O6 Cs1 128.8(3) . 5_666 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.103

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.332 -0.221 0.116 118 36 ' '
2 0.332 0.221 0.616 117 35 ' '
3 0.667 -0.222 0.384 116 35 ' '
4 0.667 0.221 0.884 115 34 ' '
5 0.037 0.050 0.568 8 1 ' '
6 0.963 0.050 0.932 8 1 ' '
7 0.066 0.084 0.054 12 1 ' '
8 0.165 0.279 0.380 113 32 ' '
9 0.835 0.279 0.120 114 32 ' '
10 0.934 0.084 0.446 11 1 ' '
11 0.037 0.140 0.987 6 0 ' '
12 0.963 0.140 0.513 7 1 ' '
13 0.458 0.367 0.004 8 1 ' '
14 0.542 0.367 0.496 8 1 ' '
15 0.431 0.425 0.938 8 1 ' '
16 0.569 0.425 0.562 9 1 ' '
17 0.463 0.450 0.431 7 1 ' '
18 0.537 0.450 0.069 7 1 ' '
19 0.165 0.720 0.880 112 31 ' '
20 0.835 0.720 0.620 113 32 ' '
21 0.465 0.559 0.931 7 1 ' '
22 0.535 0.559 0.569 7 1 ' '
23 0.432 0.591 0.447 10 1 ' '
24 0.568 0.591 0.053 10 1 ' '
25 0.463 0.640 0.513 7 1 ' '
26 0.537 0.640 0.987 6 0 ' '
27 0.042 0.867 0.496 8 1 ' '
28 0.958 0.867 0.004 8 1 ' '
29 0.072 0.917 0.562 8 1 ' '
30 0.928 0.917 0.938 7 0 ' '
31 0.035 0.942 0.069 6 0 ' '
32 0.965 0.942 0.431 6 1 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex3
_database_code_depnum_ccdc_archive 'CCDC 1519709'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_publ_requested_journal_name     'Eur. J. Inorg. Chem.'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 N24 O25, Cd Cl4, 2(H3 O), 11(H2 O)'
_chemical_formula_sum            'C44 H80 Cd Cl4 N24 O25'
_chemical_formula_weight         1599.52

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   13.3215(5)
_cell_length_b                   16.4274(7)
_cell_length_c                   16.0353(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.5920(10)
_cell_angle_gamma                90.00
_cell_volume                     3215.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8299
_exptl_absorpt_correction_T_max  0.8585
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29192
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         27.53
_reflns_number_total             14265
_reflns_number_gt                12984
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.0468P)²+1.1298P] 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   0.00
_chemical_absolute_configuration unk
_refine_ls_number_reflns         14265
_refine_ls_number_parameters     766
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0963
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.041
_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 0.2358(3) 0.2088(2) 1.2100(2) 0.0159(7) Uani 1 1 d . . .
C2 C 0.2885(3) 0.0724(2) 1.2376(2) 0.0126(6) Uani 1 1 d . . .
C3 C 0.3933(3) 0.1274(2) 1.2530(2) 0.0124(6) Uani 1 1 d . . .
C4 C 0.3667(3) 0.0352(2) 1.1344(2) 0.0138(7) Uani 1 1 d . . .
C5 C 0.4050(3) 0.2843(2) 1.2374(2) 0.0150(6) Uani 1 1 d . . .
H5A H 0.3600 0.3288 1.2445 0.018 Uiso 1 1 calc R . .
H5B H 0.4718 0.2815 1.2934 0.018 Uiso 1 1 calc R . .
C6 C 0.5336(2) 0.11798(19) 1.1799(2) 0.0121(6) Uani 1 1 d . . .
H6A H 0.5904 0.1290 1.2406 0.015 Uiso 1 1 calc R . .
H6B H 0.5592 0.0725 1.1540 0.015 Uiso 1 1 calc R . .
C7 C 0.3809(2) 0.36050(19) 1.1002(2) 0.0122(6) Uani 1 1 d . . .
C8 C 0.5342(2) 0.2737(2) 1.1549(2) 0.0118(6) Uani 1 1 d . . .
C9 C 0.5335(2) 0.32161(18) 1.06952(19) 0.0112(6) Uani 1 1 d U . .
C10 C 0.5175(2) 0.1814(2) 1.0366(2) 0.0143(6) Uani 1 1 d . . .
C11 C 0.4107(3) 0.44052(19) 0.9822(2) 0.0137(6) Uani 1 1 d . . .
H11A H 0.4798 0.4649 0.9866 0.016 Uiso 1 1 calc R . .
H11B H 0.3719 0.4813 1.0027 0.016 Uiso 1 1 calc R . .
C12 C 0.5217(3) 0.2687(2) 0.9150(2) 0.0166(7) Uani 1 1 d . . .
H12A H 0.5780 0.3085 0.9182 0.020 Uiso 1 1 calc R . .
H12B H 0.5398 0.2172 0.8935 0.020 Uiso 1 1 calc R . .
C13 C 0.2418(2) 0.4496(2) 0.8400(2) 0.0121(6) Uani 1 1 d . . .
C14 C 0.3920(3) 0.3817(2) 0.8295(2) 0.0112(6) Uani 1 1 d . . .
H14 H 0.4551 0.4126 0.8279 0.013 Uiso 1 1 calc R . .
C15 C 0.2933(2) 0.3806(2) 0.7354(2) 0.0112(7) Uani 1 1 d . . .
H15 H 0.3117 0.4076 0.6881 0.013 Uiso 1 1 calc R . .
C16 C 0.3511(3) 0.2463(2) 0.7802(2) 0.0164(7) Uani 1 1 d . . .
C17 C 0.1051(3) 0.4462(2) 0.6793(2) 0.0145(6) Uani 1 1 d . . .
H17A H 0.0735 0.4916 0.7003 0.017 Uiso 1 1 calc R . .
H17B H 0.1189 0.4655 0.6270 0.017 Uiso 1 1 calc R . .
C18 C 0.2058(2) 0.2619(2) 0.6264(2) 0.0159(7) Uani 1 1 d . . .
H18A H 0.2135 0.2973 0.5801 0.019 Uiso 1 1 calc R . .
H18B H 0.2340 0.2080 0.6208 0.019 Uiso 1 1 calc R . .
C19 C -0.0470(2) 0.3706(2) 0.6871(2) 0.0137(6) Uani 1 1 d . . .
C20 C 0.0134(2) 0.3229(2) 0.5775(2) 0.0146(7) Uani 1 1 d . . .
C21 C -0.0986(2) 0.2788(2) 0.5647(2) 0.0125(6) Uani 1 1 d . . .
C22 C 0.0413(2) 0.1819(2) 0.6004(2) 0.0144(7) Uani 1 1 d . . .
C23 C -0.2142(2) 0.29390(19) 0.6612(2) 0.0130(6) Uani 1 1 d . . .
H23A H -0.2237 0.3391 0.6973 0.016 Uiso 1 1 calc R . .
H23B H -0.2784 0.2929 0.6032 0.016 Uiso 1 1 calc R . .
C24 C -0.1439(2) 0.1263(2) 0.5577(2) 0.0142(6) Uani 1 1 d . . .
H24A H -0.1137 0.0788 0.5388 0.017 Uiso 1 1 calc R . .
H24B H -0.2131 0.1404 0.5074 0.017 Uiso 1 1 calc R . .
C25 C -0.1986(3) 0.2192(2) 0.7976(2) 0.0151(6) Uani 1 1 d . . .
C26 C -0.2488(3) 0.1405(2) 0.6635(2) 0.0136(6) Uani 1 1 d . . .
C27 C -0.2451(2) 0.0838(2) 0.7451(2) 0.0130(6) Uani 1 1 d . . .
C28 C -0.1095(3) 0.0428(2) 0.6938(2) 0.0140(6) Uani 1 1 d . . .
C29 C -0.2275(3) 0.1272(2) 0.9061(2) 0.0184(7) Uani 1 1 d . . .
H29A H -0.2841 0.0864 0.8984 0.022 Uiso 1 1 calc R . .
H29B H -0.2489 0.1774 0.9276 0.022 Uiso 1 1 calc R . .
C30 C -0.1089(3) -0.0323(2) 0.8252(2) 0.0150(7) Uani 1 1 d . . .
H30A H -0.1717 -0.0620 0.8271 0.018 Uiso 1 1 calc R . .
H30B H -0.0663 -0.0703 0.8053 0.018 Uiso 1 1 calc R . .
C31 C -0.0648(3) 0.1428(2) 1.0503(2) 0.0153(7) Uani 1 1 d . . .
C32 C -0.0887(3) 0.0157(2) 0.9800(2) 0.0155(7) Uani 1 1 d . . .
H32 H -0.1465 -0.0235 0.9770 0.019 Uiso 1 1 calc R . .
C33 C 0.0113(3) 0.0132(2) 1.0741(2) 0.0141(6) Uani 1 1 d . . .
H33 H -0.0017 -0.0250 1.1166 0.017 Uiso 1 1 calc R . .
C34 C 0.0668(3) -0.0286(2) 0.9594(2) 0.0127(7) Uani 1 1 d . . .
C35 C 0.0875(2) 0.1163(2) 1.1995(2) 0.0152(7) Uani 1 1 d . . .
H35A H 0.0851 0.0711 1.2385 0.018 Uiso 1 1 calc R . .
H35B H 0.0563 0.1643 1.2167 0.018 Uiso 1 1 calc R . .
C36 C 0.2040(3) -0.0414(2) 1.1187(2) 0.0144(6) Uani 1 1 d . . .
H36A H 0.1917 -0.0696 1.1677 0.017 Uiso 1 1 calc R . .
H36B H 0.2370 -0.0805 1.0909 0.017 Uiso 1 1 calc R . .
C37 C 0.2977(3) 0.0184(2) 1.3179(2) 0.0213(8) Uani 1 1 d . . .
H37A H 0.3033 0.0523 1.3691 0.032 Uiso 1 1 calc R . .
H37B H 0.3624 -0.0156 1.3350 0.032 Uiso 1 1 calc R . .
H37C H 0.2332 -0.0158 1.3007 0.032 Uiso 1 1 calc R . .
C38 C 0.4810(3) 0.1266(2) 1.3499(2) 0.0188(7) Uani 1 1 d . . .
H38A H 0.5110 0.0722 1.3650 0.028 Uiso 1 1 calc R . .
H38B H 0.4487 0.1428 1.3919 0.028 Uiso 1 1 calc R . .
H38C H 0.5389 0.1643 1.3544 0.028 Uiso 1 1 calc R . .
C39 C 0.6334(3) 0.2875(2) 1.2436(2) 0.0214(7) Uani 1 1 d . . .
H39A H 0.6367 0.3444 1.2608 0.032 Uiso 1 1 calc R . .
H39B H 0.6995 0.2730 1.2356 0.032 Uiso 1 1 calc R . .
H39C H 0.6271 0.2540 1.2911 0.032 Uiso 1 1 calc R . .
C40 C 0.6379(3) 0.3718(3) 1.0884(3) 0.0262(8) Uani 1 1 d U . .
H40A H 0.6430 0.4151 1.1311 0.039 Uiso 1 1 calc R . .
H40B H 0.6349 0.3953 1.0319 0.039 Uiso 1 1 calc R . .
H40C H 0.7016 0.3368 1.1140 0.039 Uiso 1 1 calc R . .
C41 C 0.0150(3) 0.3629(2) 0.4929(2) 0.0235(8) Uani 1 1 d . . .
H41A H -0.0376 0.4072 0.4743 0.035 Uiso 1 1 calc R . .
H41B H -0.0042 0.3231 0.4443 0.035 Uiso 1 1 calc R . .
H41C H 0.0877 0.3841 0.5058 0.035 Uiso 1 1 calc R . .
C42 C -0.1930(3) 0.2995(2) 0.4737(2) 0.0221(7) Uani 1 1 d . . .
H42A H -0.2090 0.3573 0.4717 0.033 Uiso 1 1 calc R . .
H42B H -0.2576 0.2687 0.4680 0.033 Uiso 1 1 calc R . .
H42C H -0.1722 0.2856 0.4241 0.033 Uiso 1 1 calc R . .
C43 C -0.3603(3) 0.1469(2) 0.5859(2) 0.0183(7) Uani 1 1 d . . .
H43A H -0.3819 0.0941 0.5574 0.027 Uiso 1 1 calc R . .
H43B H -0.3571 0.1857 0.5414 0.027 Uiso 1 1 calc R . .
H43C H -0.4134 0.1651 0.6092 0.027 Uiso 1 1 calc R . .
C44 C -0.3480(3) 0.0325(2) 0.7268(2) 0.0213(8) Uani 1 1 d . . .
H44A H -0.4093 0.0681 0.7185 0.032 Uiso 1 1 calc R . .
H44B H -0.3354 -0.0033 0.7782 0.032 Uiso 1 1 calc R . .
H44C H -0.3642 0.0002 0.6723 0.032 Uiso 1 1 calc R . .
N1 N 0.2017(2) 0.13313(18) 1.21639(18) 0.0148(6) Uani 1 1 d . . .
N2 N 0.3450(2) 0.20828(17) 1.22718(18) 0.0134(5) Uani 1 1 d . . .
N3 N 0.2793(2) 0.02458(17) 1.15712(17) 0.0127(5) Uani 1 1 d . . .
N4 N 0.4350(2) 0.09297(18) 1.18997(17) 0.0120(5) Uani 1 1 d . . .
N5 N 0.4351(2) 0.30380(18) 1.16282(19) 0.0164(6) Uani 1 1 d . . .
N6 N 0.4350(2) 0.37152(18) 1.04221(18) 0.0143(5) Uani 1 1 d . . .
N7 N 0.5225(2) 0.18877(17) 1.12376(18) 0.0133(5) Uani 1 1 d . . .
N8 N 0.5250(2) 0.25676(17) 1.00498(18) 0.0140(6) Uani 1 1 d . . .
N9 N 0.3444(2) 0.42109(18) 0.88665(17) 0.0140(6) Uani 1 1 d . . .
N10 N 0.2089(2) 0.42406(18) 0.75159(18) 0.0148(6) Uani 1 1 d . . .
N11 N 0.4175(2) 0.29663(18) 0.85004(18) 0.0136(6) Uani 1 1 d . . .
N12 N 0.2715(2) 0.29480(18) 0.71629(18) 0.0116(6) Uani 1 1 d . . .
N13 N 0.0266(2) 0.38182(17) 0.64986(17) 0.0133(5) Uani 1 1 d . . .
N14 N -0.1174(2) 0.30933(17) 0.64306(17) 0.0144(6) Uani 1 1 d . . .
N15 N 0.0909(2) 0.25498(17) 0.60938(18) 0.0134(5) Uani 1 1 d . . .
N16 N -0.0689(2) 0.19337(17) 0.57228(19) 0.0141(5) Uani 1 1 d . . .
N17 N -0.2107(2) 0.21895(17) 0.70889(17) 0.0149(6) Uani 1 1 d . . .
N18 N -0.2248(2) 0.14290(18) 0.81848(17) 0.0147(6) Uani 1 1 d . . .
N19 N -0.1672(2) 0.10331(18) 0.63602(17) 0.0133(5) Uani 1 1 d . . .
N20 N -0.1488(2) 0.03374(18) 0.75898(18) 0.0152(6) Uani 1 1 d . . .
N21 N -0.1252(2) 0.09895(19) 0.97521(17) 0.0153(5) Uani 1 1 d . . .
N22 N 0.0209(2) 0.09599(19) 1.10633(18) 0.0162(6) Uani 1 1 d . . .
N23 N -0.0415(2) -0.00386(17) 0.91567(17) 0.0122(5) Uani 1 1 d . . .
N24 N 0.0988(2) -0.01472(18) 1.05027(17) 0.0127(5) Uani 1 1 d . . .
O1 O 0.1797(2) 0.27095(16) 1.19448(17) 0.0219(5) Uani 1 1 d . . .
O2 O 0.29991(19) 0.39795(16) 1.09516(16) 0.0195(5) Uani 1 1 d . . .
O3 O 0.18876(19) 0.49219(15) 0.87057(15) 0.0174(5) Uani 1 1 d . . .
O4 O -0.0480(2) 0.40751(16) 0.75352(16) 0.0216(5) Uani 1 1 d . . .
O5 O -0.1707(2) 0.27622(16) 0.84991(16) 0.0217(5) Uani 1 1 d . . .
O6 O -0.0835(2) 0.21351(17) 1.06790(17) 0.0220(6) Uani 1 1 d . . .
O7 O 0.38365(18) -0.00286(15) 1.07553(15) 0.0172(5) Uani 1 1 d . . .
O8 O 0.5100(2) 0.11762(15) 0.99617(16) 0.0241(6) Uani 1 1 d . . .
O9 O 0.3613(2) 0.17409(15) 0.77686(18) 0.0231(5) Uani 1 1 d . . .
O10 O 0.08787(18) 0.11480(15) 0.61351(16) 0.0201(5) Uani 1 1 d . . .
O11 O -0.0365(2) 0.00304(16) 0.68699(17) 0.0235(6) Uani 1 1 d . . .
O12 O 0.12413(19) -0.05710(16) 0.92329(15) 0.0185(5) Uani 1 1 d . . .
Cd1 Cd 0.429798(17) 0.335763(15) 0.539718(15) 0.01818(6) Uani 1 1 d . . .
Cl1 Cl 0.53919(6) 0.33052(9) 0.70285(5) 0.0310(2) Uani 1 1 d . . .
Cl2 Cl 0.54681(7) 0.36680(6) 0.45773(6) 0.02482(19) Uani 1 1 d . . .
Cl3 Cl 0.28478(8) 0.43899(6) 0.49833(8) 0.0351(2) Uani 1 1 d . . .
Cl4 Cl 0.33316(8) 0.20621(6) 0.47738(7) 0.0332(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 O1 1.230(4) . ?
C1 N1 1.342(4) . ?
C1 N2 1.368(4) . ?
C2 N1 1.461(4) . ?
C2 N3 1.473(4) . ?
C2 C37 1.529(5) . ?
C2 C3 1.596(4) . ?
C3 N4 1.450(4) . ?
C3 N2 1.462(4) . ?
C3 C38 1.525(4) . ?
C4 O7 1.227(4) . ?
C4 N3 1.363(4) . ?
C4 N4 1.368(4) . ?
C5 N5 1.441(4) . ?
C5 N2 1.456(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N7 1.442(4) . ?
C6 N4 1.446(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.216(4) . ?
C7 N5 1.348(4) . ?
C7 N6 1.398(4) . ?
C8 N5 1.462(4) . ?
C8 N7 1.469(4) . ?
C8 C39 1.522(4) . ?
C8 C9 1.576(4) . ?
C9 N8 1.458(4) . ?
C9 N6 1.458(4) . ?
C9 C40 1.539(5) . ?
C10 O8 1.216(4) . ?
C10 N8 1.356(4) . ?
C10 N7 1.377(4) . ?
C11 N6 1.437(4) . ?
C11 N9 1.465(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.437(4) . ?
C12 N8 1.439(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.227(4) . ?
C13 N9 1.353(4) . ?
C13 N10 1.371(4) . ?
C14 N11 1.445(4) . ?
C14 N9 1.458(4) . ?
C14 C15 1.555(4) . ?
C14 H14 0.9900 . ?
C15 N10 1.441(4) . ?
C15 N12 1.446(4) . ?
C15 H15 0.9900 . ?
C16 O9 1.197(4) . ?
C16 N11 1.388(4) . ?
C16 N12 1.393(4) . ?
C17 N13 1.428(4) . ?
C17 N10 1.452(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N15 1.448(4) . ?
C18 N12 1.458(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 O4 1.231(4) . ?
C19 N13 1.349(4) . ?
C19 N14 1.364(4) . ?
C20 N13 1.466(4) . ?
C20 N15 1.467(4) . ?
C20 C41 1.515(4) . ?
C20 C21 1.596(4) . ?
C21 N16 1.450(4) . ?
C21 N14 1.465(4) . ?
C21 C42 1.535(4) . ?
C22 O10 1.241(4) . ?
C22 N15 1.350(4) . ?
C22 N16 1.365(4) . ?
C23 N17 1.440(4) . ?
C23 N14 1.453(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 N16 1.442(4) . ?
C24 N19 1.459(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C25 O5 1.213(4) . ?
C25 N17 1.366(4) . ?
C25 N18 1.377(4) . ?
C26 N19 1.459(4) . ?
C26 N17 1.468(4) . ?
C26 C43 1.512(4) . ?
C26 C27 1.591(4) . ?
C27 N20 1.464(4) . ?
C27 N18 1.465(4) . ?
C27 C44 1.534(5) . ?
C28 O11 1.212(4) . ?
C28 N20 1.352(4) . ?
C28 N19 1.366(4) . ?
C29 N18 1.442(4) . ?
C29 N21 1.446(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C30 N23 1.444(4) . ?
C30 N20 1.461(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C31 O6 1.244(4) . ?
C31 N21 1.357(4) . ?
C31 N22 1.371(4) . ?
C32 N23 1.442(4) . ?
C32 N21 1.444(5) . ?
C32 C33 1.564(4) . ?
C32 H32 0.9900 . ?
C33 N24 1.439(4) . ?
C33 N22 1.443(4) . ?
C33 H33 0.9900 . ?
C34 O12 1.222(4) . ?
C34 N24 1.363(4) . ?
C34 N23 1.389(4) . ?
C35 N22 1.439(4) . ?
C35 N1 1.461(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C36 N3 1.438(4) . ?
C36 N24 1.460(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 H40C 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 H41C 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 H42C 0.9700 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 H43C 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 H44C 0.9700 . ?
Cd1 Cl1 2.4337(8) . ?
Cd1 Cl3 2.4539(10) . ?
Cd1 Cl2 2.4615(9) . ?
Cd1 Cl4 2.4811(10) . ?

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
O1 C1 N1 125.9(3) . . ?
O1 C1 N2 123.9(3) . . ?
N1 C1 N2 110.1(3) . . ?
N1 C2 N3 112.3(3) . . ?
N1 C2 C37 112.4(3) . . ?
N3 C2 C37 112.3(3) . . ?
N1 C2 C3 102.2(2) . . ?
N3 C2 C3 101.5(2) . . ?
C37 C2 C3 115.3(3) . . ?
N4 C3 N2 113.9(3) . . ?
N4 C3 C38 110.9(3) . . ?
N2 C3 C38 111.6(3) . . ?
N4 C3 C2 103.1(2) . . ?
N2 C3 C2 102.3(2) . . ?
C38 C3 C2 114.8(3) . . ?
O7 C4 N3 125.4(3) . . ?
O7 C4 N4 125.2(3) . . ?
N3 C4 N4 109.4(3) . . ?
N5 C5 N2 114.8(3) . . ?
N5 C5 H5A 108.6 . . ?
N2 C5 H5A 108.6 . . ?
N5 C5 H5B 108.6 . . ?
N2 C5 H5B 108.6 . . ?
H5A C5 H5B 107.5 . . ?
N7 C6 N4 115.3(2) . . ?
N7 C6 H6A 108.4 . . ?
N4 C6 H6A 108.4 . . ?
N7 C6 H6B 108.4 . . ?
N4 C6 H6B 108.4 . . ?
H6A C6 H6B 107.5 . . ?
O2 C7 N5 126.6(3) . . ?
O2 C7 N6 124.7(3) . . ?
N5 C7 N6 108.6(3) . . ?
N5 C8 N7 111.9(2) . . ?
N5 C8 C39 110.2(3) . . ?
N7 C8 C39 113.2(3) . . ?
N5 C8 C9 102.4(2) . . ?
N7 C8 C9 102.5(2) . . ?
C39 C8 C9 116.0(3) . . ?
N8 C9 N6 113.1(2) . . ?
N8 C9 C40 109.8(3) . . ?
N6 C9 C40 113.0(3) . . ?
N8 C9 C8 102.9(2) . . ?
N6 C9 C8 103.5(2) . . ?
C40 C9 C8 114.0(2) . . ?
O8 C10 N8 126.1(3) . . ?
O8 C10 N7 125.2(3) . . ?
N8 C10 N7 108.6(3) . . ?
N6 C11 N9 114.1(3) . . ?
N6 C11 H11A 108.7 . . ?
N9 C11 H11A 108.7 . . ?
N6 C11 H11B 108.7 . . ?
N9 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N11 C12 N8 113.8(3) . . ?
N11 C12 H12A 108.8 . . ?
N8 C12 H12A 108.8 . . ?
N11 C12 H12B 108.8 . . ?
N8 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
O3 C13 N9 126.3(3) . . ?
O3 C13 N10 126.3(3) . . ?
N9 C13 N10 107.4(3) . . ?
N11 C14 N9 114.1(3) . . ?
N11 C14 C15 103.9(3) . . ?
N9 C14 C15 101.8(2) . . ?
N11 C14 H14 112.1 . . ?
N9 C14 H14 112.1 . . ?
C15 C14 H14 112.1 . . ?
N10 C15 N12 114.6(3) . . ?
N10 C15 C14 103.7(3) . . ?
N12 C15 C14 103.7(3) . . ?
N10 C15 H15 111.4 . . ?
N12 C15 H15 111.4 . . ?
C14 C15 H15 111.4 . . ?
O9 C16 N11 125.4(3) . . ?
O9 C16 N12 126.9(3) . . ?
N11 C16 N12 107.7(3) . . ?
N13 C17 N10 114.5(3) . . ?
N13 C17 H17A 108.6 . . ?
N10 C17 H17A 108.6 . . ?
N13 C17 H17B 108.6 . . ?
N10 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
N15 C18 N12 112.8(3) . . ?
N15 C18 H18A 109.0 . . ?
N12 C18 H18A 109.0 . . ?
N15 C18 H18B 109.0 . . ?
N12 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
O4 C19 N13 125.3(3) . . ?
O4 C19 N14 124.6(3) . . ?
N13 C19 N14 110.1(3) . . ?
N13 C20 N15 112.4(2) . . ?
N13 C20 C41 112.5(3) . . ?
N15 C20 C41 112.5(3) . . ?
N13 C20 C21 102.2(2) . . ?
N15 C20 C21 101.0(3) . . ?
C41 C20 C21 115.4(2) . . ?
N16 C21 N14 113.2(3) . . ?
N16 C21 C42 112.7(3) . . ?
N14 C21 C42 112.5(3) . . ?
N16 C21 C20 102.7(2) . . ?
N14 C21 C20 101.9(2) . . ?
C42 C21 C20 113.0(3) . . ?
O10 C22 N15 125.6(3) . . ?
O10 C22 N16 125.3(3) . . ?
N15 C22 N16 109.2(3) . . ?
N17 C23 N14 114.4(3) . . ?
N17 C23 H23A 108.7 . . ?
N14 C23 H23A 108.7 . . ?
N17 C23 H23B 108.7 . . ?
N14 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
N16 C24 N19 115.5(3) . . ?
N16 C24 H24A 108.4 . . ?
N19 C24 H24A 108.4 . . ?
N16 C24 H24B 108.4 . . ?
N19 C24 H24B 108.4 . . ?
H24A C24 H24B 107.5 . . ?
O5 C25 N17 126.7(3) . . ?
O5 C25 N18 124.9(3) . . ?
N17 C25 N18 108.4(3) . . ?
N19 C26 N17 111.5(3) . . ?
N19 C26 C43 112.7(3) . . ?
N17 C26 C43 112.2(3) . . ?
N19 C26 C27 102.8(3) . . ?
N17 C26 C27 102.4(2) . . ?
C43 C26 C27 114.5(3) . . ?
N20 C27 N18 112.5(2) . . ?
N20 C27 C44 112.4(3) . . ?
N18 C27 C44 112.4(3) . . ?
N20 C27 C26 101.0(3) . . ?
N18 C27 C26 102.0(3) . . ?
C44 C27 C26 115.7(2) . . ?
O11 C28 N20 125.6(3) . . ?
O11 C28 N19 125.9(3) . . ?
N20 C28 N19 108.5(3) . . ?
N18 C29 N21 114.9(3) . . ?
N18 C29 H29A 108.5 . . ?
N21 C29 H29A 108.5 . . ?
N18 C29 H29B 108.5 . . ?
N21 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
N23 C30 N20 112.9(3) . . ?
N23 C30 H30A 109.0 . . ?
N20 C30 H30A 109.0 . . ?
N23 C30 H30B 109.0 . . ?
N20 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
O6 C31 N21 126.5(3) . . ?
O6 C31 N22 124.4(3) . . ?
N21 C31 N22 109.1(3) . . ?
N23 C32 N21 114.0(3) . . ?
N23 C32 C33 103.7(2) . . ?
N21 C32 C33 102.4(3) . . ?
N23 C32 H32 112.0 . . ?
N21 C32 H32 112.0 . . ?
C33 C32 H32 112.0 . . ?
N24 C33 N22 115.5(3) . . ?
N24 C33 C32 102.7(2) . . ?
N22 C33 C32 103.9(3) . . ?
N24 C33 H33 111.4 . . ?
N22 C33 H33 111.4 . . ?
C32 C33 H33 111.4 . . ?
O12 C34 N24 125.7(3) . . ?
O12 C34 N23 126.4(3) . . ?
N24 C34 N23 107.9(3) . . ?
N22 C35 N1 113.6(3) . . ?
N22 C35 H35A 108.8 . . ?
N1 C35 H35A 108.8 . . ?
N22 C35 H35B 108.8 . . ?
N1 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
N3 C36 N24 113.0(3) . . ?
N3 C36 H36A 109.0 . . ?
N24 C36 H36A 109.0 . . ?
N3 C36 H36B 109.0 . . ?
N24 C36 H36B 109.0 . . ?
H36A C36 H36B 107.8 . . ?
C2 C37 H37A 109.5 . . ?
C2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C3 C38 H38A 109.5 . . ?
C3 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C3 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C8 C39 H39A 109.5 . . ?
C8 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C8 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C9 C40 H40A 109.5 . . ?
C9 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C9 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C20 C41 H41A 109.5 . . ?
C20 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C20 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C21 C42 H42A 109.5 . . ?
C21 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C21 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C26 C43 H43A 109.5 . . ?
C26 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C26 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C27 C44 H44A 109.5 . . ?
C27 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C27 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C1 N1 C2 112.9(3) . . ?
C1 N1 C35 121.4(3) . . ?
C2 N1 C35 125.7(3) . . ?
C1 N2 C5 120.5(3) . . ?
C1 N2 C3 112.0(3) . . ?
C5 N2 C3 126.1(3) . . ?
C4 N3 C36 120.4(3) . . ?
C4 N3 C2 112.6(3) . . ?
C36 N3 C2 125.2(3) . . ?
C4 N4 C6 121.4(3) . . ?
C4 N4 C3 112.6(3) . . ?
C6 N4 C3 125.9(3) . . ?
C7 N5 C5 121.8(3) . . ?
C7 N5 C8 113.7(3) . . ?
C5 N5 C8 123.9(3) . . ?
C7 N6 C11 120.7(3) . . ?
C7 N6 C9 111.7(2) . . ?
C11 N6 C9 125.3(3) . . ?
C10 N7 C6 121.0(3) . . ?
C10 N7 C8 112.5(3) . . ?
C6 N7 C8 125.7(3) . . ?
C10 N8 C12 121.5(3) . . ?
C10 N8 C9 113.4(3) . . ?
C12 N8 C9 125.1(3) . . ?
C13 N9 C14 113.8(3) . . ?
C13 N9 C11 123.8(3) . . ?
C14 N9 C11 121.4(3) . . ?
C13 N10 C15 112.9(3) . . ?
C13 N10 C17 123.8(3) . . ?
C15 N10 C17 122.9(3) . . ?
C16 N11 C12 120.9(3) . . ?
C16 N11 C14 112.2(3) . . ?
C12 N11 C14 123.0(3) . . ?
C16 N12 C15 111.9(3) . . ?
C16 N12 C18 119.6(3) . . ?
C15 N12 C18 124.1(3) . . ?
C19 N13 C17 121.4(3) . . ?
C19 N13 C20 112.4(3) . . ?
C17 N13 C20 126.2(3) . . ?
C19 N14 C23 120.4(3) . . ?
C19 N14 C21 112.2(3) . . ?
C23 N14 C21 125.6(3) . . ?
C22 N15 C18 121.7(3) . . ?
C22 N15 C20 113.2(3) . . ?
C18 N15 C20 123.3(3) . . ?
C22 N16 C24 122.1(3) . . ?
C22 N16 C21 112.5(3) . . ?
C24 N16 C21 125.3(3) . . ?
C25 N17 C23 121.0(3) . . ?
C25 N17 C26 113.1(3) . . ?
C23 N17 C26 123.8(3) . . ?
C25 N18 C29 120.4(3) . . ?
C25 N18 C27 113.0(3) . . ?
C29 N18 C27 126.5(3) . . ?
C28 N19 C24 121.0(3) . . ?
C28 N19 C26 112.6(3) . . ?
C24 N19 C26 126.3(3) . . ?
C28 N20 C30 120.2(3) . . ?
C28 N20 C27 114.1(3) . . ?
C30 N20 C27 124.7(3) . . ?
C31 N21 C32 112.9(3) . . ?
C31 N21 C29 123.5(3) . . ?
C32 N21 C29 122.6(3) . . ?
C31 N22 C35 123.8(3) . . ?
C31 N22 C33 111.3(3) . . ?
C35 N22 C33 121.3(3) . . ?
C34 N23 C32 111.5(2) . . ?
C34 N23 C30 121.0(3) . . ?
C32 N23 C30 121.1(3) . . ?
C34 N24 C33 113.4(2) . . ?
C34 N24 C36 123.3(3) . . ?
C33 N24 C36 122.2(2) . . ?
Cl1 Cd1 Cl3 112.53(4) . . ?
Cl1 Cd1 Cl2 110.28(3) . . ?
Cl3 Cd1 Cl2 108.10(3) . . ?
Cl1 Cd1 Cl4 113.18(4) . . ?
Cl3 Cd1 Cl4 104.97(4) . . ?
Cl2 Cd1 Cl4 107.45(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.075

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.367 0.500 739 253 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex2
_database_code_depnum_ccdc_archive 'CCDC 1519708'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_publ_requested_journal_name     'Eur. J. Inorg. Chem.'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H72 K4 N24 O22, Cd2 Cl8, 2(H2 O)'
_chemical_formula_sum            'C44 H76 Cd2 Cl8 K4 N24 O24'
_chemical_formula_weight         1990.09

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   12.4353(9)
_cell_length_b                   12.8181(9)
_cell_length_c                   13.2339(9)
_cell_angle_alpha                61.113(2)
_cell_angle_beta                 79.450(2)
_cell_angle_gamma                79.892(2)
_cell_volume                     1806.4(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7689
_exptl_absorpt_correction_T_max  0.8212
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14143
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         26.00
_reflns_number_total             7072
_reflns_number_gt                5733
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.1195P)²+13.1129P] 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         7072
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0824
_refine_ls_wR_factor_ref         0.2330
_refine_ls_wR_factor_gt          0.2225
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
O1W O 0.3332(9) -1.1463(8) 0.9946(7) 0.095(3) Uani 1 1 d . . .
O2W O 0.5353(12) -0.3988(9) 1.0091(15) 0.165(7) Uani 1 1 d . . .
O3W O 0.6859(15) -0.3756(12) 0.7572(9) 0.155(6) Uani 1 1 d . . .
O4W O 0.3491(13) -0.271(2) 0.8814(14) 0.203(9) Uani 1 1 d . . .
O5W O 0.5476(13) -0.500(2) 0.6811(14) 0.205(8) Uani 1 1 d . . .
K1 K 0.27445(18) -0.3800(2) 0.17231(18) 0.0591(6) Uani 1 1 d . . .
K2 K 0.4783(5) -0.3851(4) 0.8182(4) 0.1491(19) Uani 1 1 d . . .
Cd1 Cd 0.00205(5) 0.08842(6) 0.10064(4) 0.0483(2) Uani 1 1 d . . .
Cl1 Cl -0.10698(14) -0.02049(14) 0.28732(14) 0.0325(4) Uani 1 1 d . . .
Cl2 Cl -0.05740(17) 0.14881(17) -0.09056(16) 0.0437(4) Uani 1 1 d . . .
Cl3 Cl 0.20053(19) 0.0848(2) 0.08413(18) 0.0594(6) Uani 1 1 d . . .
Cl4 Cl -0.0580(5) 0.3027(3) 0.0882(3) 0.1269(19) Uani 1 1 d . . .
C1 C 0.4133(6) -0.1536(5) 0.5325(5) 0.0270(13) Uani 1 1 d . . .
C2 C 0.3874(5) -0.0347(5) 0.3350(5) 0.0244(12) Uani 1 1 d . . .
C3 C 0.2744(5) -0.0799(5) 0.4076(5) 0.0240(12) Uani 1 1 d . . .
C4 C 0.3287(5) -0.1627(5) 0.2803(5) 0.0232(12) Uani 1 1 d . . .
C5 C 0.2266(6) -0.2041(6) 0.6289(6) 0.0342(15) Uani 1 1 d . . .
H5A H 0.1590 -0.1497 0.6212 0.041 Uiso 1 1 calc R . .
H5B H 0.2577 -0.2162 0.6971 0.041 Uiso 1 1 calc R . .
C6 C 0.1474(5) -0.2058(6) 0.3856(6) 0.0267(13) Uani 1 1 d . . .
H6A H 0.1390 -0.2140 0.3176 0.032 Uiso 1 1 calc R . .
H6B H 0.0879 -0.1476 0.3924 0.032 Uiso 1 1 calc R . .
C7 C 0.2455(5) -0.4237(6) 0.7316(6) 0.0291(14) Uani 1 1 d . . .
C8 C 0.1074(5) -0.3370(6) 0.6070(5) 0.0268(13) Uani 1 1 d . . .
C9 C 0.0988(5) -0.4767(6) 0.6811(5) 0.0274(13) Uani 1 1 d . . .
C10 C 0.1413(4) -0.4245(6) 0.4814(5) 0.0258(13) Uani 1 1 d . . .
C11 C 0.2152(6) -0.6350(6) 0.8440(5) 0.0315(14) Uani 1 1 d . . .
H11A H 0.2534 -0.6291 0.8993 0.038 Uiso 1 1 calc R . .
H11B H 0.1456 -0.6685 0.8852 0.038 Uiso 1 1 calc R . .
C12 C 0.1114(5) -0.6350(6) 0.6107(6) 0.0285(13) Uani 1 1 d . . .
H12A H 0.0944 -0.6308 0.5393 0.034 Uiso 1 1 calc R . .
H12B H 0.0507 -0.6694 0.6713 0.034 Uiso 1 1 calc R . .
C13 C 0.3803(5) -0.7723(6) 0.8455(5) 0.0284(13) Uani 1 1 d . . .
C14 C 0.2332(5) -0.7820(5) 0.7646(5) 0.0240(12) Uani 1 1 d . . .
H14 H 0.1675 -0.8185 0.8169 0.029 Uiso 1 1 calc R . .
C15 C 0.3271(5) -0.8784(5) 0.7635(5) 0.0236(12) Uani 1 1 d . . .
H15 H 0.3028 -0.9599 0.8067 0.028 Uiso 1 1 calc R . .
C16 C 0.2770(5) -0.7559(6) 0.5758(6) 0.0276(13) Uani 1 1 d . . .
C17 C 0.5118(5) -0.9391(6) 0.8419(5) 0.0261(13) Uani 1 1 d . . .
H17A H 0.4976 -1.0226 0.8735 0.031 Uiso 1 1 calc R . .
H17B H 0.5426 -0.9324 0.9013 0.031 Uiso 1 1 calc R . .
C18 C 0.4192(5) -0.9228(6) 0.5980(6) 0.0293(14) Uani 1 1 d . . .
H18A H 0.4068 -1.0054 0.6558 0.035 Uiso 1 1 calc R . .
H18B H 0.3924 -0.9072 0.5263 0.035 Uiso 1 1 calc R . .
C19 C 0.3890(6) 0.1008(6) 0.2665(7) 0.0382(16) Uani 1 1 d . . .
H19A H 0.3380 0.1334 0.2085 0.057 Uiso 1 1 calc R . .
H19B H 0.4626 0.1196 0.2284 0.057 Uiso 1 1 calc R . .
H19C H 0.3675 0.1355 0.3189 0.057 Uiso 1 1 calc R . .
C20 C 0.1814(6) 0.0182(6) 0.3957(7) 0.0397(17) Uani 1 1 d . . .
H20A H 0.2002 0.0680 0.4252 0.060 Uiso 1 1 calc R . .
H20B H 0.1145 -0.0176 0.4397 0.060 Uiso 1 1 calc R . .
H20C H 0.1701 0.0670 0.3144 0.060 Uiso 1 1 calc R . .
C21 C 0.0018(6) -0.2572(7) 0.6157(7) 0.0437(19) Uani 1 1 d . . .
H21A H -0.0566 -0.2728 0.5867 0.066 Uiso 1 1 calc R . .
H21B H 0.0152 -0.1737 0.5698 0.066 Uiso 1 1 calc R . .
H21C H -0.0198 -0.2750 0.6962 0.066 Uiso 1 1 calc R . .
C22 C -0.0089(6) -0.5120(7) 0.7581(7) 0.0412(17) Uani 1 1 d . . .
H22A H -0.0177 -0.4842 0.8159 0.062 Uiso 1 1 calc R . .
H22B H -0.0083 -0.5985 0.7967 0.062 Uiso 1 1 calc R . .
H22C H -0.0695 -0.4758 0.7110 0.062 Uiso 1 1 calc R . .
N1 N 0.4636(4) -0.0877(5) 0.4247(5) 0.0290(12) Uani 1 1 d . . .
N2 N 0.3040(5) -0.1468(5) 0.5268(4) 0.0277(11) Uani 1 1 d . . .
N3 N 0.4075(4) -0.0911(5) 0.2599(4) 0.0231(10) Uani 1 1 d . . .
N4 N 0.2510(4) -0.1593(5) 0.3660(4) 0.0242(11) Uani 1 1 d . . .
N5 N 0.1982(5) -0.3189(5) 0.6495(5) 0.0278(11) Uani 1 1 d . . .
N6 N 0.1917(5) -0.5155(5) 0.7496(5) 0.0286(11) Uani 1 1 d . . .
N7 N 0.1355(4) -0.3203(5) 0.4881(5) 0.0264(11) Uani 1 1 d . . .
N8 N 0.1172(4) -0.5149(5) 0.5910(4) 0.0277(11) Uani 1 1 d . . .
N9 N 0.2815(4) -0.7153(5) 0.8048(4) 0.0262(11) Uani 1 1 d . . .
N10 N 0.4091(4) -0.8643(5) 0.8189(4) 0.0247(11) Uani 1 1 d . . .
N11 N 0.2111(4) -0.7146(5) 0.6453(4) 0.0239(10) Uani 1 1 d . . .
N12 N 0.3555(4) -0.8421(5) 0.6397(5) 0.0258(11) Uani 1 1 d . . .
O1 O 0.4592(4) -0.2065(5) 0.6218(4) 0.0390(12) Uani 1 1 d . . .
O2 O 0.3225(4) -0.4331(5) 0.7834(4) 0.0388(11) Uani 1 1 d . . .
O3 O 0.4342(4) -0.7459(5) 0.8967(4) 0.0358(11) Uani 1 1 d . . .
O4 O 0.3284(4) -0.2209(4) 0.2293(4) 0.0315(10) Uani 1 1 d . . .
O5 O 0.1589(4) -0.4347(4) 0.3930(4) 0.0316(10) Uani 1 1 d . . .
O6 O 0.2683(4) -0.7242(5) 0.4741(4) 0.0406(12) 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
O1W K1 2.894(9) 1_546 ?
O2W K2 2.614(14) 2_647 ?
O2W K2 2.664(13) . ?
O3W K2 2.565(18) . ?
O3W K1 2.781(14) 2_646 ?
O4W K2 2.301(18) . ?
O4W K1 3.404(15) 1_556 ?
O5W K2 2.78(2) . ?
O5W K1 2.919(17) 2_646 ?
K1 O4 2.708(5) . ?
K1 O3W 2.781(14) 2_646 ?
K1 O5 2.815(5) . ?
K1 O1W 2.894(9) 1_564 ?
K1 O5W 2.919(17) 2_646 ?
K1 O4W 3.404(15) 1_554 ?
K1 Cl2 3.522(3) 2 ?
K1 K2 3.881(6) 2_646 ?
K1 K2 4.928(6) 1_554 ?
K2 O2 2.316(7) . ?
K2 O1 2.517(6) . ?
K2 O2W 2.614(14) 2_647 ?
K2 C7 3.494(9) . ?
K2 K1 3.881(6) 2_646 ?
K2 K2 4.339(8) 2_647 ?
K2 K1 4.928(6) 1_556 ?
Cd1 Cl3 2.432(2) . ?
Cd1 Cl1 2.4487(17) . ?
Cd1 Cl2 2.4779(18) . ?
Cd1 Cl4 2.649(3) . ?
Cl2 K1 3.522(3) 2 ?
C1 O1 1.232(8) . ?
C1 N1 1.355(9) . ?
C1 N2 1.361(9) . ?
C2 N3 1.454(8) . ?
C2 N1 1.475(8) . ?
C2 C19 1.524(9) . ?
C2 C3 1.577(9) . ?
C3 N4 1.459(8) . ?
C3 N2 1.467(8) . ?
C3 C20 1.520(8) . ?
C4 O4 1.225(7) . ?
C4 N4 1.361(8) . ?
C4 N3 1.361(8) . ?
C5 N2 1.451(9) . ?
C5 N5 1.458(9) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.442(8) . ?
C6 N7 1.447(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.234(8) . ?
C7 N6 1.355(9) . ?
C7 N5 1.370(9) . ?
C8 N5 1.446(9) . ?
C8 N7 1.465(8) . ?
C8 C21 1.540(8) . ?
C8 C9 1.585(9) . ?
C9 N8 1.464(8) . ?
C9 N6 1.465(8) . ?
C9 C22 1.518(9) . ?
C10 O5 1.215(8) . ?
C10 N8 1.369(8) . ?
C10 N7 1.370(9) . ?
C11 N9 1.438(8) . ?
C11 N6 1.457(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N8 1.444(8) . ?
C12 N11 1.449(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.221(8) . ?
C13 N10 1.360(8) . ?
C13 N9 1.371(8) . ?
C14 N11 1.440(8) . ?
C14 N9 1.454(8) . ?
C14 C15 1.548(8) . ?
C14 H14 0.9900 . ?
C15 N10 1.441(7) . ?
C15 N12 1.461(8) . ?
C15 H15 0.9900 . ?
C16 O6 1.225(8) . ?
C16 N11 1.356(8) . ?
C16 N12 1.381(8) . ?
C17 N10 1.439(8) . ?
C17 N3 1.452(8) 2_646 ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N1 1.449(8) 2_646 ?
C18 N12 1.452(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
N1 C18 1.449(8) 2_646 ?
N3 C17 1.452(8) 2_646 ?

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
K2 O2W K2 110.6(3) 2_647 . ?
K2 O3W K1 93.0(5) . 2_646 ?
K2 O4W K1 118.2(8) . 1_556 ?
K2 O5W K1 85.7(5) . 2_646 ?
O4 K1 O3W 137.9(3) . 2_646 ?
O4 K1 O5 74.81(14) . . ?
O3W K1 O5 88.4(3) 2_646 . ?
O4 K1 O1W 59.1(2) . 1_564 ?
O3W K1 O1W 144.4(4) 2_646 1_564 ?
O5 K1 O1W 126.4(2) . 1_564 ?
O4 K1 O5W 73.0(5) . 2_646 ?
O3W K1 O5W 66.0(6) 2_646 2_646 ?
O5 K1 O5W 79.3(3) . 2_646 ?
O1W K1 O5W 108.8(5) 1_564 2_646 ?
O4 K1 O4W 106.1(3) . 1_554 ?
O3W K1 O4W 100.0(4) 2_646 1_554 ?
O5 K1 O4W 164.6(3) . 1_554 ?
O1W K1 O4W 48.6(4) 1_564 1_554 ?
O5W K1 O4W 115.8(4) 2_646 1_554 ?
O4 K1 Cl2 75.99(12) . 2 ?
O3W K1 Cl2 139.7(4) 2_646 2 ?
O5 K1 Cl2 80.62(11) . 2 ?
O1W K1 Cl2 63.8(2) 1_564 2 ?
O5W K1 Cl2 146.5(5) 2_646 2 ?
O4W K1 Cl2 84.7(3) 1_554 2 ?
O4 K1 K2 111.03(14) . 2_646 ?
O3W K1 K2 41.3(4) 2_646 2_646 ?
O5 K1 K2 112.83(13) . 2_646 ?
O1W K1 K2 108.4(2) 1_564 2_646 ?
O5W K1 K2 45.7(4) 2_646 2_646 ?
O4W K1 K2 81.5(3) 1_554 2_646 ?
Cl2 K1 K2 165.81(9) 2 2_646 ?
O4 K1 K2 116.42(12) . 1_554 ?
O3W K1 K2 78.4(3) 2_646 1_554 ?
O5 K1 K2 166.65(13) . 1_554 ?
O1W K1 K2 66.98(18) 1_564 1_554 ?
O5W K1 K2 96.6(3) 2_646 1_554 ?
O4W K1 K2 24.3(4) 1_554 1_554 ?
Cl2 K1 K2 108.40(8) 2 1_554 ?
K2 K1 K2 57.56(9) 2_646 1_554 ?
O4W K2 O2 81.8(4) . . ?
O4W K2 O1 83.4(5) . . ?
O2 K2 O1 83.1(2) . . ?
O4W K2 O3W 131.4(6) . . ?
O2 K2 O3W 143.0(4) . . ?
O1 K2 O3W 85.1(3) . . ?
O4W K2 O2W 102.9(7) . 2_647 ?
O2 K2 O2W 79.7(3) . 2_647 ?
O1 K2 O2W 160.6(3) . 2_647 ?
O3W K2 O2W 103.4(5) . 2_647 ?
O4W K2 O2W 70.6(5) . . ?
O2 K2 O2W 131.8(4) . . ?
O1 K2 O2W 129.6(3) . . ?
O3W K2 O2W 81.5(5) . . ?
O2W K2 O2W 69.4(3) 2_647 . ?
O4W K2 O5W 151.5(5) . . ?
O2 K2 O5W 72.7(4) . . ?
O1 K2 O5W 81.3(4) . . ?
O3W K2 O5W 70.9(5) . . ?
O2W K2 O5W 85.1(5) 2_647 . ?
O2W K2 O5W 136.7(5) . . ?
O4W K2 C7 81.1(4) . . ?
O2 K2 C7 7.40(17) . . ?
O1 K2 C7 75.7(2) . . ?
O3W K2 C7 140.2(3) . . ?
O2W K2 C7 87.0(3) 2_647 . ?
O2W K2 C7 137.2(4) . . ?
O5W K2 C7 72.0(4) . . ?
O4W K2 K1 158.4(4) . 2_646 ?
O2 K2 K1 110.4(2) . 2_646 ?
O1 K2 K1 115.1(2) . 2_646 ?
O3W K2 K1 45.7(3) . 2_646 ?
O2W K2 K1 63.7(4) 2_647 2_646 ?
O2W K2 K1 88.3(3) . 2_646 ?
O5W K2 K1 48.6(4) . 2_646 ?
C7 K2 K1 113.32(16) . 2_646 ?
O4W K2 K2 86.0(5) . 2_647 ?
O2 K2 K2 107.6(2) . 2_647 ?
O1 K2 K2 163.7(2) . 2_647 ?
O3W K2 K2 92.8(3) . 2_647 ?
O2W K2 K2 35.1(2) 2_647 2_647 ?
O2W K2 K2 34.3(3) . 2_647 ?
O5W K2 K2 113.3(4) . 2_647 ?
C7 K2 K2 114.8(2) . 2_647 ?
K1 K2 K2 73.43(15) 2_646 2_647 ?
O4W K2 K1 37.5(5) . 1_556 ?
O2 K2 K1 89.5(2) . 1_556 ?
O1 K2 K1 120.8(2) . 1_556 ?
O3W K2 K1 126.4(3) . 1_556 ?
O2W K2 K1 68.2(4) 2_647 1_556 ?
O2W K2 K1 45.3(4) . 1_556 ?
O5W K2 K1 150.3(4) . 1_556 ?
C7 K2 K1 93.28(16) . 1_556 ?
K1 K2 K1 122.44(9) 2_646 1_556 ?
K2 K2 K1 49.01(13) 2_647 1_556 ?
Cl3 Cd1 Cl1 121.96(7) . . ?
Cl3 Cd1 Cl2 110.45(7) . . ?
Cl1 Cd1 Cl2 124.18(7) . . ?
Cl3 Cd1 Cl4 99.58(14) . . ?
Cl1 Cd1 Cl4 95.37(8) . . ?
Cl2 Cd1 Cl4 93.60(11) . . ?
Cd1 Cl2 K1 114.70(8) . 2 ?
O1 C1 N1 124.9(6) . . ?
O1 C1 N2 125.9(6) . . ?
N1 C1 N2 109.2(5) . . ?
N3 C2 N1 112.1(5) . . ?
N3 C2 C19 112.2(5) . . ?
N1 C2 C19 111.1(5) . . ?
N3 C2 C3 102.4(5) . . ?
N1 C2 C3 102.8(5) . . ?
C19 C2 C3 115.7(5) . . ?
N4 C3 N2 111.7(5) . . ?
N4 C3 C20 112.5(6) . . ?
N2 C3 C20 111.6(5) . . ?
N4 C3 C2 103.1(5) . . ?
N2 C3 C2 102.2(5) . . ?
C20 C3 C2 115.1(5) . . ?
O4 C4 N4 125.6(6) . . ?
O4 C4 N3 125.1(6) . . ?
N4 C4 N3 109.4(5) . . ?
N2 C5 N5 114.9(5) . . ?
N2 C5 H5A 108.5 . . ?
N5 C5 H5A 108.5 . . ?
N2 C5 H5B 108.5 . . ?
N5 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
N4 C6 N7 114.4(5) . . ?
N4 C6 H6A 108.7 . . ?
N7 C6 H6A 108.7 . . ?
N4 C6 H6B 108.7 . . ?
N7 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
O2 C7 N6 125.3(6) . . ?
O2 C7 N5 125.8(6) . . ?
N6 C7 N5 108.9(6) . . ?
O2 C7 K2 14.0(3) . . ?
N6 C7 K2 137.9(4) . . ?
N5 C7 K2 112.9(4) . . ?
N5 C8 N7 112.0(5) . . ?
N5 C8 C21 112.5(6) . . ?
N7 C8 C21 110.4(5) . . ?
N5 C8 C9 103.3(5) . . ?
N7 C8 C9 102.9(5) . . ?
C21 C8 C9 115.1(5) . . ?
N8 C9 N6 112.9(5) . . ?
N8 C9 C22 112.5(6) . . ?
N6 C9 C22 111.7(6) . . ?
N8 C9 C8 102.1(5) . . ?
N6 C9 C8 101.7(5) . . ?
C22 C9 C8 115.2(5) . . ?
O5 C10 N8 125.3(6) . . ?
O5 C10 N7 126.2(6) . . ?
N8 C10 N7 108.4(5) . . ?
N9 C11 N6 113.0(5) . . ?
N9 C11 H11A 109.0 . . ?
N6 C11 H11A 109.0 . . ?
N9 C11 H11B 109.0 . . ?
N6 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N8 C12 N11 114.4(5) . . ?
N8 C12 H12A 108.7 . . ?
N11 C12 H12A 108.7 . . ?
N8 C12 H12B 108.7 . . ?
N11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O3 C13 N10 125.2(6) . . ?
O3 C13 N9 126.4(6) . . ?
N10 C13 N9 108.4(5) . . ?
N11 C14 N9 113.9(5) . . ?
N11 C14 C15 103.7(5) . . ?
N9 C14 C15 103.6(5) . . ?
N11 C14 H14 111.7 . . ?
N9 C14 H14 111.7 . . ?
C15 C14 H14 111.7 . . ?
N10 C15 N12 115.3(5) . . ?
N10 C15 C14 102.6(5) . . ?
N12 C15 C14 102.8(5) . . ?
N10 C15 H15 111.8 . . ?
N12 C15 H15 111.8 . . ?
C14 C15 H15 111.8 . . ?
O6 C16 N11 126.2(6) . . ?
O6 C16 N12 125.2(6) . . ?
N11 C16 N12 108.5(5) . . ?
N10 C17 N3 113.7(5) . 2_646 ?
N10 C17 H17A 108.8 . . ?
N3 C17 H17A 108.8 2_646 . ?
N10 C17 H17B 108.8 . . ?
N3 C17 H17B 108.8 2_646 . ?
H17A C17 H17B 107.7 . . ?
N1 C18 N12 114.1(5) 2_646 . ?
N1 C18 H18A 108.7 2_646 . ?
N12 C18 H18A 108.7 . . ?
N1 C18 H18B 108.7 2_646 . ?
N12 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 H20A 109.5 . . ?
C3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C22 H22A 109.5 . . ?
C9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C18 122.5(5) . 2_646 ?
C1 N1 C2 112.6(5) . . ?
C18 N1 C2 124.9(5) 2_646 . ?
C1 N2 C5 122.6(5) . . ?
C1 N2 C3 113.2(5) . . ?
C5 N2 C3 124.2(6) . . ?
C4 N3 C17 120.1(5) . 2_646 ?
C4 N3 C2 112.9(5) . . ?
C17 N3 C2 126.0(5) 2_646 . ?
C4 N4 C6 119.7(5) . . ?
C4 N4 C3 112.1(5) . . ?
C6 N4 C3 126.3(5) . . ?
C7 N5 C8 112.7(5) . . ?
C7 N5 C5 120.3(6) . . ?
C8 N5 C5 126.0(5) . . ?
C7 N6 C11 120.3(6) . . ?
C7 N6 C9 113.3(5) . . ?
C11 N6 C9 125.5(6) . . ?
C10 N7 C6 122.1(5) . . ?
C10 N7 C8 112.9(5) . . ?
C6 N7 C8 124.8(5) . . ?
C10 N8 C12 121.2(5) . . ?
C10 N8 C9 113.5(5) . . ?
C12 N8 C9 125.3(5) . . ?
C13 N9 C11 121.8(5) . . ?
C13 N9 C14 111.1(5) . . ?
C11 N9 C14 121.8(5) . . ?
C13 N10 C17 123.6(5) . . ?
C13 N10 C15 113.2(5) . . ?
C17 N10 C15 123.2(5) . . ?
C16 N11 C14 112.5(5) . . ?
C16 N11 C12 123.0(5) . . ?
C14 N11 C12 122.4(5) . . ?
C16 N12 C18 120.4(5) . . ?
C16 N12 C15 110.8(5) . . ?
C18 N12 C15 122.0(5) . . ?
C1 O1 K2 149.2(5) . . ?
C7 O2 K2 158.6(5) . . ?
C4 O4 K1 161.4(4) . . ?
C10 O5 K1 151.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.879
_refine_diff_density_min         -2.249
_refine_diff_density_rms         0.161

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.173 0.359 0.099 21 7 ' '
2 0.500 0.500 0.500 66 9 ' '
3 0.827 0.641 0.901 21 7 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex5
_database_code_depnum_ccdc_archive 'CCDC 1519711'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_publ_requested_journal_name     'Eur. J. Inorg. Chem.'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H76 N24 Na2 O24, 2(C7 H6 O3), 2Cl, (H2 O)'
_chemical_formula_sum            'C72 H90 Cl2 N24 Na2 O31'
_chemical_formula_weight         1904.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.239(6)
_cell_length_b                   15.408(8)
_cell_length_c                   24.027(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.565(14)
_cell_angle_gamma                90.00
_cell_volume                     4114(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1988
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9464
_exptl_absorpt_correction_T_max  0.9572
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34438
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         25.10
_reflns_number_total             7236
_reflns_number_gt                3766
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.1074P)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     SHELXL
_refine_ls_extinction_coef       0.0048(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7236
_refine_ls_number_parameters     587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1919
_refine_ls_wR_factor_gt          0.1618
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_restrained_S_all      0.922
_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
Cl1 Cl 0.54530(11) 0.00132(7) 0.63892(5) 0.0622(4) Uani 1 1 d . . .
C23 C 0.9089(3) -0.0782(3) 0.78680(17) 0.0440(10) Uani 1 1 d . . .
C24 C 0.9240(3) -0.1613(3) 0.80968(16) 0.0453(10) Uani 1 1 d . . .
H24 H 0.9075 -0.1721 0.8463 0.054 Uiso 1 1 calc R . .
C25 C 0.9633(3) -0.2279(3) 0.77827(16) 0.0468(10) Uani 1 1 d . . .
H25 H 0.9771 -0.2831 0.7945 0.056 Uiso 1 1 calc R . .
C26 C 0.9269(4) -0.0643(3) 0.73188(17) 0.0520(11) Uani 1 1 d . . .
H26 H 0.9135 -0.0089 0.7157 0.062 Uiso 1 1 calc R . .
C27 C 0.9646(3) -0.1319(3) 0.70046(16) 0.0499(10) Uani 1 1 d . . .
H27 H 0.9780 -0.1215 0.6633 0.060 Uiso 1 1 calc R . .
C28 C 0.9828(3) -0.2144(2) 0.72320(16) 0.0418(10) Uani 1 1 d . . .
C29 C 1.0245(4) -0.2876(3) 0.69198(17) 0.0487(11) Uani 1 1 d . . .
C30 C -0.0360(4) 0.6298(3) 0.9329(2) 0.0586(12) Uani 1 1 d . . .
C31 C -0.0034(4) 0.6500(3) 0.98855(19) 0.0614(12) Uani 1 1 d . . .
H31 H -0.0481 0.6906 1.0060 0.074 Uiso 1 1 calc R . .
C32 C 0.0964(4) 0.6099(3) 1.0192(2) 0.0600(12) Uani 1 1 d . . .
H32 H 0.1188 0.6233 1.0574 0.072 Uiso 1 1 calc R . .
C33 C 0.0320(4) 0.5696(3) 0.9067(2) 0.0668(13) Uani 1 1 d . . .
H33 H 0.0099 0.5559 0.8685 0.080 Uiso 1 1 calc R . .
C34 C 0.1303(4) 0.5313(3) 0.9374(2) 0.0670(13) Uani 1 1 d . . .
H34 H 0.1763 0.4916 0.9198 0.080 Uiso 1 1 calc R . .
C35 C 0.1629(4) 0.5501(3) 0.9935(2) 0.0551(11) Uani 1 1 d . . .
C36 C 0.2711(4) 0.5082(3) 1.0249(2) 0.0640(13) Uani 1 1 d . . .
O7 O 0.8761(3) -0.01446(17) 0.82026(11) 0.0552(8) Uani 1 1 d . . .
H7 H 0.8927 0.0414 0.8077 0.066 Uiso 1 1 calc R . .
O8 O 1.0398(3) -0.36001(19) 0.71099(12) 0.0637(8) Uani 1 1 d . . .
O9 O 1.0406(3) -0.26706(19) 0.64032(13) 0.0762(10) Uani 1 1 d . . .
H9 H 1.0640 -0.3105 0.6246 0.114 Uiso 1 1 calc R . .
O10 O -0.1323(3) 0.6673(2) 0.90039(13) 0.0756(9) Uani 1 1 d . . .
H10 H -0.1651 0.7020 0.9197 0.113 Uiso 1 1 calc R . .
O11 O 0.2997(3) 0.5374(2) 1.07708(17) 0.0866(11) Uani 1 1 d . . .
H11 H 0.3604 0.5115 1.0927 0.130 Uiso 1 1 calc R . .
O12 O 0.3284(3) 0.4532(2) 1.00600(16) 0.1009(13) Uani 1 1 d . . .
O1W O 0.9182(2) 0.11025(17) 0.92761(11) 0.0521(7) Uani 1 1 d . . .
O2W O 0.7297(3) 0.0027(2) 0.99645(13) 0.0741(10) Uani 1 1 d . . .
O3W O 0.9411(2) -0.10586(19) 0.95737(12) 0.0644(9) Uani 1 1 d . . .
Na1 Na 0.78514(13) -0.01225(10) 0.90462(6) 0.0484(4) Uani 1 1 d . . .
C1 C 0.5484(3) -0.1322(2) 0.84256(14) 0.0350(9) Uani 1 1 d . . .
C2 C 0.3661(3) -0.2118(2) 0.82930(14) 0.0352(9) Uani 1 1 d . . .
C3 C 0.3465(3) -0.1195(2) 0.79826(14) 0.0345(9) Uani 1 1 d . . .
C4 C 0.2280(3) -0.1272(3) 0.87149(16) 0.0394(9) Uani 1 1 d . . .
C5 C 0.5068(3) -0.0026(2) 0.78464(15) 0.0378(9) Uani 1 1 d . . .
H5A H 0.5943 -0.0055 0.7862 0.045 Uiso 1 1 calc R . .
H5B H 0.4710 -0.0016 0.7449 0.045 Uiso 1 1 calc R . .
C6 C 0.2016(3) 0.0048(2) 0.81539(16) 0.0428(10) Uani 1 1 d . . .
H6A H 0.1286 0.0072 0.8331 0.051 Uiso 1 1 calc R . .
H6B H 0.1766 0.0074 0.7746 0.051 Uiso 1 1 calc R . .
C7 C 0.5632(3) 0.1237(2) 0.84382(14) 0.0396(9) Uani 1 1 d . . .
C8 C 0.3598(3) 0.1219(2) 0.80108(14) 0.0354(9) Uani 1 1 d . . .
C9 C 0.3876(3) 0.2110(2) 0.83363(14) 0.0354(9) Uani 1 1 d . . .
C10 C 0.2476(3) 0.1304(2) 0.87665(15) 0.0374(9) Uani 1 1 d . . .
C11 C 0.5899(3) 0.2671(2) 0.88786(14) 0.0373(9) Uani 1 1 d . . .
H11A H 0.6740 0.2565 0.8835 0.045 Uiso 1 1 calc R . .
H11B H 0.5676 0.3242 0.8716 0.045 Uiso 1 1 calc R . .
C12 C 0.2899(3) 0.2751(2) 0.91608(14) 0.0401(9) Uani 1 1 d . . .
H12A H 0.2930 0.3314 0.8973 0.048 Uiso 1 1 calc R . .
H12B H 0.2090 0.2687 0.9262 0.048 Uiso 1 1 calc R . .
C13 C 0.6728(3) 0.2455(2) 0.98734(15) 0.0387(9) Uani 1 1 d . . .
C14 C 0.4906(3) 0.3197(2) 0.96938(14) 0.0355(9) Uani 1 1 d . . .
H14 H 0.4816 0.3785 0.9528 0.043 Uiso 1 1 calc R . .
C15 C 0.5364(3) 0.3228(2) 1.03340(13) 0.0346(8) Uani 1 1 d . . .
H15 H 0.5490 0.3831 1.0472 0.042 Uiso 1 1 calc R . .
C16 C 0.3449(3) 0.2595(2) 1.01874(15) 0.0379(9) Uani 1 1 d . . .
C17 C 0.7339(3) 0.2724(2) 1.08873(14) 0.0392(9) Uani 1 1 d . . .
H17A H 0.7332 0.3286 1.1078 0.047 Uiso 1 1 calc R . .
H17B H 0.8142 0.2644 1.0783 0.047 Uiso 1 1 calc R . .
C18 C 0.5610(3) -0.2789(2) 0.88231(13) 0.0373(9) Uani 1 1 d . . .
H18A H 0.6449 -0.2750 0.8760 0.045 Uiso 1 1 calc R . .
H18B H 0.5288 -0.3342 0.8665 0.045 Uiso 1 1 calc R . .
C19 C 0.3353(4) -0.2907(2) 0.79217(15) 0.0489(10) Uani 1 1 d . . .
H19A H 0.2496 -0.2912 0.7786 0.073 Uiso 1 1 calc R . .
H19B H 0.3572 -0.3430 0.8138 0.073 Uiso 1 1 calc R . .
H19C H 0.3794 -0.2883 0.7604 0.073 Uiso 1 1 calc R . .
C20 C 0.3034(3) -0.1253(3) 0.73561(15) 0.0495(10) Uani 1 1 d . . .
H20A H 0.3642 -0.1538 0.7174 0.074 Uiso 1 1 calc R . .
H20B H 0.2891 -0.0674 0.7203 0.074 Uiso 1 1 calc R . .
H20C H 0.2293 -0.1585 0.7290 0.074 Uiso 1 1 calc R . .
C21 C 0.3139(4) 0.1306(3) 0.73868(15) 0.0516(11) Uani 1 1 d . . .
H21A H 0.2373 0.1608 0.7335 0.077 Uiso 1 1 calc R . .
H21B H 0.3034 0.0733 0.7219 0.077 Uiso 1 1 calc R . .
H21C H 0.3715 0.1632 0.7207 0.077 Uiso 1 1 calc R . .
C22 C 0.3653(3) 0.2922(2) 0.79763(15) 0.0452(10) Uani 1 1 d . . .
H22A H 0.2802 0.2969 0.7833 0.068 Uiso 1 1 calc R . .
H22B H 0.4106 0.2887 0.7664 0.068 Uiso 1 1 calc R . .
H22C H 0.3909 0.3429 0.8203 0.068 Uiso 1 1 calc R . .
N1 N 0.4940(2) -0.20917(18) 0.85233(12) 0.0350(7) Uani 1 1 d . . .
N2 N 0.4667(2) -0.08079(19) 0.81040(11) 0.0349(7) Uani 1 1 d . . .
N3 N 0.2866(2) -0.20501(19) 0.87220(12) 0.0368(7) Uani 1 1 d . . .
N4 N 0.2603(2) -0.07790(19) 0.82911(12) 0.0369(7) Uani 1 1 d . . .
N5 N 0.4768(2) 0.07794(19) 0.81077(12) 0.0363(7) Uani 1 1 d . . .
N6 N 0.5154(2) 0.20197(18) 0.85601(11) 0.0355(7) Uani 1 1 d . . .
N7 N 0.2739(2) 0.08107(19) 0.83250(12) 0.0376(7) Uani 1 1 d . . .
N8 N 0.3090(2) 0.20698(19) 0.87674(11) 0.0356(7) Uani 1 1 d . . .
N9 N 0.5813(2) 0.26992(19) 0.94693(11) 0.0368(7) Uani 1 1 d . . .
N10 N 0.6478(2) 0.27492(19) 1.03835(11) 0.0379(7) Uani 1 1 d . . .
N11 N 0.3754(2) 0.27567(19) 0.96659(11) 0.0371(7) Uani 1 1 d . . .
N12 N 0.4418(2) 0.27957(19) 1.05774(11) 0.0369(7) Uani 1 1 d . . .
O1 O 0.6541(2) -0.11572(16) 0.85766(10) 0.0450(7) Uani 1 1 d . . .
O2 O 0.6675(2) 0.10168(16) 0.85772(10) 0.0464(7) Uani 1 1 d . . .
O3 O 0.7639(2) 0.20630(18) 0.98012(10) 0.0497(7) Uani 1 1 d . . .
O4 O 0.1554(2) -0.10691(17) 0.90292(11) 0.0493(7) Uani 1 1 d . . .
O5 O 0.1777(2) 0.11078(17) 0.90926(11) 0.0480(7) Uani 1 1 d . . .
O6 O 0.2479(2) 0.23295(17) 1.02867(10) 0.0452(7) 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
C23 O7 1.354(4) . ?
C23 C26 1.381(5) . ?
C23 C24 1.394(5) . ?
C24 C25 1.384(5) . ?
C24 H24 0.9400 . ?
C25 C28 1.388(5) . ?
C25 H25 0.9400 . ?
C26 C27 1.389(5) . ?
C26 H26 0.9400 . ?
C27 C28 1.388(5) . ?
C27 H27 0.9400 . ?
C28 C29 1.468(5) . ?
C29 O8 1.209(5) . ?
C29 O9 1.319(5) . ?
C30 O10 1.364(5) . ?
C30 C31 1.369(6) . ?
C30 C33 1.408(6) . ?
C31 C32 1.390(6) . ?
C31 H31 0.9400 . ?
C32 C35 1.388(6) . ?
C32 H32 0.9400 . ?
C33 C34 1.368(6) . ?
C33 H33 0.9400 . ?
C34 C35 1.374(6) . ?
C34 H34 0.9400 . ?
C35 C36 1.480(6) . ?
C36 O12 1.195(5) . ?
C36 O11 1.325(6) . ?
O7 Na1 2.403(3) . ?
O7 H7 0.9400 . ?
O9 H9 0.8300 . ?
O10 H10 0.8300 . ?
O11 H11 0.8300 . ?
O1W Na1 2.420(3) . ?
O2W Na1 2.391(4) . ?
O3W Na1 2.470(3) . ?
Na1 O1 2.343(3) . ?
Na1 O2 2.378(3) . ?
C1 O1 1.215(4) . ?
C1 N2 1.363(4) . ?
C1 N1 1.371(4) . ?
C2 N1 1.462(4) . ?
C2 N3 1.465(4) . ?
C2 C19 1.517(5) . ?
C2 C3 1.605(5) . ?
C3 N4 1.454(4) . ?
C3 N2 1.466(4) . ?
C3 C20 1.514(5) . ?
C4 O4 1.233(4) . ?
C4 N4 1.362(5) . ?
C4 N3 1.366(4) . ?
C5 N5 1.453(4) . ?
C5 N2 1.456(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.451(4) . ?
C6 N7 1.452(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.219(4) . ?
C7 N5 1.356(4) . ?
C7 N6 1.370(4) . ?
C8 N7 1.455(4) . ?
C8 N5 1.467(4) . ?
C8 C21 1.517(5) . ?
C8 C9 1.588(5) . ?
C9 N8 1.459(4) . ?
C9 N6 1.464(4) . ?
C9 C22 1.520(5) . ?
C10 O5 1.227(4) . ?
C10 N8 1.367(4) . ?
C10 N7 1.372(5) . ?
C11 N9 1.437(4) . ?
C11 N6 1.450(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.431(4) . ?
C12 N8 1.450(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.223(4) . ?
C13 N9 1.358(4) . ?
C13 N10 1.374(4) . ?
C14 N9 1.443(4) . ?
C14 N11 1.454(4) . ?
C14 C15 1.548(5) . ?
C14 H14 0.9900 . ?
C15 N10 1.443(4) . ?
C15 N12 1.449(4) . ?
C15 H15 0.9900 . ?
C16 O6 1.220(4) . ?
C16 N12 1.362(4) . ?
C16 N11 1.370(4) . ?
C17 N10 1.433(4) . ?
C17 N3 1.441(4) 3_657 ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N1 1.442(4) . ?
C18 N12 1.445(4) 3_657 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
N3 C17 1.441(4) 3_657 ?
N12 C18 1.445(4) 3_657 ?

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
O7 C23 C26 123.1(4) . . ?
O7 C23 C24 117.4(4) . . ?
C26 C23 C24 119.5(4) . . ?
C25 C24 C23 119.7(4) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C28 121.1(4) . . ?
C24 C25 H25 119.4 . . ?
C28 C25 H25 119.4 . . ?
C23 C26 C27 120.2(4) . . ?
C23 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C28 C27 C26 120.8(4) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C27 C28 C25 118.5(4) . . ?
C27 C28 C29 122.8(4) . . ?
C25 C28 C29 118.7(4) . . ?
O8 C29 O9 123.0(4) . . ?
O8 C29 C28 123.6(4) . . ?
O9 C29 C28 113.3(4) . . ?
O10 C30 C31 122.5(4) . . ?
O10 C30 C33 117.4(4) . . ?
C31 C30 C33 120.1(4) . . ?
C30 C31 C32 119.6(4) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C35 C32 C31 120.3(4) . . ?
C35 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C34 C33 C30 119.6(5) . . ?
C34 C33 H33 120.2 . . ?
C30 C33 H33 120.2 . . ?
C33 C34 C35 120.8(5) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C34 C35 C32 119.6(4) . . ?
C34 C35 C36 119.2(4) . . ?
C32 C35 C36 121.2(4) . . ?
O12 C36 O11 122.1(5) . . ?
O12 C36 C35 124.3(5) . . ?
O11 C36 C35 113.6(4) . . ?
C23 O7 Na1 134.3(2) . . ?
C23 O7 H7 112.8 . . ?
Na1 O7 H7 112.8 . . ?
C29 O9 H9 109.5 . . ?
C30 O10 H10 109.5 . . ?
C36 O11 H11 109.5 . . ?
O1 Na1 O2 90.51(11) . . ?
O1 Na1 O2W 106.15(12) . . ?
O2 Na1 O2W 99.42(11) . . ?
O1 Na1 O7 84.27(10) . . ?
O2 Na1 O7 83.51(10) . . ?
O2W Na1 O7 169.06(13) . . ?
O1 Na1 O1W 164.44(11) . . ?
O2 Na1 O1W 79.25(10) . . ?
O2W Na1 O1W 87.22(11) . . ?
O7 Na1 O1W 82.96(10) . . ?
O1 Na1 O3W 101.37(11) . . ?
O2 Na1 O3W 167.52(11) . . ?
O2W Na1 O3W 81.09(11) . . ?
O7 Na1 O3W 93.78(11) . . ?
O1W Na1 O3W 88.34(11) . . ?
O1 C1 N2 126.4(3) . . ?
O1 C1 N1 124.8(3) . . ?
N2 C1 N1 108.6(3) . . ?
N1 C2 N3 113.6(3) . . ?
N1 C2 C19 111.7(3) . . ?
N3 C2 C19 111.1(3) . . ?
N1 C2 C3 102.2(3) . . ?
N3 C2 C3 102.0(3) . . ?
C19 C2 C3 115.6(3) . . ?
N4 C3 N2 112.5(3) . . ?
N4 C3 C20 113.2(3) . . ?
N2 C3 C20 111.7(3) . . ?
N4 C3 C2 102.1(3) . . ?
N2 C3 C2 102.1(3) . . ?
C20 C3 C2 114.3(3) . . ?
O4 C4 N4 126.2(4) . . ?
O4 C4 N3 125.3(4) . . ?
N4 C4 N3 108.5(3) . . ?
N5 C5 N2 114.6(3) . . ?
N5 C5 H5A 108.6 . . ?
N2 C5 H5A 108.6 . . ?
N5 C5 H5B 108.6 . . ?
N2 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N4 C6 N7 115.5(3) . . ?
N4 C6 H6A 108.4 . . ?
N7 C6 H6A 108.4 . . ?
N4 C6 H6B 108.4 . . ?
N7 C6 H6B 108.4 . . ?
H6A C6 H6B 107.5 . . ?
O2 C7 N5 126.2(4) . . ?
O2 C7 N6 125.3(3) . . ?
N5 C7 N6 108.3(3) . . ?
N7 C8 N5 111.5(3) . . ?
N7 C8 C21 113.4(3) . . ?
N5 C8 C21 111.3(3) . . ?
N7 C8 C9 102.5(3) . . ?
N5 C8 C9 102.4(3) . . ?
C21 C8 C9 115.1(3) . . ?
N8 C9 N6 113.6(3) . . ?
N8 C9 C22 111.9(3) . . ?
N6 C9 C22 110.9(3) . . ?
N8 C9 C8 102.5(3) . . ?
N6 C9 C8 102.0(3) . . ?
C22 C9 C8 115.3(3) . . ?
O5 C10 N8 125.6(4) . . ?
O5 C10 N7 126.1(4) . . ?
N8 C10 N7 108.2(3) . . ?
N9 C11 N6 115.1(3) . . ?
N9 C11 H11A 108.5 . . ?
N6 C11 H11A 108.5 . . ?
N9 C11 H11B 108.5 . . ?
N6 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
N11 C12 N8 114.3(3) . . ?
N11 C12 H12A 108.7 . . ?
N8 C12 H12A 108.7 . . ?
N11 C12 H12B 108.7 . . ?
N8 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O3 C13 N9 126.6(3) . . ?
O3 C13 N10 125.1(3) . . ?
N9 C13 N10 108.3(3) . . ?
N9 C14 N11 114.2(3) . . ?
N9 C14 C15 103.8(3) . . ?
N11 C14 C15 102.8(3) . . ?
N9 C14 H14 111.8 . . ?
N11 C14 H14 111.8 . . ?
C15 C14 H14 111.8 . . ?
N10 C15 N12 114.3(3) . . ?
N10 C15 C14 102.8(3) . . ?
N12 C15 C14 103.4(3) . . ?
N10 C15 H15 111.9 . . ?
N12 C15 H15 111.9 . . ?
C14 C15 H15 111.9 . . ?
O6 C16 N12 126.0(3) . . ?
O6 C16 N11 126.3(3) . . ?
N12 C16 N11 107.7(3) . . ?
N10 C17 N3 114.6(3) . 3_657 ?
N10 C17 H17A 108.6 . . ?
N3 C17 H17A 108.6 3_657 . ?
N10 C17 H17B 108.6 . . ?
N3 C17 H17B 108.6 3_657 . ?
H17A C17 H17B 107.6 . . ?
N1 C18 N12 114.6(3) . 3_657 ?
N1 C18 H18A 108.6 . . ?
N12 C18 H18A 108.6 3_657 . ?
N1 C18 H18B 108.6 . . ?
N12 C18 H18B 108.6 3_657 . ?
H18A C18 H18B 107.6 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 H20A 109.5 . . ?
C3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C22 H22A 109.5 . . ?
C9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C18 121.2(3) . . ?
C1 N1 C2 113.4(3) . . ?
C18 N1 C2 125.4(3) . . ?
C1 N2 C5 119.7(3) . . ?
C1 N2 C3 113.6(3) . . ?
C5 N2 C3 125.9(3) . . ?
C4 N3 C17 121.1(3) . 3_657 ?
C4 N3 C2 113.4(3) . . ?
C17 N3 C2 125.5(3) 3_657 . ?
C4 N4 C6 119.9(3) . . ?
C4 N4 C3 114.0(3) . . ?
C6 N4 C3 125.9(3) . . ?
C7 N5 C5 120.3(3) . . ?
C7 N5 C8 113.5(3) . . ?
C5 N5 C8 125.9(3) . . ?
C7 N6 C11 120.6(3) . . ?
C7 N6 C9 113.6(3) . . ?
C11 N6 C9 125.8(3) . . ?
C10 N7 C6 119.4(3) . . ?
C10 N7 C8 113.4(3) . . ?
C6 N7 C8 126.1(3) . . ?
C10 N8 C12 120.2(3) . . ?
C10 N8 C9 113.2(3) . . ?
C12 N8 C9 126.5(3) . . ?
C13 N9 C11 122.9(3) . . ?
C13 N9 C14 112.4(3) . . ?
C11 N9 C14 122.7(3) . . ?
C13 N10 C17 122.9(3) . . ?
C13 N10 C15 112.6(3) . . ?
C17 N10 C15 123.5(3) . . ?
C16 N11 C12 123.1(3) . . ?
C16 N11 C14 112.6(3) . . ?
C12 N11 C14 121.5(3) . . ?
C16 N12 C18 123.4(3) . 3_657 ?
C16 N12 C15 112.7(3) . . ?
C18 N12 C15 122.1(3) 3_657 . ?
C1 O1 Na1 143.3(3) . . ?
C7 O2 Na1 141.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.125

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 1.000 69 9 ' '
2 0.500 0.500 0.500 69 9 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex1
_database_code_depnum_ccdc_archive 'CCDC 1519707'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_publ_requested_journal_name     'Eur. J. Inorg. Chem.'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 N24 O12, Cd2 Cl7, 3(H3 O), 10(H2 O)'
_chemical_formula_sum            'C44 H81 Cd2 Cl7 N24 O25'
_chemical_formula_weight         1819.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 2/n'
_symmetry_space_group_name_Hall  '-P 2yac'

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

_cell_length_a                   12.3158(7)
_cell_length_b                   16.9613(9)
_cell_length_c                   16.6577(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.410(2)
_cell_angle_gamma                90.00
_cell_volume                     3457.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7778
_exptl_absorpt_correction_T_max  0.8281
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30888
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         27.57
_reflns_number_total             7980
_reflns_number_gt                5870
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.0926P)²+9.8750P] 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         7980
_refine_ls_number_parameters     402
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.1763
_refine_ls_wR_factor_gt          0.1647
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.035
_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 0.94553(3) 0.32061(2) 1.22325(2) 0.01686(13) Uani 1 1 d . . .
Cl1 Cl 1.02352(11) 0.18977(7) 1.23638(7) 0.0151(3) Uani 1 1 d . . .
Cl2 Cl 0.91454(14) 0.36338(9) 1.08251(9) 0.0282(4) Uani 1 1 d . . .
Cl3 Cl 1.01716(15) 0.41577(10) 1.32254(11) 0.0406(5) Uani 1 1 d . . .
Cl4 Cl 0.7500 0.29665(15) 1.2500 0.0550(9) Uani 1 2 d S . .
C1 C 1.3929(4) 0.3222(3) 0.9885(3) 0.0111(10) Uani 1 1 d . . .
C2 C 1.2226(4) 0.3861(3) 0.9926(3) 0.0117(10) Uani 1 1 d . . .
C3 C 1.2263(4) 0.3065(3) 1.0438(3) 0.0118(10) Uani 1 1 d . . .
C4 C 1.0861(4) 0.2975(3) 0.9357(3) 0.0107(10) Uani 1 1 d . . .
C5 C 1.3765(4) 0.2016(3) 1.0661(3) 0.0097(10) Uani 1 1 d . . .
H5A H 1.3612 0.2009 1.1226 0.012 Uiso 1 1 calc R . .
H5B H 1.4561 0.2031 1.0660 0.012 Uiso 1 1 calc R . .
C6 C 1.0896(4) 0.1913(3) 1.0367(3) 0.0086(10) Uani 1 1 d . . .
H6A H 1.0994 0.1948 1.0958 0.010 Uiso 1 1 calc R . .
H6B H 1.0109 0.1899 1.0194 0.010 Uiso 1 1 calc R . .
C7 C 1.3895(4) 0.0944(3) 0.9708(3) 0.0094(10) Uani 1 1 d . . .
C8 C 1.2413(4) 0.0844(3) 1.0481(3) 0.0087(10) Uani 1 1 d . . .
C9 C 1.2499(4) 0.0055(3) 0.9985(3) 0.0106(10) Uani 1 1 d . . .
C10 C 1.0838(4) 0.0707(3) 0.9556(3) 0.0101(10) Uani 1 1 d U . .
C11 C 1.3962(4) -0.0343(3) 0.9043(3) 0.0111(10) Uani 1 1 d . . .
H11A H 1.4733 -0.0195 0.9061 0.013 Uiso 1 1 calc R . .
H11B H 1.3930 -0.0862 0.9296 0.013 Uiso 1 1 calc R . .
C12 C 1.1079(4) -0.0544(3) 0.8880(3) 0.0134(11) Uani 1 1 d . . .
H12A H 1.1279 -0.1065 0.9104 0.016 Uiso 1 1 calc R . .
H12B H 1.0281 -0.0523 0.8778 0.016 Uiso 1 1 calc R . .
C13 C 1.0926(4) -0.0222(3) 0.7428(3) 0.0092(10) Uani 1 1 d U . .
C14 C 1.2524(4) -0.0857(3) 0.7964(3) 0.0089(10) Uani 1 1 d . . .
H14 H 1.2567 -0.1398 0.8188 0.011 Uiso 1 1 calc R . .
C15 C 1.2426(4) 0.4806(3) 0.7955(3) 0.0084(10) Uani 1 1 d . . .
H15 H 1.2359 0.5347 0.8167 0.010 Uiso 1 1 calc R . .
C16 C 1.4045(4) 0.4169(3) 0.7793(3) 0.0071(9) Uani 1 1 d U . .
C17 C 1.0863(4) 0.4243(3) 0.8682(3) 0.0098(10) Uani 1 1 d . . .
H17A H 1.0109 0.4077 0.8518 0.012 Uiso 1 1 calc R . .
H17B H 1.0835 0.4750 0.8961 0.012 Uiso 1 1 calc R . .
C18 C 1.3741(4) 0.4492(3) 0.9191(3) 0.0110(10) Uani 1 1 d . . .
H18A H 1.4541 0.4473 0.9269 0.013 Uiso 1 1 calc R . .
H18B H 1.3515 0.5009 0.9375 0.013 Uiso 1 1 calc R . .
C19 C 1.1943(5) 0.4603(3) 1.0377(3) 0.0209(12) Uani 1 1 d . . .
H19A H 1.1207 0.4558 1.0528 0.031 Uiso 1 1 calc R . .
H19B H 1.1987 0.5059 1.0031 0.031 Uiso 1 1 calc R . .
H19C H 1.2455 0.4664 1.0860 0.031 Uiso 1 1 calc R . .
C20 C 1.2190(5) 0.3189(4) 1.1339(3) 0.0189(12) Uani 1 1 d . . .
H20A H 1.1485 0.3414 1.1414 0.028 Uiso 1 1 calc R . .
H20B H 1.2766 0.3545 1.1557 0.028 Uiso 1 1 calc R . .
H20C H 1.2274 0.2686 1.1616 0.028 Uiso 1 1 calc R . .
C21 C 1.2434(4) 0.0721(3) 1.1400(3) 0.0138(11) Uani 1 1 d . . .
H21A H 1.1796 0.0421 1.1509 0.021 Uiso 1 1 calc R . .
H21B H 1.2428 0.1229 1.1666 0.021 Uiso 1 1 calc R . .
H21C H 1.3090 0.0435 1.1602 0.021 Uiso 1 1 calc R . .
C22 C 1.2675(4) -0.0697(3) 1.0470(3) 0.0139(11) Uani 1 1 d . . .
H22A H 1.3377 -0.0675 1.0797 0.021 Uiso 1 1 calc R . .
H22B H 1.2660 -0.1144 1.0107 0.021 Uiso 1 1 calc R . .
H22C H 1.2099 -0.0753 1.0819 0.021 Uiso 1 1 calc R . .
N1 N 1.3318(3) 0.3890(3) 0.9683(2) 0.0107(9) Uani 1 1 d . . .
N2 N 1.3313(3) 0.2726(2) 1.0290(2) 0.0093(8) Uani 1 1 d . . .
N3 N 1.1381(3) 0.3667(2) 0.9243(2) 0.0099(9) Uani 1 1 d . . .
N4 N 1.1353(3) 0.2615(2) 1.0037(3) 0.0097(8) Uani 1 1 d . . .
N5 N 1.3364(3) 0.1293(2) 1.0283(2) 0.0091(8) Uani 1 1 d . . .
N6 N 1.3416(3) 0.0225(2) 0.9515(2) 0.0078(8) Uani 1 1 d . . .
N7 N 1.1379(3) 0.1186(2) 1.0126(2) 0.0101(9) Uani 1 1 d . . .
N8 N 1.1443(3) 0.0050(2) 0.9475(2) 0.0094(9) Uani 1 1 d . . .
N9 N 1.3510(3) -0.0405(2) 0.8211(2) 0.0085(8) Uani 1 1 d U . .
N10 N 1.1528(3) -0.0458(2) 0.8125(2) 0.0102(9) Uani 1 1 d . . .
N11 N 1.1411(3) 0.4355(2) 0.7964(2) 0.0103(9) Uani 1 1 d . . .
N12 N 1.3373(3) 0.4409(2) 0.8334(2) 0.0102(9) Uani 1 1 d . . .
O1 O 1.4866(3) 0.3114(2) 0.9746(2) 0.0136(8) Uani 1 1 d . . .
O2 O 1.4700(3) 0.1204(2) 0.9432(2) 0.0112(7) Uani 1 1 d . . .
O3 O 1.0037(3) 0.0104(2) 0.7375(2) 0.0146(8) Uani 1 1 d . . .
O4 O 0.9935(3) 0.0835(2) 0.9197(2) 0.0101(7) Uani 1 1 d U . .
O5 O 1.0071(3) 0.2719(2) 0.8923(2) 0.0111(7) Uani 1 1 d . . .
O6 O 1.4916(3) 0.3821(2) 0.7953(2) 0.0134(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 Cl3 2.4068(17) . ?
Cd1 Cl1 2.4185(13) . ?
Cd1 Cl2 2.4431(15) . ?
Cd1 Cl4 2.5303(6) . ?
Cl4 Cd1 2.5303(6) 2_657 ?
C1 O1 1.215(6) . ?
C1 N2 1.361(6) . ?
C1 N1 1.380(7) . ?
C2 N1 1.448(7) . ?
C2 N3 1.489(6) . ?
C2 C19 1.527(7) . ?
C2 C3 1.594(7) . ?
C3 N4 1.456(6) . ?
C3 N2 1.461(6) . ?
C3 C20 1.527(7) . ?
C4 O5 1.226(6) . ?
C4 N3 1.360(7) . ?
C4 N4 1.367(6) . ?
C5 N2 1.438(6) . ?
C5 N5 1.440(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N7 1.445(6) . ?
C6 N4 1.451(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.221(6) . ?
C7 N5 1.355(6) . ?
C7 N6 1.377(6) . ?
C8 N7 1.462(6) . ?
C8 N5 1.466(6) . ?
C8 C21 1.543(7) . ?
C8 C9 1.583(7) . ?
C9 N8 1.472(6) . ?
C9 N6 1.472(6) . ?
C9 C22 1.512(7) . ?
C10 O4 1.222(6) . ?
C10 N8 1.356(6) . ?
C10 N7 1.365(6) . ?
C11 N9 1.438(6) . ?
C11 N6 1.454(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N10 1.436(7) . ?
C12 N8 1.449(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.221(6) . ?
C13 N10 1.366(6) . ?
C13 N9 1.371(6) 2_756 ?
C14 N10 1.452(6) . ?
C14 N9 1.456(6) . ?
C14 C14 1.540(9) 2_756 ?
C14 H14 0.9900 . ?
C15 N12 1.431(6) . ?
C15 N11 1.467(6) . ?
C15 C15 1.546(9) 2_756 ?
C15 H15 0.9900 . ?
C16 O6 1.227(6) . ?
C16 N12 1.353(6) . ?
C16 N11 1.359(6) 2_756 ?
C17 N11 1.449(6) . ?
C17 N3 1.449(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N1 1.442(6) . ?
C18 N12 1.455(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
N9 C13 1.371(6) 2_756 ?
N11 C16 1.359(6) 2_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl3 Cd1 Cl1 116.22(5) . . ?
Cl3 Cd1 Cl2 117.80(6) . . ?
Cl1 Cd1 Cl2 112.16(5) . . ?
Cl3 Cd1 Cl4 105.65(6) . . ?
Cl1 Cd1 Cl4 102.29(7) . . ?
Cl2 Cd1 Cl4 99.61(5) . . ?
Cd1 Cl4 Cd1 161.52(12) . 2_657 ?
O1 C1 N2 126.5(5) . . ?
O1 C1 N1 125.5(5) . . ?
N2 C1 N1 107.9(4) . . ?
N1 C2 N3 112.7(4) . . ?
N1 C2 C19 112.3(4) . . ?
N3 C2 C19 112.3(4) . . ?
N1 C2 C3 101.9(4) . . ?
N3 C2 C3 101.4(4) . . ?
C19 C2 C3 115.4(4) . . ?
N4 C3 N2 111.5(4) . . ?
N4 C3 C20 113.3(4) . . ?
N2 C3 C20 111.7(4) . . ?
N4 C3 C2 102.9(4) . . ?
N2 C3 C2 102.5(4) . . ?
C20 C3 C2 114.1(4) . . ?
O5 C4 N3 125.4(5) . . ?
O5 C4 N4 125.4(5) . . ?
N3 C4 N4 109.2(4) . . ?
N2 C5 N5 115.3(4) . . ?
N2 C5 H5A 108.4 . . ?
N5 C5 H5A 108.4 . . ?
N2 C5 H5B 108.4 . . ?
N5 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
N7 C6 N4 114.0(4) . . ?
N7 C6 H6A 108.8 . . ?
N4 C6 H6A 108.8 . . ?
N7 C6 H6B 108.8 . . ?
N4 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
O2 C7 N5 125.8(5) . . ?
O2 C7 N6 125.2(5) . . ?
N5 C7 N6 108.9(4) . . ?
N7 C8 N5 112.6(4) . . ?
N7 C8 C21 111.8(4) . . ?
N5 C8 C21 111.6(4) . . ?
N7 C8 C9 103.3(4) . . ?
N5 C8 C9 102.8(4) . . ?
C21 C8 C9 114.1(4) . . ?
N8 C9 N6 112.1(4) . . ?
N8 C9 C22 111.6(4) . . ?
N6 C9 C22 112.1(4) . . ?
N8 C9 C8 101.5(4) . . ?
N6 C9 C8 102.2(4) . . ?
C22 C9 C8 116.6(4) . . ?
O4 C10 N8 125.2(5) . . ?
O4 C10 N7 125.6(5) . . ?
N8 C10 N7 109.1(4) . . ?
N9 C11 N6 114.7(4) . . ?
N9 C11 H11A 108.6 . . ?
N6 C11 H11A 108.6 . . ?
N9 C11 H11B 108.6 . . ?
N6 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
N10 C12 N8 114.1(4) . . ?
N10 C12 H12A 108.7 . . ?
N8 C12 H12A 108.7 . . ?
N10 C12 H12B 108.7 . . ?
N8 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O3 C13 N10 126.3(5) . . ?
O3 C13 N9 125.0(5) . 2_756 ?
N10 C13 N9 108.7(4) . 2_756 ?
N10 C14 N9 113.4(4) . . ?
N10 C14 C14 104.3(4) . 2_756 ?
N9 C14 C14 102.8(4) . 2_756 ?
N10 C14 H14 111.9 . . ?
N9 C14 H14 111.9 . . ?
C14 C14 H14 111.9 2_756 . ?
N12 C15 N11 113.8(4) . . ?
N12 C15 C15 104.6(4) . 2_756 ?
N11 C15 C15 101.8(4) . 2_756 ?
N12 C15 H15 112.0 . . ?
N11 C15 H15 112.0 . . ?
C15 C15 H15 112.0 2_756 . ?
O6 C16 N12 125.8(4) . . ?
O6 C16 N11 125.0(4) . 2_756 ?
N12 C16 N11 109.2(4) . 2_756 ?
N11 C17 N3 114.1(4) . . ?
N11 C17 H17A 108.7 . . ?
N3 C17 H17A 108.7 . . ?
N11 C17 H17B 108.7 . . ?
N3 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
N1 C18 N12 113.4(4) . . ?
N1 C18 H18A 108.9 . . ?
N12 C18 H18A 108.9 . . ?
N1 C18 H18B 108.9 . . ?
N12 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 H20A 109.5 . . ?
C3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C22 H22A 109.5 . . ?
C9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C18 119.8(4) . . ?
C1 N1 C2 113.7(4) . . ?
C18 N1 C2 126.1(4) . . ?
C1 N2 C5 121.3(4) . . ?
C1 N2 C3 113.2(4) . . ?
C5 N2 C3 124.4(4) . . ?
C4 N3 C17 119.4(4) . . ?
C4 N3 C2 112.5(4) . . ?
C17 N3 C2 124.3(4) . . ?
C4 N4 C6 121.7(4) . . ?
C4 N4 C3 113.1(4) . . ?
C6 N4 C3 124.6(4) . . ?
C7 N5 C5 120.8(4) . . ?
C7 N5 C8 113.1(4) . . ?
C5 N5 C8 126.0(4) . . ?
C7 N6 C11 120.0(4) . . ?
C7 N6 C9 112.6(4) . . ?
C11 N6 C9 125.9(4) . . ?
C10 N7 C6 121.1(4) . . ?
C10 N7 C8 112.4(4) . . ?
C6 N7 C8 126.4(4) . . ?
C10 N8 C12 120.6(4) . . ?
C10 N8 C9 113.4(4) . . ?
C12 N8 C9 125.7(4) . . ?
C13 N9 C11 123.8(4) 2_756 . ?
C13 N9 C14 112.2(4) 2_756 . ?
C11 N9 C14 122.2(4) . . ?
C13 N10 C12 123.3(4) . . ?
C13 N10 C14 111.7(4) . . ?
C12 N10 C14 122.0(4) . . ?
C16 N11 C17 123.6(4) 2_756 . ?
C16 N11 C15 112.0(4) 2_756 . ?
C17 N11 C15 123.6(4) . . ?
C16 N12 C15 112.1(4) . . ?
C16 N12 C18 122.4(4) . . ?
C15 N12 C18 122.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.076
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.164

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.113 0.735 0.250 407 129 ' '
2 -0.117 0.265 0.750 407 131 ' '
_platon_squeeze_details          
;
;
