# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1564036'
_audit_update_record             
;
2017-09-09 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H80 N24 Ni4 O26 S2'
_chemical_formula_weight         2140.68

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   22.6020(10)
_cell_length_b                   13.6460(10)
_cell_length_c                   17.1630(10)
_cell_angle_alpha                90
_cell_angle_beta                 125.8120(10)
_cell_angle_gamma                90
_cell_volume                     4292.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5445
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_F_000             2208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.010
_shelx_estimated_absorpt_T_min   0.752
_shelx_estimated_absorpt_T_max   0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6045
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11888
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.861
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_full        25.005
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3798
_reflns_number_gt                3399
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0515P)²+10.4258P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3798
_refine_ls_number_parameters     390
_refine_ls_number_restraints     198
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.1044
_refine_ls_wR_factor_gt          0.1008
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.75406(2) -0.01286(3) 0.04068(2) 0.02170(13) Uani 1 1 d . . . . .
S1 S 0.000000 0.41127(8) 0.750000 0.0431(3) Uani 1 2 d S T P . .
O1 O 0.68589(11) -0.12817(16) -0.03617(15) 0.0383(5) Uani 1 1 d . . . . .
H1A H 0.660283 -0.171237 -0.032854 0.046 Uiso 1 1 d R U . . .
H1B H 0.719083 -0.166966 -0.026234 0.046 Uiso 1 1 d R U . . .
O2 O 0.83687(11) 0.07219(16) 0.16476(15) 0.0390(5) Uani 1 1 d . . . . .
O3 O 0.80142(12) -0.06968(16) 0.18210(14) 0.0360(5) Uani 1 1 d . U . . .
O4 O 0.0444(2) 0.3976(4) 0.8680(3) 0.0425(11) Uani 0.5 1 d . . P . .
O5 O 0.0551(2) 0.3664(3) 0.7532(4) 0.1140(16) Uani 1 1 d . . . . .
O6 O 0.000000 0.5183(2) 0.750000 0.0456(8) Uani 1 2 d S T P . .
N1 N 0.56721(12) 0.10877(17) 0.00765(16) 0.0266(5) Uani 1 1 d . . . . .
N2 N 0.67143(13) 0.04774(18) 0.04584(16) 0.0278(5) Uani 1 1 d . . . . .
N3 N 0.32392(12) 0.15119(17) -0.28895(16) 0.0268(5) Uani 1 1 d . . . . .
N4 N 0.27019(12) 0.07603(17) -0.42831(16) 0.0255(5) Uani 1 1 d . . . . .
N5 N 0.39443(12) 0.31382(16) 0.00795(15) 0.0232(5) Uani 1 1 d . . . . .
N6 N 0.33788(12) 0.41524(17) 0.04451(16) 0.0265(5) Uani 1 1 d . . . . .
C1 C 0.49587(15) 0.1515(2) -0.04608(19) 0.0268(6) Uani 1 1 d . . . . .
C2 C 0.47864(15) 0.2109(2) 0.00318(19) 0.0278(6) Uani 1 1 d . . . . .
H2 H 0.513208 0.223755 0.068145 0.033 Uiso 1 1 calc R U . . .
C3 C 0.40958(15) 0.2510(2) -0.04496(19) 0.0240(6) Uani 1 1 d . . . . .
C4 C 0.35711(15) 0.2313(2) -0.14131(19) 0.0259(6) Uani 1 1 d . . . . .
H4A H 0.310057 0.256141 -0.173169 0.031 Uiso 1 1 calc R U . . .
C5 C 0.37723(15) 0.1728(2) -0.18901(19) 0.0260(6) Uani 1 1 d . . . . .
C6 C 0.44624(15) 0.1332(2) -0.1432(2) 0.0287(6) Uani 1 1 d . . . . .
H6 H 0.458877 0.095424 -0.176466 0.034 Uiso 1 1 calc R U . . .
C7 C 0.60843(16) 0.0851(2) -0.0232(2) 0.0339(7) Uani 1 1 d . . . . .
H7 H 0.593831 0.094249 -0.085871 0.041 Uiso 1 1 calc R U . . .
C8 C 0.67055(17) 0.0475(2) 0.1254(2) 0.0360(7) Uani 1 1 d . . . . .
H8 H 0.708255 0.024692 0.185850 0.043 Uiso 1 1 calc R U . . .
C9 C 0.60745(17) 0.0849(2) 0.1032(2) 0.0363(7) Uani 1 1 d . . . . .
H9 H 0.593785 0.092949 0.144440 0.044 Uiso 1 1 calc R U . . .
C10 C 0.32367(15) 0.0715(2) -0.33632(19) 0.0272(6) Uani 1 1 d . . . . .
H10 H 0.357032 0.020336 -0.307420 0.033 Uiso 1 1 calc R U . . .
C11 C 0.23444(16) 0.1623(2) -0.4410(2) 0.0359(7) Uani 1 1 d . . . . .
H11 H 0.193918 0.185036 -0.499357 0.043 Uiso 1 1 calc R U . . .
C12 C 0.26671(17) 0.2092(2) -0.3563(2) 0.0382(7) Uani 1 1 d . . . . .
H12 H 0.252986 0.269138 -0.345606 0.046 Uiso 1 1 calc R U . . .
C13 C 0.44132(16) 0.3325(3) 0.1049(2) 0.0382(8) Uani 1 1 d . . . . .
H13 H 0.487907 0.306924 0.147608 0.046 Uiso 1 1 calc R U . . .
C14 C 0.33313(15) 0.3657(2) -0.0245(2) 0.0293(6) Uani 1 1 d . . . . .
H14 H 0.292410 0.366253 -0.088204 0.035 Uiso 1 1 calc R U . . .
C15 C 0.40664(16) 0.3949(2) 0.1256(2) 0.0366(7) Uani 1 1 d . . . . .
H15 H 0.426214 0.420824 0.186176 0.044 Uiso 1 1 calc R U . . .
C16 C 0.84284(17) 0.0035(2) 0.2178(2) 0.0343(7) Uani 1 1 d . U . . .
C17 C 0.9089(4) 0.0212(5) 0.3206(5) 0.0247(13) Uani 0.5 1 d . U P A 1
C18 C 0.9677(3) 0.0855(5) 0.3485(4) 0.0291(12) Uani 0.5 1 d . U P A 1
H18A H 0.965517 0.124683 0.300469 0.035 Uiso 0.5 1 d R U P A 1
C19 C 1.0261(3) 0.0904(4) 0.4418(4) 0.0280(11) Uani 0.5 1 d . U P A 1
H19A H 1.065519 0.133909 0.459582 0.034 Uiso 0.5 1 d R U P A 1
C20 C 1.030(2) 0.039(2) 0.513(3) 0.023(3) Uani 0.25 1 d . U P A 1
C21 C 0.970(2) -0.0262(19) 0.485(3) 0.022(3) Uani 0.25 1 d . U P A 1
C22 C 0.9110(3) -0.0372(4) 0.3882(4) 0.0237(11) Uani 0.5 1 d . U P A 1
H22 H 0.865366 -0.058602 0.378779 0.028 Uiso 0.5 1 d R U P A 1
C17' C 0.8936(4) -0.0102(5) 0.3267(5) 0.0294(14) Uani 0.5 1 d . U P A 2
C18' C 0.9536(4) 0.0465(5) 0.3723(5) 0.0361(13) Uani 0.5 1 d . U P A 2
H18' H 0.961715 0.091433 0.338673 0.043 Uiso 0.5 1 d R U P A 2
C19' C 1.0116(14) 0.0444(15) 0.4739(19) 0.031(3) Uani 0.25 1 d . U P A 2
C20' C 0.9965(13) -0.0246(16) 0.5222(19) 0.030(3) Uani 0.25 1 d . U P A 2
C21' C 0.9290(4) -0.0896(5) 0.4746(5) 0.0417(14) Uani 0.5 1 d . U P A 2
H21' H 0.920943 -0.134535 0.508189 0.050 Uiso 0.5 1 d R U P A 2
C22' C 0.8809(4) -0.0802(5) 0.3774(5) 0.0347(13) Uani 0.5 1 d . U P A 2
H22' H 0.839370 -0.119316 0.344718 0.042 Uiso 0.5 1 d R U P A 2
O1W O 0.18058(16) 0.2752(2) 0.8074(2) 0.0751(9) Uani 1 1 d . . . . .
H1WA H 0.182861 0.212958 0.807997 0.090 Uiso 1 1 d R U . . .
H1WB H 0.151021 0.293648 0.819876 0.090 Uiso 1 1 d R U . . .
O2W O 0.9242(4) 0.2194(6) 0.1649(4) 0.091(2) Uani 0.5 1 d D . P . .
H2WA H 0.956607 0.271955 0.201227 0.137 Uiso 0.5 1 d DR U P . .
H2WB H 0.903140 0.164948 0.175126 0.137 Uiso 0.5 1 d DR U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.052(2) . ?
Ni1 N4 2.062(2) 2_654 ?
Ni1 N2 2.091(2) . ?
Ni1 N6 2.100(2) 3_545 ?
Ni1 O3 2.144(2) . ?
Ni1 O2 2.173(2) . ?
S1 O5 1.358(3) 2_556 ?
S1 O5 1.358(3) . ?
S1 O6 1.461(3) . ?
S1 O4 1.663(4) . ?
S1 O4 1.663(4) 2_556 ?
O1 H1A 0.8499 . ?
O1 H1B 0.8499 . ?
O2 C16 1.258(4) . ?
O3 C16 1.256(4) . ?
N1 C7 1.353(4) . ?
N1 C9 1.370(4) . ?
N1 C1 1.432(3) . ?
N2 C7 1.311(4) . ?
N2 C8 1.377(4) . ?
N3 C10 1.356(4) . ?
N3 C12 1.374(4) . ?
N3 C5 1.436(3) . ?
N4 C10 1.313(4) . ?
N4 C11 1.372(4) . ?
N5 C14 1.352(4) . ?
N5 C13 1.376(4) . ?
N5 C3 1.429(3) . ?
N6 C14 1.312(4) . ?
N6 C15 1.378(4) . ?
C1 C6 1.382(4) . ?
C1 C2 1.381(4) . ?
C2 C3 1.382(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(4) . ?
C4 C5 1.396(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.381(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.343(4) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.346(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C15 1.337(4) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.523(7) . ?
C16 C17' 1.528(8) . ?
C17 C22 1.385(9) . ?
C17 C18 1.422(10) . ?
C18 C19 1.355(8) . ?
C18 H18A 0.9599 . ?
C19 C20 1.37(4) . ?
C19 C21 1.49(3) 5_756 ?
C19 H19A 0.9600 . ?
C20 C21 0.17(5) 5_756 ?
C20 C22 1.42(5) 5_756 ?
C20 C21 1.444(19) . ?
C20 C20 1.55(7) 5_756 ?
C21 C21 1.35(8) 5_756 ?
C21 C22 1.41(4) . ?
C22 H22 0.9892 . ?
C17' C18' 1.345(10) . ?
C17' C22' 1.429(11) . ?
C18' C19' 1.44(3) . ?
C18' C20' 1.50(3) 5_756 ?
C18' H18' 0.9301 . ?
C19' C20' 0.35(4) 5_756 ?
C19' C21' 1.25(3) 5_756 ?
C19' C20' 1.42(3) . ?
C19' C19' 1.76(4) 5_756 ?
C20' C20' 1.09(5) 5_756 ?
C20' C21' 1.52(2) . ?
C21' C22' 1.364(9) . ?
C21' H21' 0.9300 . ?
C22' H22' 0.9302 . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8499 . ?
O2W H2WA 0.9510 . ?
O2W H2WB 0.9527 . ?

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 Ni1 N4 99.27(9) . 2_654 ?
O1 Ni1 N2 88.69(9) . . ?
N4 Ni1 N2 92.96(9) 2_654 . ?
O1 Ni1 N6 89.21(9) . 3_545 ?
N4 Ni1 N6 92.60(9) 2_654 3_545 ?
N2 Ni1 N6 174.30(9) . 3_545 ?
O1 Ni1 O3 98.05(9) . . ?
N4 Ni1 O3 162.67(9) 2_654 . ?
N2 Ni1 O3 87.81(8) . . ?
N6 Ni1 O3 87.24(8) 3_545 . ?
O1 Ni1 O2 158.71(9) . . ?
N4 Ni1 O2 101.98(9) 2_654 . ?
N2 Ni1 O2 91.47(9) . . ?
N6 Ni1 O2 88.56(9) 3_545 . ?
O3 Ni1 O2 60.69(9) . . ?
O5 S1 O5 126.5(3) 2_556 . ?
O5 S1 O6 116.77(16) 2_556 . ?
O5 S1 O6 116.77(16) . . ?
O5 S1 O4 83.4(3) 2_556 . ?
O5 S1 O4 90.8(3) . . ?
O6 S1 O4 96.42(18) . . ?
O5 S1 O4 90.8(3) 2_556 2_556 ?
O5 S1 O4 83.4(3) . 2_556 ?
O6 S1 O4 96.42(18) . 2_556 ?
O4 S1 O4 167.2(4) . 2_556 ?
Ni1 O1 H1A 140.5 . . ?
Ni1 O1 H1B 96.1 . . ?
H1A O1 H1B 96.4 . . ?
C16 O2 Ni1 88.68(19) . . ?
C16 O3 Ni1 90.02(18) . . ?
C7 N1 C9 106.6(2) . . ?
C7 N1 C1 128.2(2) . . ?
C9 N1 C1 125.2(2) . . ?
C7 N2 C8 105.0(2) . . ?
C7 N2 Ni1 129.79(19) . . ?
C8 N2 Ni1 124.92(19) . . ?
C10 N3 C12 106.6(2) . . ?
C10 N3 C5 126.0(2) . . ?
C12 N3 C5 127.3(2) . . ?
C10 N4 C11 105.8(2) . . ?
C10 N4 Ni1 130.6(2) . 2_654 ?
C11 N4 Ni1 123.17(18) . 2_654 ?
C14 N5 C13 106.2(2) . . ?
C14 N5 C3 128.4(2) . . ?
C13 N5 C3 125.4(2) . . ?
C14 N6 C15 104.8(2) . . ?
C14 N6 Ni1 128.05(19) . 3_455 ?
C15 N6 Ni1 126.16(18) . 3_455 ?
C6 C1 C2 121.6(3) . . ?
C6 C1 N1 121.1(2) . . ?
C2 C1 N1 117.3(2) . . ?
C1 C2 C3 119.4(2) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C2 C3 C4 121.0(2) . . ?
C2 C3 N5 117.7(2) . . ?
C4 C3 N5 121.3(2) . . ?
C3 C4 C5 117.8(3) . . ?
C3 C4 H4A 121.1 . . ?
C5 C4 H4A 121.1 . . ?
C6 C5 C4 122.4(2) . . ?
C6 C5 N3 118.6(2) . . ?
C4 C5 N3 119.0(2) . . ?
C1 C6 C5 117.7(2) . . ?
C1 C6 H6 121.1 . . ?
C5 C6 H6 121.1 . . ?
N2 C7 N1 111.8(2) . . ?
N2 C7 H7 124.1 . . ?
N1 C7 H7 124.1 . . ?
C9 C8 N2 110.3(3) . . ?
C9 C8 H8 124.9 . . ?
N2 C8 H8 124.9 . . ?
C8 C9 N1 106.3(3) . . ?
C8 C9 H9 126.8 . . ?
N1 C9 H9 126.8 . . ?
N4 C10 N3 111.2(2) . . ?
N4 C10 H10 124.4 . . ?
N3 C10 H10 124.4 . . ?
C12 C11 N4 109.9(3) . . ?
C12 C11 H11 125.0 . . ?
N4 C11 H11 125.0 . . ?
C11 C12 N3 106.4(3) . . ?
C11 C12 H12 126.8 . . ?
N3 C12 H12 126.8 . . ?
C15 C13 N5 106.4(2) . . ?
C15 C13 H13 126.8 . . ?
N5 C13 H13 126.8 . . ?
N6 C14 N5 112.0(2) . . ?
N6 C14 H14 124.0 . . ?
N5 C14 H14 124.0 . . ?
C13 C15 N6 110.5(3) . . ?
C13 C15 H15 124.7 . . ?
N6 C15 H15 124.7 . . ?
O3 C16 O2 120.4(3) . . ?
O3 C16 C17 129.6(4) . . ?
O2 C16 C17 109.7(4) . . ?
O3 C16 C17' 108.1(4) . . ?
O2 C16 C17' 131.4(4) . . ?
C22 C17 C18 120.4(6) . . ?
C22 C17 C16 114.2(6) . . ?
C18 C17 C16 125.3(6) . . ?
C19 C18 C17 120.1(6) . . ?
C19 C18 H18A 120.8 . . ?
C17 C18 H18A 119.1 . . ?
C20 C19 C18 122.5(19) . . ?
C20 C19 C21 5(2) . 5_756 ?
C18 C19 C21 120.2(18) . 5_756 ?
C20 C19 H19A 118.3 . . ?
C18 C19 H19A 119.2 . . ?
C21 C19 H19A 120.6 5_756 . ?
C21 C20 C22 83(10) 5_756 5_756 ?
C19 C20 C22 126(3) . 5_756 ?
C19 C20 C21 118(2) . . ?
C22 C20 C21 115.8(16) 5_756 . ?
C19 C20 C20 120(5) . 5_756 ?
C22 C20 C20 113(4) 5_756 5_756 ?
C21 C20 C20 5(2) . 5_756 ?
C20 C21 C22 90(10) 5_756 . ?
C21 C21 C22 123(4) 5_756 . ?
C21 C21 C20 6(3) 5_756 . ?
C22 C21 C20 120.9(19) . . ?
C20 C21 C19 47(10) 5_756 5_756 ?
C21 C21 C19 116(4) 5_756 5_756 ?
C22 C21 C19 119(3) . 5_756 ?
C20 C21 C19 119.9(16) . 5_756 ?
C17 C22 C21 118.4(16) . . ?
C17 C22 C20 123.6(16) . 5_756 ?
C21 C22 C20 7(2) . 5_756 ?
C17 C22 H22 120.7 . . ?
C21 C22 H22 113.6 . . ?
C20 C22 H22 111.0 5_756 . ?
C18' C17' C22' 121.5(7) . . ?
C18' C17' C16 114.9(7) . . ?
C22' C17' C16 123.5(6) . . ?
C17' C18' C19' 125.8(11) . . ?
C17' C18' H18' 121.0 . . ?
C19' C18' H18' 113.2 . . ?
C20' C18' H18' 126.8 5_756 . ?
C20' C19' C21' 135(9) 5_756 5_756 ?
C20' C19' C20' 20(8) 5_756 . ?
C21' C19' C20' 116.0(17) 5_756 . ?
C20' C19' C18' 92(9) 5_756 . ?
C21' C19' C18' 132.9(18) 5_756 . ?
C20' C19' C18' 111.1(13) . . ?
C19' C20' C19' 160(8) 5_756 . ?
C20' C20' C19' 6(2) 5_756 . ?
C19' C20' C21' 36(7) 5_756 . ?
C20' C20' C21' 119(3) 5_756 . ?
C19' C20' C21' 125.4(12) . . ?
C18' C20' C21' 109.9(16) 5_756 . ?
C19' C21' C22' 125.0(13) 5_756 . ?
C19' C21' C20' 9.6(18) 5_756 . ?
C22' C21' C20' 115.6(12) . . ?
C19' C21' H21' 113.9 5_756 . ?
C22' C21' H21' 121.0 . . ?
C20' C21' H21' 123.3 . . ?
C21' C22' C17' 120.5(7) . . ?
C21' C22' H22' 119.0 . . ?
C17' C22' H22' 120.5 . . ?
H1WA O1W H1WB 110.2 . . ?
H2WA O2W H2WB 138.1 . . ?

_refine_diff_density_max         0.755
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.066

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1564034'
_audit_update_record             
;
2017-09-09 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H42 Cd2 N12 O14 S'
_chemical_formula_sum            'C42 H42 Cd2 N12 O14 S'
_chemical_formula_weight         1195.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   23.6468(18)
_cell_length_b                   13.2610(10)
_cell_length_c                   17.991(2)
_cell_angle_alpha                90
_cell_angle_beta                 126.7580(10)
_cell_angle_gamma                90
_cell_volume                     4519.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7082
_cell_measurement_theta_min      2.7075
_cell_measurement_theta_max      27.5354

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_F_000             2408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.070
_shelx_estimated_absorpt_T_min   0.754
_shelx_estimated_absorpt_T_max   0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6330
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12400
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.874
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_full        25.004
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3984
_reflns_number_gt                3592
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0196P)²+5.3298P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3984
_refine_ls_number_parameters     420
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0502
_refine_ls_wR_factor_gt          0.0483
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.24925(2) 0.49319(2) 0.46255(2) 0.02822(6) Uani 1 1 d D . . . .
N1 N 0.33772(9) 0.55124(16) 0.45711(12) 0.0361(4) Uani 1 1 d . . . . .
N2 N 0.43847(9) 0.60918(14) 0.49357(11) 0.0296(4) Uani 1 1 d . . . . .
N3 N 0.72578(9) 0.59707(15) 0.91979(12) 0.0331(4) Uani 1 1 d . . . . .
N4 N 0.67289(9) 0.66477(13) 0.78137(11) 0.0289(4) Uani 1 1 d . . . . .
N5 N 0.65913(9) 0.91427(15) 0.45473(12) 0.0355(4) Uani 1 1 d . . . . .
N6 N 0.60476(9) 0.81219(13) 0.48969(11) 0.0293(4) Uani 1 1 d . . . . .
O1 O 0.1580(4) 0.5658(5) 0.3142(3) 0.0392(11) Uani 0.786(6) 1 d D . P A 1
O2 O 0.2007(2) 0.4181(3) 0.3122(2) 0.0392(8) Uani 0.786(6) 1 d D . P A 1
O3 O 0.31799(10) 0.35730(16) 0.54350(14) 0.0585(5) Uani 1 1 d D . . . .
H3A H 0.3118(14) 0.333(2) 0.5803(17) 0.070 Uiso 1 1 d D U . . .
H3B H 0.3616(9) 0.370(2) 0.5788(17) 0.070 Uiso 1 1 d D U . . .
O4 O 0.500000 0.53869(19) 0.750000 0.0514(6) Uani 1 2 d S T P B .
O5 O 0.4613(2) 0.3836(4) 0.7755(3) 0.0532(11) Uani 0.5 1 d . . P B 1
O6 O 0.45633(19) 0.4075(3) 0.6390(2) 0.0538(9) Uani 0.5 1 d . . P B .
O5' O 0.5676(2) 0.3874(4) 0.7838(4) 0.0744(15) Uani 0.5 1 d . . P B 2
O1W O 0.32117(14) 0.2875(2) 0.69630(18) 0.0875(8) Uani 1 1 d D . . . .
H1WC H 0.318(2) 0.2267(13) 0.709(3) 0.105 Uiso 1 1 d D U . . .
H1WB H 0.3656(6) 0.294(3) 0.731(2) 0.105 Uiso 1 1 d D U . . .
O2W O 0.07528(16) 0.7129(2) 0.3358(2) 0.1124(10) Uani 0.786(6) 1 d . . P A 1
H2WD H 0.100901 0.670376 0.332831 0.135 Uiso 0.786(6) 1 d R U P A 1
H2WA H 0.044341 0.735916 0.279861 0.169 Uiso 0.786(6) 1 d R U P A 1
O2W' O 0.07528(16) 0.7129(2) 0.3358(2) 0.1124(10) Uani 0.214(6) 1 d . . P A 2
H2WF H 0.098941 0.670866 0.328471 0.135 Uiso 0.214(6) 1 d R U P A 2
H2WE H 0.042991 0.738316 0.281481 0.169 Uiso 0.214(6) 1 d R U P A 2
S1 S 0.500000 0.42875(7) 0.750000 0.0453(2) Uani 1 2 d S T P . .
C1 C 0.52372(11) 0.70924(17) 0.49538(14) 0.0310(5) Uani 1 1 d . . . . .
H1 H 0.490595 0.718376 0.431773 0.037 Uiso 1 1 calc R U . . .
C2 C 0.50718(10) 0.65345(16) 0.54447(14) 0.0282(5) Uani 1 1 d . . . . .
C3 C 0.55457(11) 0.64054(17) 0.63938(14) 0.0301(5) Uani 1 1 d . . . . .
H3 H 0.542026 0.605622 0.672353 0.036 Uiso 1 1 calc R U . . .
C4 C 0.62152(11) 0.68151(16) 0.68374(14) 0.0277(4) Uani 1 1 d . . . . .
C5 C 0.64040(11) 0.73609(16) 0.63589(14) 0.0295(5) Uani 1 1 d . . . . .
H5 H 0.685817 0.761737 0.666398 0.035 Uiso 1 1 calc R U . . .
C6 C 0.59011(11) 0.75149(16) 0.54175(14) 0.0277(4) Uani 1 1 d . . . . .
C7 C 0.39904(12) 0.5899(2) 0.52335(16) 0.0423(6) Uani 1 1 d . . . . .
H7 H 0.413523 0.602494 0.583260 0.051 Uiso 1 1 calc R U . . .
C8 C 0.33765(12) 0.54506(19) 0.38110(15) 0.0380(5) Uani 1 1 d . . . . .
H8 H 0.300731 0.519905 0.323481 0.046 Uiso 1 1 calc R U . . .
C9 C 0.39873(12) 0.58068(19) 0.40201(15) 0.0376(5) Uani 1 1 d . . . . .
H9 H 0.411610 0.585177 0.362373 0.045 Uiso 1 1 calc R U . . .
C10 C 0.67216(11) 0.58983(18) 0.83162(14) 0.0347(5) Uani 1 1 d . . . . .
H10 H 0.638041 0.539494 0.806938 0.042 Uiso 1 1 calc R U . . .
C11 C 0.76275(12) 0.68095(18) 0.92690(15) 0.0376(5) Uani 1 1 d . . . . .
H11 H 0.803558 0.704911 0.981667 0.045 Uiso 1 1 calc R U . . .
C12 C 0.73113(12) 0.72332(18) 0.84282(15) 0.0374(5) Uani 1 1 d . . . . .
H12 H 0.745699 0.780762 0.828896 0.045 Uiso 1 1 calc R U . . .
C13 C 0.66311(12) 0.86647(18) 0.52131(15) 0.0372(5) Uani 1 1 d . . . . .
H13 H 0.701876 0.869676 0.583419 0.045 Uiso 1 1 calc R U . . .
C14 C 0.59446(12) 0.8892(2) 0.37562(16) 0.0456(6) Uani 1 1 d . . . . .
H14 H 0.576548 0.912688 0.316608 0.055 Uiso 1 1 calc R U . . .
C15 C 0.56051(12) 0.8264(2) 0.39475(16) 0.0476(7) Uani 1 1 d . . . . .
H15 H 0.516128 0.798066 0.352696 0.057 Uiso 1 1 calc R U . . .
C16 C 0.1580(2) 0.4907(4) 0.2718(2) 0.0293(9) Uani 0.786(6) 1 d D . P A 1
C17 C 0.1049(2) 0.4852(4) 0.1678(3) 0.0342(10) Uani 0.786(6) 1 d D . P A 1
C18 C 0.1177(2) 0.4189(3) 0.1182(2) 0.0427(9) Uani 0.786(6) 1 d D . P A 1
H18 H 0.158665 0.380339 0.149486 0.051 Uiso 0.786(6) 1 calc R U P A 1
C19 C 0.06951(17) 0.4111(3) 0.0235(2) 0.0451(10) Uani 0.786(6) 1 d D . P A 1
H19 H 0.078747 0.368273 -0.008986 0.054 Uiso 0.786(6) 1 calc R U P A 1
C20 C -0.0065(2) 0.5331(3) 0.0249(3) 0.0373(10) Uani 0.786(6) 1 d D . P A 1
C21 C 0.0446(2) 0.5420(3) 0.1222(3) 0.0388(9) Uani 0.786(6) 1 d D . P A 1
H21 H 0.037179 0.586882 0.155269 0.047 Uiso 0.786(6) 1 calc R U P A 1
O1A O 0.1518(13) 0.5843(18) 0.3299(10) 0.037(4) Uani 0.214(6) 1 d D . P A 2
O2A O 0.1879(8) 0.4451(11) 0.3030(9) 0.028(3) Uani 0.214(6) 1 d D U P A 2
C16A C 0.1466(7) 0.5214(13) 0.2751(9) 0.019(4) Uani 0.214(6) 1 d D U P A 2
C17A C 0.0855(7) 0.5204(11) 0.1721(9) 0.028(3) Uani 0.214(6) 1 d D . P A 2
C18A C 0.0878(7) 0.4635(11) 0.1092(8) 0.032(3) Uani 0.214(6) 1 d D . P A 2
H18A H 0.126676 0.423181 0.129356 0.039 Uiso 0.214(6) 1 calc R U P A 2
C19A C 0.0291(6) 0.4680(10) 0.0124(8) 0.024(4) Uani 0.214(6) 1 d D U P A 2
C20A C -0.0290(5) 0.5862(9) 0.0537(7) 0.037(3) Uani 0.214(6) 1 d D . P A 2
H20A H -0.067536 0.626423 0.035568 0.044 Uiso 0.214(6) 1 calc R U P A 2
C21A C 0.0278(6) 0.5808(10) 0.1458(7) 0.037(3) Uani 0.214(6) 1 d D . P A 2
H21A H 0.027777 0.616899 0.190086 0.045 Uiso 0.214(6) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O3 2.275(2) . ?
Cd1 N1 2.2854(17) . ?
Cd1 N3 2.2872(18) 2_656 ?
Cd1 N5 2.3017(17) 3_445 ?
Cd1 O1 2.411(4) . ?
Cd1 O2A 2.402(13) . ?
Cd1 O2 2.431(3) . ?
Cd1 O1A 2.426(15) . ?
Cd1 C16A 2.758(12) . ?
N1 C7 1.311(3) . ?
N1 C8 1.369(3) . ?
N2 C7 1.349(3) . ?
N2 C9 1.374(3) . ?
N2 C2 1.429(3) . ?
N3 C10 1.314(3) . ?
N3 C11 1.373(3) . ?
N4 C10 1.350(3) . ?
N4 C12 1.378(3) . ?
N4 C4 1.434(3) . ?
N5 C13 1.308(3) . ?
N5 C14 1.367(3) . ?
N6 C13 1.344(3) . ?
N6 C15 1.382(3) . ?
N6 C6 1.426(2) . ?
O1 C16 1.255(6) . ?
O2 C16 1.263(6) . ?
O3 H3A 0.827(16) . ?
O3 H3B 0.844(17) . ?
O4 S1 1.458(3) . ?
O5 S1 1.381(4) . ?
O5 O6 1.635(6) 2_656 ?
O6 S1 1.632(3) . ?
O6 O5' 1.806(6) 2_656 ?
O5' S1 1.437(4) . ?
O1W H1WC 0.855(10) . ?
O1W H1WB 0.847(10) . ?
O2W H2WD 0.8518 . ?
O2W H2WA 0.8715 . ?
O2W' H2WF 0.8534 . ?
O2W' H2WE 0.8707 . ?
C1 C2 1.376(3) . ?
C1 C6 1.381(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.382(3) . ?
C3 C4 1.388(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(3) . ?
C5 C6 1.383(3) . ?
C5 H5 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.342(3) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.345(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.337(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.507(5) . ?
C17 C21 1.369(5) . ?
C17 C18 1.408(6) . ?
C18 C19 1.373(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.405(5) 5_565 ?
C19 H19 0.9300 . ?
C20 C20 1.413(8) 5_565 ?
C20 C21 1.416(5) . ?
C21 H21 0.9300 . ?
O1A C16A 1.241(15) . ?
O2A C16A 1.281(13) . ?
C16A C17A 1.523(13) . ?
C17A C18A 1.387(14) . ?
C17A C21A 1.398(14) . ?
C18A C19A 1.439(14) . ?
C18A H18A 0.9300 . ?
C19A C20A 1.387(17) 5_565 ?
C19A C19A 1.44(3) 5_565 ?
C20A C21A 1.375(12) . ?
C20A H20A 0.9300 . ?
C21A H21A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cd1 N1 88.43(7) . . ?
O3 Cd1 N3 101.23(7) . 2_656 ?
N1 Cd1 N3 95.79(7) . 2_656 ?
O3 Cd1 N5 87.69(7) . 3_445 ?
N1 Cd1 N5 171.21(7) . 3_445 ?
N3 Cd1 N5 92.70(6) 2_656 3_445 ?
O3 Cd1 O1 148.02(14) . . ?
N1 Cd1 O1 93.1(2) . . ?
N3 Cd1 O1 110.36(13) 2_656 . ?
N5 Cd1 O1 86.1(2) 3_445 . ?
O3 Cd1 O2A 104.1(3) . . ?
N1 Cd1 O2A 87.2(4) . . ?
N3 Cd1 O2A 154.5(3) 2_656 . ?
N5 Cd1 O2A 86.1(4) 3_445 . ?
O3 Cd1 O2 93.94(12) . . ?
N1 Cd1 O2 85.71(11) . . ?
N3 Cd1 O2 164.78(11) 2_656 . ?
N5 Cd1 O2 86.69(11) 3_445 . ?
O1 Cd1 O2 54.42(14) . . ?
O3 Cd1 O1A 156.7(5) . . ?
N1 Cd1 O1A 98.3(8) . . ?
N3 Cd1 O1A 100.2(4) 2_656 . ?
N5 Cd1 O1A 82.3(8) 3_445 . ?
O2A Cd1 O1A 54.4(4) . . ?
O3 Cd1 C16A 131.2(3) . . ?
N1 Cd1 C16A 93.4(4) . . ?
N3 Cd1 C16A 127.0(3) 2_656 . ?
N5 Cd1 C16A 83.2(4) 3_445 . ?
O2A Cd1 C16A 27.7(3) . . ?
O1A Cd1 C16A 26.7(3) . . ?
C7 N1 C8 105.72(18) . . ?
C7 N1 Cd1 129.49(15) . . ?
C8 N1 Cd1 124.66(14) . . ?
C7 N2 C9 106.55(17) . . ?
C7 N2 C2 127.90(18) . . ?
C9 N2 C2 125.52(17) . . ?
C10 N3 C11 105.81(18) . . ?
C10 N3 Cd1 126.99(15) . 2_656 ?
C11 N3 Cd1 127.19(14) . 2_656 ?
C10 N4 C12 106.53(18) . . ?
C10 N4 C4 126.38(18) . . ?
C12 N4 C4 127.06(18) . . ?
C13 N5 C14 104.97(18) . . ?
C13 N5 Cd1 127.44(15) . 3 ?
C14 N5 Cd1 126.29(14) . 3 ?
C13 N6 C15 106.03(17) . . ?
C13 N6 C6 128.01(18) . . ?
C15 N6 C6 125.96(18) . . ?
C16 O1 Cd1 91.7(3) . . ?
C16 O2 Cd1 90.6(2) . . ?
Cd1 O3 H3A 115.3(18) . . ?
Cd1 O3 H3B 113.9(18) . . ?
H3A O3 H3B 101(3) . . ?
S1 O5 O6 64.9(2) . 2_656 ?
S1 O6 O5 50.02(17) . 2_656 ?
S1 O6 O5' 49.07(17) . 2_656 ?
O5 O6 O5' 89.6(2) 2_656 2_656 ?
S1 O5' O6 59.1(2) . 2_656 ?
H1WC O1W H1WB 100(4) . . ?
H2WD O2W H2WA 107.3 . . ?
H2WF O2W' H2WE 107.2 . . ?
O5 S1 O5 128.6(4) 2_656 . ?
O5 S1 O5' 119.0(2) 2_656 2_656 ?
O5 S1 O5' 35.4(2) . 2_656 ?
O5' S1 O5' 135.1(5) 2_656 . ?
O5 S1 O4 115.7(2) 2_656 . ?
O5 S1 O4 115.7(2) . . ?
O5' S1 O4 112.5(2) 2_656 . ?
O5' S1 O4 112.5(2) . . ?
O5 S1 O6 65.1(2) 2_656 . ?
O5 S1 O6 105.8(2) . . ?
O5' S1 O6 71.8(3) 2_656 . ?
O5' S1 O6 100.4(3) . . ?
O4 S1 O6 99.93(15) . . ?
O5 S1 O6 105.8(2) 2_656 2_656 ?
O5 S1 O6 65.1(2) . 2_656 ?
O4 S1 O6 99.93(15) . 2_656 ?
O6 S1 O6 160.1(3) . 2_656 ?
C2 C1 C6 119.17(19) . . ?
C2 C1 H1 120.4 . . ?
C6 C1 H1 120.4 . . ?
C1 C2 C3 121.86(19) . . ?
C1 C2 N2 117.41(18) . . ?
C3 C2 N2 120.73(18) . . ?
C2 C3 C4 117.67(18) . . ?
C2 C3 H3 121.2 . . ?
C4 C3 H3 121.2 . . ?
C5 C4 C3 121.83(19) . . ?
C5 C4 N4 119.31(18) . . ?
C3 C4 N4 118.85(18) . . ?
C6 C5 C4 118.47(19) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
C1 C6 C5 120.88(19) . . ?
C1 C6 N6 117.87(18) . . ?
C5 C6 N6 121.25(18) . . ?
N1 C7 N2 111.38(19) . . ?
N1 C7 H7 124.3 . . ?
N2 C7 H7 124.3 . . ?
C9 C8 N1 109.95(19) . . ?
C9 C8 H8 125.0 . . ?
N1 C8 H8 125.0 . . ?
C8 C9 N2 106.40(19) . . ?
C8 C9 H9 126.8 . . ?
N2 C9 H9 126.8 . . ?
N3 C10 N4 111.4(2) . . ?
N3 C10 H10 124.3 . . ?
N4 C10 H10 124.3 . . ?
C12 C11 N3 109.8(2) . . ?
C12 C11 H11 125.1 . . ?
N3 C11 H11 125.1 . . ?
C11 C12 N4 106.4(2) . . ?
C11 C12 H12 126.8 . . ?
N4 C12 H12 126.8 . . ?
N5 C13 N6 112.28(19) . . ?
N5 C13 H13 123.9 . . ?
N6 C13 H13 123.9 . . ?
C15 C14 N5 110.7(2) . . ?
C15 C14 H14 124.7 . . ?
N5 C14 H14 124.7 . . ?
C14 C15 N6 106.0(2) . . ?
C14 C15 H15 127.0 . . ?
N6 C15 H15 127.0 . . ?
O1 C16 O2 123.1(3) . . ?
O1 C16 C17 119.4(5) . . ?
O2 C16 C17 117.5(4) . . ?
C21 C17 C18 120.3(4) . . ?
C21 C17 C16 120.8(4) . . ?
C18 C17 C16 118.8(4) . . ?
C19 C18 C17 120.0(4) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.9(4) . 5_565 ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 5_565 . ?
C19 C20 C20 119.1(5) 5_565 5_565 ?
C19 C20 C21 121.8(4) 5_565 . ?
C20 C20 C21 119.2(5) 5_565 . ?
C17 C21 C20 120.5(4) . . ?
C17 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C16A O1A Cd1 91.8(10) . . ?
C16A O2A Cd1 91.8(9) . . ?
O1A C16A O2A 122.0(13) . . ?
O1A C16A C17A 122.9(14) . . ?
O2A C16A C17A 114.6(13) . . ?
O1A C16A Cd1 61.5(9) . . ?
O2A C16A Cd1 60.5(7) . . ?
C17A C16A Cd1 170.7(11) . . ?
C18A C17A C21A 122.8(11) . . ?
C18A C17A C16A 121.6(12) . . ?
C21A C17A C16A 115.5(11) . . ?
C17A C18A C19A 119.0(12) . . ?
C17A C18A H18A 120.5 . . ?
C19A C18A H18A 120.5 . . ?
C20A C19A C18A 121.5(12) 5_565 . ?
C21A C20A H20A 119.8 . . ?
C19A C20A H20A 119.8 5_565 . ?
C20A C21A C17A 119.3(12) . . ?
C20A C21A H21A 120.4 . . ?
C17A C21A H21A 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 O5 S1 O5 90.7(2) 2_656 . . 2_656 ?
O6 O5 S1 O4 -89.3(2) 2_656 . . . ?
O6 O5 S1 O6 161.2(3) 2_656 . . . ?
O6 O5' S1 O5' -86.54(19) 2_656 . . 2_656 ?
O6 O5' S1 O4 93.47(19) 2_656 . . . ?
O6 O5' S1 O6 -161.1(3) 2_656 . . . ?
O5 O6 S1 O5 -125.7(4) 2_656 . . . ?
O5' O6 S1 O5' 134.2(5) 2_656 . . . ?
O5 O6 S1 O4 113.8(2) 2_656 . . . ?
O5' O6 S1 O4 -110.5(2) 2_656 . . . ?
O5 O6 S1 O6 -66.2(2) 2_656 . . 2_656 ?
O5' O6 S1 O6 69.5(2) 2_656 . . 2_656 ?
C6 C1 C2 C3 1.6(3) . . . . ?
C6 C1 C2 N2 -178.7(2) . . . . ?
C7 N2 C2 C1 -149.5(2) . . . . ?
C9 N2 C2 C1 28.3(3) . . . . ?
C7 N2 C2 C3 30.2(4) . . . . ?
C9 N2 C2 C3 -152.0(2) . . . . ?
C1 C2 C3 C4 -3.4(3) . . . . ?
N2 C2 C3 C4 177.0(2) . . . . ?
C2 C3 C4 C5 1.8(3) . . . . ?
C2 C3 C4 N4 -176.78(19) . . . . ?
C10 N4 C4 C5 -157.1(2) . . . . ?
C12 N4 C4 C5 25.2(3) . . . . ?
C10 N4 C4 C3 21.5(3) . . . . ?
C12 N4 C4 C3 -156.2(2) . . . . ?
C3 C4 C5 C6 1.5(3) . . . . ?
N4 C4 C5 C6 -179.98(19) . . . . ?
C2 C1 C6 C5 1.8(3) . . . . ?
C2 C1 C6 N6 -177.57(19) . . . . ?
C4 C5 C6 C1 -3.3(3) . . . . ?
C4 C5 C6 N6 176.03(19) . . . . ?
C13 N6 C6 C1 174.4(2) . . . . ?
C15 N6 C6 C1 -5.8(3) . . . . ?
C13 N6 C6 C5 -4.9(3) . . . . ?
C15 N6 C6 C5 174.9(2) . . . . ?
C8 N1 C7 N2 0.1(3) . . . . ?
Cd1 N1 C7 N2 176.01(16) . . . . ?
C9 N2 C7 N1 0.2(3) . . . . ?
C2 N2 C7 N1 178.3(2) . . . . ?
C7 N1 C8 C9 -0.4(3) . . . . ?
Cd1 N1 C8 C9 -176.54(17) . . . . ?
N1 C8 C9 N2 0.5(3) . . . . ?
C7 N2 C9 C8 -0.4(3) . . . . ?
C2 N2 C9 C8 -178.6(2) . . . . ?
C11 N3 C10 N4 0.3(3) . . . . ?
Cd1 N3 C10 N4 179.01(14) 2_656 . . . ?
C12 N4 C10 N3 -0.2(3) . . . . ?
C4 N4 C10 N3 -178.29(19) . . . . ?
C10 N3 C11 C12 -0.2(3) . . . . ?
Cd1 N3 C11 C12 -178.93(15) 2_656 . . . ?
N3 C11 C12 N4 0.0(3) . . . . ?
C10 N4 C12 C11 0.1(3) . . . . ?
C4 N4 C12 C11 178.1(2) . . . . ?
C14 N5 C13 N6 0.0(3) . . . . ?
Cd1 N5 C13 N6 -167.56(15) 3 . . . ?
C15 N6 C13 N5 0.6(3) . . . . ?
C6 N6 C13 N5 -179.5(2) . . . . ?
C13 N5 C14 C15 -0.6(3) . . . . ?
Cd1 N5 C14 C15 167.14(18) 3 . . . ?
N5 C14 C15 N6 0.9(3) . . . . ?
C13 N6 C15 C14 -0.9(3) . . . . ?
C6 N6 C15 C14 179.2(2) . . . . ?
Cd1 O1 C16 O2 -4.0(6) . . . . ?
Cd1 O1 C16 C17 175.9(3) . . . . ?
Cd1 O2 C16 O1 4.0(6) . . . . ?
Cd1 O2 C16 C17 -175.9(3) . . . . ?
O1 C16 C17 C21 -20.1(7) . . . . ?
O2 C16 C17 C21 159.8(4) . . . . ?
O1 C16 C17 C18 161.2(6) . . . . ?
O2 C16 C17 C18 -18.9(5) . . . . ?
C21 C17 C18 C19 0.1(6) . . . . ?
C16 C17 C18 C19 178.8(3) . . . . ?
C17 C18 C19 C20 -1.4(5) . . . 5_565 ?
C18 C17 C21 C20 1.6(6) . . . . ?
C16 C17 C21 C20 -177.1(3) . . . . ?
C19 C20 C21 C17 178.7(4) 5_565 . . . ?
C20 C20 C21 C17 -1.9(6) 5_565 . . . ?
Cd1 O1A C16A O2A -1(3) . . . . ?
Cd1 O1A C16A C17A 170.5(14) . . . . ?
Cd1 O2A C16A O1A 1(3) . . . . ?
Cd1 O2A C16A C17A -171.1(12) . . . . ?
O1A C16A C17A C18A 167(2) . . . . ?
O2A C16A C17A C18A -21(2) . . . . ?
O1A C16A C17A C21A -13(3) . . . . ?
O2A C16A C17A C21A 159.1(16) . . . . ?
C21A C17A C18A C19A 1.2(19) . . . . ?
C16A C17A C18A C19A -178.2(12) . . . . ?
C17A C18A C19A C20A 179.2(12) . . . 5_565 ?
C17A C18A C19A C19A 0(2) . . . 5_565 ?
C19A C20A C21A C17A 0.2(18) 5_565 . . . ?
C18A C17A C21A C20A -1(2) . . . . ?
C16A C17A C21A C20A 178.4(12) . . . . ?

_refine_diff_density_max         0.223
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.047

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1564035'
_audit_update_record             
;
2017-09-09 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H84 Co4 N24 O28 S2'
_chemical_formula_weight         2177.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   22.802(2)
_cell_length_b                   13.5397(12)
_cell_length_c                   17.2991(15)
_cell_angle_alpha                90
_cell_angle_beta                 125.9900(10)
_cell_angle_gamma                90
_cell_volume                     4321.4(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2872
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      26.54

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_F_000             2240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.903
_shelx_estimated_absorpt_T_min   0.793
_shelx_estimated_absorpt_T_max   0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14338
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.208
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_full        25.010
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3793
_reflns_number_gt                3101
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0758P)²+12.9434P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3793
_refine_ls_number_parameters     371
_refine_ls_number_restraints     126
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1353
_refine_ls_wR_factor_gt          0.1239
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.979
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.24676(2) -0.01173(3) 0.45978(3) 0.02288(17) Uani 1 1 d . . . . .
N1 N 0.27105(16) 0.0809(2) 0.5730(2) 0.0273(7) Uani 1 1 d . . . . .
N2 N 0.32478(15) 0.1537(2) 0.7129(2) 0.0260(6) Uani 1 1 d . . . . .
N3 N 0.33861(16) 0.4153(2) 1.0452(2) 0.0285(7) Uani 1 1 d . . . . .
N4 N 0.39446(14) 0.3136(2) 1.0086(2) 0.0234(6) Uani 1 1 d . . . . .
N5 N 0.66935(16) 0.0487(2) 1.0457(2) 0.0297(7) Uani 1 1 d . . . . .
N6 N 0.56590(15) 0.1091(2) 1.0075(2) 0.0267(7) Uani 1 1 d . . . . .
O1 O 0.16157(14) 0.0713(2) 0.3298(2) 0.0412(7) Uani 1 1 d . . . . .
O2 O 0.20000(15) -0.0714(2) 0.31839(19) 0.0383(7) Uani 1 1 d . . . . .
O3 O 0.31429(14) -0.1294(2) 0.5391(2) 0.0407(7) Uani 1 1 d . . . . .
H3A H 0.309441 -0.179806 0.496608 0.061 Uiso 1 1 d R U . . .
H3C H 0.363637 -0.107048 0.578942 0.061 Uiso 1 1 d R U . . .
O4 O 0.500000 -0.0216(3) 0.250000 0.0458(10) Uani 1 2 d S T P . .
O6 O 0.5455(3) 0.1008(5) 0.3675(4) 0.0426(14) Uani 0.5 1 d . . P . .
C1 C 0.44626(19) 0.1343(3) 0.8578(3) 0.0288(8) Uani 1 1 d . . . . .
H1 H 0.458858 0.096766 0.824521 0.035 Uiso 1 1 calc R U . . .
C2 C 0.37742(19) 0.1747(3) 0.8120(2) 0.0263(8) Uani 1 1 d . . . . .
C3 C 0.35770(18) 0.2319(3) 0.8599(2) 0.0267(8) Uani 1 1 d . . . . .
H3 H 0.310905 0.256722 0.828358 0.032 Uiso 1 1 calc R U . . .
C4 C 0.40959(18) 0.2510(3) 0.9557(2) 0.0244(7) Uani 1 1 d . . . . .
C5 C 0.47804(19) 0.2104(3) 1.0039(2) 0.0274(8) Uani 1 1 d . . . . .
H5 H 0.512135 0.222273 1.068792 0.033 Uiso 1 1 calc R U . . .
C6 C 0.49520(18) 0.1518(3) 0.9543(2) 0.0264(8) Uani 1 1 d . . . . .
C7 C 0.32474(19) 0.0759(3) 0.6644(3) 0.0296(8) Uani 1 1 d . . . . .
H7 H 0.358482 0.024922 0.692139 0.035 Uiso 1 1 calc R U . . .
C8 C 0.2350(2) 0.1666(3) 0.5622(3) 0.0352(9) Uani 1 1 d . . . . .
H8 H 0.194396 0.189948 0.504621 0.042 Uiso 1 1 calc R U . . .
C9 C 0.2669(2) 0.2121(3) 0.6469(3) 0.0348(9) Uani 1 1 d . . . . .
H9 H 0.252798 0.271216 0.658710 0.042 Uiso 1 1 calc R U . . .
C10 C 0.33407(19) 0.3661(3) 0.9762(3) 0.0311(8) Uani 1 1 d . . . . .
H10 H 0.293891 0.367418 0.912636 0.037 Uiso 1 1 calc R U . . .
C11 C 0.4065(2) 0.3940(3) 1.1258(3) 0.0376(9) Uani 1 1 d . . . . .
H11 H 0.425809 0.419617 1.186186 0.045 Uiso 1 1 calc R U . . .
C12 C 0.4408(2) 0.3316(3) 1.1055(3) 0.0398(10) Uani 1 1 d . . . . .
H12 H 0.486861 0.305282 1.148278 0.048 Uiso 1 1 calc R U . . .
C13 C 0.6067(2) 0.0859(3) 0.9770(3) 0.0351(9) Uani 1 1 d . . . . .
H13 H 0.592125 0.095145 0.914749 0.042 Uiso 1 1 calc R U . . .
C14 C 0.6691(2) 0.0477(3) 1.1248(3) 0.0349(9) Uani 1 1 d . . . . .
H14 H 0.706887 0.025126 1.184984 0.042 Uiso 1 1 calc R U . . .
C15 C 0.6060(2) 0.0842(3) 1.1023(3) 0.0364(9) Uani 1 1 d . . . . .
H15 H 0.592288 0.091158 1.143105 0.044 Uiso 1 1 calc R U . . .
C16 C 0.1579(2) 0.0001(3) 0.2799(3) 0.0374(10) Uani 1 1 d . . . . .
C17 C 0.1071(3) -0.0110(5) 0.1729(5) 0.0234(13) Uani 0.6 1 d . U P A 2
C18 C 0.1200(4) -0.0803(5) 0.1215(5) 0.0323(13) Uani 0.6 1 d . U P A 2
H18 H 0.161873 -0.118505 0.154036 0.039 Uiso 0.6 1 calc R U P A 2
C19 C 0.0713(4) -0.0900(5) 0.0261(5) 0.0344(14) Uani 0.6 1 d . U P A 2
H19 H 0.080718 -0.134214 -0.006436 0.041 Uiso 0.6 1 calc R U P A 2
C20 C -0.0059(4) 0.0345(5) 0.0259(6) 0.0319(12) Uani 0.6 1 d . U P A 2
C21 C 0.0459(4) 0.0459(5) 0.1252(5) 0.0305(10) Uani 0.6 1 d . U P A 2
H21 H 0.038439 0.092122 0.158391 0.037 Uiso 0.6 1 calc R U P A 2
O5 O 0.5542(3) 0.1310(3) 0.2527(4) 0.1089(19) Uani 1 1 d . . . B 2
C17' C 0.0903(6) 0.0203(8) 0.1770(8) 0.0309(13) Uani 0.4 1 d . U P A 1
C18' C 0.0310(5) 0.0828(7) 0.1491(7) 0.0326(12) Uani 0.4 1 d . U P A 1
H18' H 0.031547 0.120114 0.194651 0.039 Uiso 0.4 1 calc R U P A 1
C19' C -0.0258(6) 0.0881(8) 0.0569(7) 0.039(2) Uani 0.4 1 d . U P A 1
H19' H -0.063907 0.130519 0.038968 0.047 Uiso 0.4 1 calc R U P A 1
C20' C 0.0289(7) -0.0324(9) 0.0113(9) 0.037(3) Uani 0.4 1 d . U P A 1
C21' C 0.0909(6) -0.0393(8) 0.1136(8) 0.035(2) Uani 0.4 1 d . U P A 1
H21' H 0.129052 -0.082746 0.133996 0.042 Uiso 0.4 1 calc R U P A 1
O1W O 0.5758(3) 0.7165(4) 0.3358(4) 0.1144(17) Uani 0.6 1 d . . P C 1
H1WB H 0.577273 0.682162 0.297446 0.172 Uiso 0.6 1 d R U P C 1
H1WC H 0.545893 0.765372 0.305956 0.172 Uiso 0.6 1 d R U P C 1
O1W' O 0.5758(3) 0.7165(4) 0.3358(4) 0.1144(17) Uani 0.4 1 d . . P D 2
H1WG H 0.575073 0.685143 0.294156 0.172 Uiso 0.4 1 d R U P D 2
H1WH H 0.547953 0.768212 0.310216 0.172 Uiso 0.4 1 d R U P D 2
O2W O 0.68087(18) 0.2221(3) 0.3080(3) 0.0710(11) Uani 1 1 d . . . E 2
H2WA H 0.681807 0.291105 0.310669 0.085 Uiso 1 1 d R U . E 2
H2WB H 0.638507 0.212305 0.290669 0.085 Uiso 1 1 d R U . E 2
S1 S 0.500000 0.08589(11) 0.250000 0.0453(4) Uani 1 2 d S T P B 2


_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
Co1 O3 2.076(3) . ?
Co1 N1 2.107(3) . ?
Co1 N5 2.133(3) 2_656 ?
Co1 N3 2.139(3) 4_546 ?
Co1 O2 2.170(3) . ?
Co1 O1 2.227(3) . ?
N1 C7 1.315(5) . ?
N1 C8 1.370(5) . ?
N2 C7 1.346(4) . ?
N2 C9 1.377(5) . ?
N2 C2 1.429(4) . ?
N3 C10 1.317(4) . ?
N3 C11 1.374(5) . ?
N4 C10 1.345(4) . ?
N4 C12 1.380(5) . ?
N4 C4 1.431(4) . ?
N5 C13 1.308(5) . ?
N5 C14 1.372(5) . ?
N6 C13 1.350(4) . ?
N6 C15 1.370(5) . ?
N6 C6 1.427(4) . ?
O1 C16 1.263(5) . ?
O2 C16 1.245(5) . ?
O3 H3A 0.9600 . ?
O3 H3C 0.9600 . ?
O4 S1 1.456(4) . ?
O6 S1 1.665(5) . ?
C1 C6 1.379(5) . ?
C1 C2 1.389(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.388(5) . ?
C3 C4 1.382(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.380(5) . ?
C5 C6 1.383(5) . ?
C5 H5 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.342(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.330(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.344(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.507(7) . ?
C16 C17' 1.547(12) . ?
C17 C21 1.367(9) . ?
C17 C18 1.436(10) . ?
C18 C19 1.349(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.421(10) 5 ?
C19 H19 0.9300 . ?
C20 C21 1.409(11) . ?
C20 C20 1.426(15) 5 ?
C21 H21 0.9300 . ?
O5 S1 1.356(4) . ?
C17' C21' 1.369(16) . ?
C17' C18' 1.418(16) . ?
C18' C19' 1.342(14) . ?
C18' H18' 0.9300 . ?
C19' C20' 1.367(16) 5 ?
C19' H19' 0.9300 . ?
C20' C20' 1.43(2) 5 ?
C20' C21' 1.483(16) . ?
C21' H21' 0.9300 . ?
O1W H1WB 0.8267 . ?
O1W H1WC 0.8693 . ?
O1W' H1WG 0.8278 . ?
O1W' H1WH 0.8712 . ?
O2W H2WA 0.9356 . ?
O2W H2WB 0.8369 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 N1 98.94(12) . . ?
O3 Co1 N5 89.27(12) . 2_656 ?
N1 Co1 N5 93.44(11) . 2_656 ?
O3 Co1 N3 88.63(11) . 4_546 ?
N1 Co1 N3 92.79(11) . 4_546 ?
N5 Co1 N3 173.67(12) 2_656 4_546 ?
O3 Co1 O2 98.12(12) . . ?
N1 Co1 O2 162.93(12) . . ?
N5 Co1 O2 87.26(11) 2_656 . ?
N3 Co1 O2 87.12(10) 4_546 . ?
O3 Co1 O1 157.33(12) . . ?
N1 Co1 O1 103.58(12) . . ?
N5 Co1 O1 91.97(11) 2_656 . ?
N3 Co1 O1 87.67(11) 4_546 . ?
O2 Co1 O1 59.36(12) . . ?
C7 N1 C8 105.5(3) . . ?
C7 N1 Co1 129.6(3) . . ?
C8 N1 Co1 124.7(2) . . ?
C7 N2 C9 106.4(3) . . ?
C7 N2 C2 126.5(3) . . ?
C9 N2 C2 126.9(3) . . ?
C10 N3 C11 104.8(3) . . ?
C10 N3 Co1 127.8(2) . 4_556 ?
C11 N3 Co1 126.4(2) . 4_556 ?
C10 N4 C12 106.2(3) . . ?
C10 N4 C4 128.2(3) . . ?
C12 N4 C4 125.6(3) . . ?
C13 N5 C14 105.5(3) . . ?
C13 N5 Co1 129.5(2) . 2_656 ?
C14 N5 Co1 124.8(2) . 2_656 ?
C13 N6 C15 106.4(3) . . ?
C13 N6 C6 128.3(3) . . ?
C15 N6 C6 125.3(3) . . ?
C16 O1 Co1 88.5(2) . . ?
C16 O2 Co1 91.5(2) . . ?
Co1 O3 H3A 109.4 . . ?
Co1 O3 H3C 109.5 . . ?
H3A O3 H3C 109.5 . . ?
C6 C1 C2 117.5(3) . . ?
C6 C1 H1 121.3 . . ?
C2 C1 H1 121.3 . . ?
C3 C2 C1 122.3(3) . . ?
C3 C2 N2 119.3(3) . . ?
C1 C2 N2 118.5(3) . . ?
C4 C3 C2 118.1(3) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C3 C4 C5 121.2(3) . . ?
C3 C4 N4 121.4(3) . . ?
C5 C4 N4 117.5(3) . . ?
C6 C5 C4 119.0(3) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C1 C6 C5 121.8(3) . . ?
C1 C6 N6 121.0(3) . . ?
C5 C6 N6 117.2(3) . . ?
N1 C7 N2 111.6(3) . . ?
N1 C7 H7 124.2 . . ?
N2 C7 H7 124.2 . . ?
C9 C8 N1 110.0(3) . . ?
C9 C8 H8 125.0 . . ?
N1 C8 H8 125.0 . . ?
C8 C9 N2 106.4(3) . . ?
C8 C9 H9 126.8 . . ?
N2 C9 H9 126.8 . . ?
N3 C10 N4 111.9(3) . . ?
N3 C10 H10 124.0 . . ?
N4 C10 H10 124.0 . . ?
C12 C11 N3 110.6(3) . . ?
C12 C11 H11 124.7 . . ?
N3 C11 H11 124.7 . . ?
C11 C12 N4 106.5(3) . . ?
C11 C12 H12 126.8 . . ?
N4 C12 H12 126.8 . . ?
N5 C13 N6 111.7(3) . . ?
N5 C13 H13 124.1 . . ?
N6 C13 H13 124.1 . . ?
C15 C14 N5 109.8(3) . . ?
C15 C14 H14 125.1 . . ?
N5 C14 H14 125.1 . . ?
C14 C15 N6 106.6(3) . . ?
C14 C15 H15 126.7 . . ?
N6 C15 H15 126.7 . . ?
O2 C16 O1 120.5(4) . . ?
O2 C16 C17 111.9(4) . . ?
O1 C16 C17 127.6(5) . . ?
O2 C16 C17' 133.3(6) . . ?
O1 C16 C17' 105.8(6) . . ?
C21 C17 C18 120.2(6) . . ?
C21 C17 C16 117.4(6) . . ?
C18 C17 C16 122.4(6) . . ?
C19 C18 C17 120.0(7) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 H19 119.1 . . ?
C20 C19 H19 119.1 5 . ?
C20 C21 C17 120.1(7) . . ?
C20 C21 H21 120.0 . . ?
C17 C21 H21 120.0 . . ?
C21' C17' C18' 122.4(11) . . ?
C21' C17' C16 110.2(10) . . ?
C18' C17' C16 127.1(9) . . ?
C19' C18' C17' 119.9(10) . . ?
C19' C18' H18' 120.1 . . ?
C17' C18' H18' 120.1 . . ?
C20' C19' C18' 121.4(11) 5 . ?
C20' C19' H19' 119.3 5 . ?
C18' C19' H19' 119.3 . . ?
C19' C20' C20' 121.9(14) 5 5 ?
C19' C20' C21' 121.6(11) 5 . ?
C20' C20' C21' 116.4(14) 5 . ?
C17' C21' C20' 117.8(11) . . ?
C17' C21' H21' 121.1 . . ?
C20' C21' H21' 121.1 . . ?
H1WB O1W H1WC 109.8 . . ?
H1WG O1W' H1WH 109.5 . . ?
H2WA O2W H2WB 99.4 . . ?
O5 S1 O5 126.4(4) 2_655 . ?
O5 S1 O4 116.80(19) 2_655 . ?
O5 S1 O4 116.80(19) . . ?
O4 S1 O6 96.9(2) . 2_655 ?
O5 S1 O6 83.6(3) 2_655 . ?
O5 S1 O6 90.1(3) . . ?
O4 S1 O6 96.9(2) . . ?
O6 S1 O6 166.1(4) 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.9(5) . . . . ?
C6 C1 C2 N2 -177.2(3) . . . . ?
C7 N2 C2 C3 -155.1(3) . . . . ?
C9 N2 C2 C3 29.5(5) . . . . ?
C7 N2 C2 C1 23.0(5) . . . . ?
C9 N2 C2 C1 -152.4(4) . . . . ?
C1 C2 C3 C4 1.9(6) . . . . ?
N2 C2 C3 C4 179.9(3) . . . . ?
C2 C3 C4 C5 -3.3(5) . . . . ?
C2 C3 C4 N4 176.8(3) . . . . ?
C10 N4 C4 C3 -4.8(6) . . . . ?
C12 N4 C4 C3 175.3(4) . . . . ?
C10 N4 C4 C5 175.3(4) . . . . ?
C12 N4 C4 C5 -4.7(5) . . . . ?
C3 C4 C5 C6 1.8(6) . . . . ?
N4 C4 C5 C6 -178.2(3) . . . . ?
C2 C1 C6 C5 -2.4(6) . . . . ?
C2 C1 C6 N6 177.0(3) . . . . ?
C4 C5 C6 C1 1.1(6) . . . . ?
C4 C5 C6 N6 -178.3(3) . . . . ?
C13 N6 C6 C1 30.5(6) . . . . ?
C15 N6 C6 C1 -150.0(4) . . . . ?
C13 N6 C6 C5 -150.0(4) . . . . ?
C15 N6 C6 C5 29.5(5) . . . . ?
C8 N1 C7 N2 0.3(4) . . . . ?
Co1 N1 C7 N2 175.1(2) . . . . ?
C9 N2 C7 N1 -0.2(4) . . . . ?
C2 N2 C7 N1 -176.4(3) . . . . ?
C7 N1 C8 C9 -0.3(4) . . . . ?
Co1 N1 C8 C9 -175.4(3) . . . . ?
N1 C8 C9 N2 0.2(4) . . . . ?
C7 N2 C9 C8 0.0(4) . . . . ?
C2 N2 C9 C8 176.2(3) . . . . ?
C11 N3 C10 N4 1.1(4) . . . . ?
Co1 N3 C10 N4 -167.8(2) 4_556 . . . ?
C12 N4 C10 N3 -0.3(4) . . . . ?
C4 N4 C10 N3 179.7(3) . . . . ?
C10 N3 C11 C12 -1.5(5) . . . . ?
Co1 N3 C11 C12 167.6(3) 4_556 . . . ?
N3 C11 C12 N4 1.3(5) . . . . ?
C10 N4 C12 C11 -0.6(5) . . . . ?
C4 N4 C12 C11 179.4(3) . . . . ?
C14 N5 C13 N6 0.1(5) . . . . ?
Co1 N5 C13 N6 174.9(3) 2_656 . . . ?
C15 N6 C13 N5 -0.2(5) . . . . ?
C6 N6 C13 N5 179.3(3) . . . . ?
C13 N5 C14 C15 0.2(5) . . . . ?
Co1 N5 C14 C15 -175.0(3) 2_656 . . . ?
N5 C14 C15 N6 -0.3(5) . . . . ?
C13 N6 C15 C14 0.3(5) . . . . ?
C6 N6 C15 C14 -179.3(4) . . . . ?
Co1 O2 C16 O1 4.0(4) . . . . ?
Co1 O2 C16 C17 -176.7(3) . . . . ?
Co1 O2 C16 C17' -167.4(7) . . . . ?
Co1 O1 C16 O2 -3.9(3) . . . . ?
Co1 O1 C16 C17 176.9(4) . . . . ?
Co1 O1 C16 C17' 169.6(5) . . . . ?
O2 C16 C17 C21 161.6(5) . . . . ?
O1 C16 C17 C21 -19.2(8) . . . . ?
O2 C16 C17 C18 -16.5(7) . . . . ?
O1 C16 C17 C18 162.7(5) . . . . ?
C21 C17 C18 C19 -0.6(9) . . . . ?
C16 C17 C18 C19 177.5(5) . . . . ?
C17 C18 C19 C20 -1.2(10) . . . 5 ?
C20 C20 C21 C17 -1.6(12) 5 . . . ?
C19 C20 C21 C17 178.2(6) 5 . . . ?
C18 C17 C21 C20 2.0(9) . . . . ?
C16 C17 C21 C20 -176.1(5) . . . . ?
O2 C16 C17' C21' -21.7(12) . . . . ?
O1 C16 C17' C21' 165.9(7) . . . . ?
O2 C16 C17' C18' 152.2(8) . . . . ?
O1 C16 C17' C18' -20.2(11) . . . . ?
C21' C17' C18' C19' -2.9(16) . . . . ?
C16 C17' C18' C19' -176.1(9) . . . . ?
C17' C18' C19' C20' 1.6(16) . . . 5 ?
C18' C17' C21' C20' 4.0(16) . . . . ?
C16 C17' C21' C20' 178.2(8) . . . . ?
C19' C20' C21' C17' 178.9(10) 5 . . . ?
C20' C20' C21' C17' -3.7(18) 5 . . . ?

_refine_diff_density_max         0.610
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.083

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1564037'
_audit_update_record             
;
2017-09-09 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C42 H30 Cd2 N14 O10, C7.5 H17.5 N2.5 O2.5, H2 O'
_chemical_formula_sum            'C49.50 H49.50 Cd2 N16.50 O13.50'
_chemical_formula_weight         1316.35

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.572(5)
_cell_length_b                   14.157(5)
_cell_length_c                   19.505(8)
_cell_angle_alpha                93.398(11)
_cell_angle_beta                 110.063(9)
_cell_angle_gamma                90.003(10)
_cell_volume                     3513(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4871
_cell_measurement_theta_min      2.5760
_cell_measurement_theta_max      25.8579

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_F_000             1332
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.667
_shelx_estimated_absorpt_T_min   0.856
_shelx_estimated_absorpt_T_max   0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3350
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20724
_diffrn_reflns_av_unetI/netI     0.1858
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.129
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_full        25.009
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             12316
_reflns_number_gt                7436
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
SQUEEZE removed 2.5 disordered DMF, and one disordered H2O
per formula unit. This value is calculated based upon charge balance
considerations, volume/count_electrons analysis, and TG experiment.
See ref. Bi, Y. F.; Wang, X. T.; Liao, W. P.; Wang, X. F.; Wang, X. W.;
Zhang, H. J.; Gao, S. J. Am. Chem. Soc. 2009, 131, 11650.
CHEMW03_ALERT_2_A ALERT
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for 2.5 disordered DMF,
and one disordered H2O omitted by SQUEEZE.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1059P)²+15.6877P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12316
_refine_ls_number_parameters     613
_refine_ls_number_restraints     720
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.1021
_refine_ls_wR_factor_ref         0.2695
_refine_ls_wR_factor_gt          0.2452
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd -0.10097(6) 0.46361(5) 0.13763(4) 0.0306(2) Uani 1 1 d . . . . .
Cd2 Cd 0.40107(6) 1.06731(5) 0.14419(4) 0.0323(2) Uani 1 1 d . . . . .
N1 N -0.1307(7) 0.6019(6) 0.0790(4) 0.0345(18) Uani 1 1 d . U . . .
N2 N -0.1242(7) 0.7542(6) 0.0709(5) 0.0317(17) Uani 1 1 d . U . . .
N3 N 0.2285(7) 1.0876(7) 0.1267(6) 0.046(2) Uani 1 1 d . . . . .
N4 N 0.0694(7) 1.0539(6) 0.1219(6) 0.045(2) Uani 1 1 d . . . . .
N5 N -0.4210(7) 1.0601(6) 0.1643(5) 0.040(2) Uani 1 1 d . . . . .
N6 N -0.2685(7) 1.0346(6) 0.1563(5) 0.039(2) Uani 1 1 d . . . . .
N7 N 0.0767(7) 0.4744(7) 0.1586(5) 0.038(2) Uani 1 1 d . . . . .
N8 N 0.2344(7) 0.5019(6) 0.1533(5) 0.038(2) Uani 1 1 d . . . . .
N9 N 0.3718(7) 0.9222(6) 0.0842(5) 0.0376(19) Uani 1 1 d . U . . .
N10 N 0.3775(7) 0.7666(6) 0.0713(5) 0.0346(18) Uani 1 1 d . U . . .
N11 N 0.7244(7) 0.4390(6) 0.1171(5) 0.038(2) Uani 1 1 d . . . . .
N12 N 0.5638(7) 0.4728(6) 0.1149(5) 0.039(2) Uani 1 1 d . . . . .
N13 N -0.1124(7) 0.2944(7) 0.0458(5) 0.042(2) Uani 1 1 d . . . . .
N14 N 0.3889(7) 1.2194(8) 0.0497(6) 0.048(2) Uani 1 1 d . . . . .
C1 C -0.1953(9) 0.8936(7) 0.1142(6) 0.038(2) Uani 1 1 d . . . . .
H1 H -0.251496 0.857341 0.115818 0.046 Uiso 1 1 calc R U . . .
C2 C -0.1179(8) 0.8546(7) 0.0922(5) 0.032(2) Uani 1 1 d . . . . .
C3 C -0.0319(9) 0.9054(8) 0.0922(7) 0.043(3) Uani 1 1 d . . . . .
H3 H 0.019692 0.877246 0.077063 0.051 Uiso 1 1 calc R U . . .
C4 C -0.0252(9) 0.9976(8) 0.1149(6) 0.038(2) Uani 1 1 d . . . . .
C5 C -0.1030(8) 1.0441(9) 0.1318(7) 0.046(3) Uani 1 1 d . . . . .
H5 H -0.099928 1.109423 0.141394 0.055 Uiso 1 1 calc R U . . .
C6 C -0.1860(8) 0.9902(8) 0.1339(6) 0.038(2) Uani 1 1 d . . . . .
C7 C -0.1360(8) 0.6835(7) 0.1090(5) 0.0306(19) Uani 1 1 d . U . . .
H7 H -0.147084 0.692359 0.153439 0.037 Uiso 1 1 calc R U . . .
C8 C -0.1098(10) 0.6224(9) 0.0177(6) 0.048(3) Uani 1 1 d . . . . .
H8 H -0.100432 0.576826 -0.015796 0.058 Uiso 1 1 calc R U . . .
C9 C -0.1044(11) 0.7140(8) 0.0116(6) 0.053(3) Uani 1 1 d . . . . .
H9 H -0.090250 0.744658 -0.024940 0.064 Uiso 1 1 calc R U . . .
C10 C 0.1530(8) 1.0264(8) 0.1048(6) 0.035(2) Uani 1 1 d . . . . .
H10 H 0.155894 0.969122 0.079746 0.043 Uiso 1 1 calc R U . . .
C11 C 0.1933(9) 1.1596(9) 0.1579(8) 0.055(3) Uani 1 1 d . . . . .
H11 H 0.231502 1.215351 0.177172 0.066 Uiso 1 1 calc R U . . .
C12 C 0.0959(9) 1.1428(8) 0.1586(8) 0.057(4) Uani 1 1 d . . . . .
H12 H 0.056055 1.181269 0.178759 0.069 Uiso 1 1 calc R U . . .
C13 C -0.3660(8) 1.0023(8) 0.1387(6) 0.036(2) Uani 1 1 d . . . . .
H13 H -0.391759 0.945788 0.111635 0.043 Uiso 1 1 calc R U . . .
C14 C -0.3562(10) 1.1325(9) 0.1969(8) 0.058(4) Uani 1 1 d . . . . .
H14 H -0.374736 1.185815 0.219553 0.070 Uiso 1 1 calc R U . . .
C15 C -0.2609(10) 1.1188(10) 0.1928(8) 0.067(4) Uani 1 1 d . . . . .
H15 H -0.202295 1.158982 0.211262 0.081 Uiso 1 1 calc R U . . .
C16 C 0.3988(9) 0.4860(7) 0.1319(6) 0.039(2) Uani 1 1 d . . . . .
H16 H 0.404551 0.424173 0.146236 0.047 Uiso 1 1 calc R U . . .
C17 C 0.3129(8) 0.5419(7) 0.1324(5) 0.032(2) Uani 1 1 d . . . . .
C18 C 0.3063(8) 0.6358(7) 0.1135(6) 0.031(2) Uani 1 1 d . . . . .
H18 H 0.252535 0.673909 0.117669 0.038 Uiso 1 1 calc R U . . .
C19 C 0.3815(8) 0.6703(8) 0.0885(5) 0.033(2) Uani 1 1 d . . . . .
C20 C 0.4686(8) 0.6200(8) 0.0893(6) 0.039(2) Uani 1 1 d . . . . .
H20 H 0.522015 0.647704 0.077078 0.047 Uiso 1 1 calc R U . . .
C21 C 0.4747(8) 0.5271(8) 0.1089(6) 0.037(2) Uani 1 1 d . . . . .
C22 C 0.1315(8) 0.5300(8) 0.1342(5) 0.033(2) Uani 1 1 d . . . . .
H22 H 0.104871 0.582056 0.107377 0.040 Uiso 1 1 calc R U . . .
C23 C 0.1444(9) 0.4082(9) 0.1956(7) 0.055(3) Uani 1 1 d . . . . .
H23 H 0.126572 0.358846 0.218909 0.066 Uiso 1 1 calc R U . . .
C25 C 0.3594(8) 0.8431(8) 0.1056(6) 0.039(2) Uani 1 1 d . U . . .
H25 H 0.337578 0.838632 0.145593 0.047 Uiso 1 1 calc R U . . .
C26 C 0.3916(11) 0.8990(8) 0.0216(6) 0.055(3) Uani 1 1 d . . . . .
H26 H 0.396110 0.941998 -0.011529 0.066 Uiso 1 1 calc R U . . .
C27 C 0.4040(10) 0.8031(9) 0.0141(7) 0.054(3) Uani 1 1 d . . . . .
H27 H 0.425064 0.769818 -0.020859 0.064 Uiso 1 1 calc R U . . .
C28 C 0.5919(11) 0.3911(9) 0.1452(10) 0.076(5) Uani 1 1 d . . . . .
H28 H 0.551054 0.353596 0.163069 0.091 Uiso 1 1 calc R U . . .
C29 C 0.6883(10) 0.3714(9) 0.1460(9) 0.066(4) Uani 1 1 d . . . . .
H29 H 0.724793 0.317582 0.164319 0.080 Uiso 1 1 calc R U . . .
C30 C 0.6462(8) 0.4989(8) 0.0976(6) 0.038(2) Uani 1 1 d . . . . .
H30 H 0.648455 0.553750 0.074073 0.046 Uiso 1 1 calc R U . . .
C31 C -0.0647(10) 0.4996(10) 0.2814(6) 0.051(3) Uani 1 1 d . . . . .
C32 C -0.0460(11) 0.5121(10) 0.3642(7) 0.062(4) Uani 1 1 d . . . . .
C33 C -0.0125(14) 0.4432(11) 0.4076(7) 0.081(5) Uani 1 1 d . . . . .
H33 H -0.000275 0.385009 0.387653 0.097 Uiso 1 1 calc R U . . .
C34 C 0.0058(15) 0.4534(11) 0.4836(8) 0.085(4) Uani 1 1 d . U . . .
C35 C 0.0381(15) 0.3821(12) 0.5329(7) 0.090(5) Uani 1 1 d . U . . .
H35 H 0.047293 0.322210 0.513952 0.109 Uiso 1 1 calc R U . . .
C36 C -0.0567(16) 0.6073(11) 0.3954(7) 0.094(6) Uani 1 1 d . . . . .
H36 H -0.075784 0.658279 0.365953 0.112 Uiso 1 1 calc R U . . .
C39 C 0.4437(10) 1.0547(10) 0.2922(7) 0.052(3) Uani 1 1 d . . . . .
C40 C 0.4676(11) 1.0493(10) 0.3722(7) 0.061(3) Uani 1 1 d . U . . .
C41 C 0.4582(13) 0.9651(12) 0.4023(8) 0.080(5) Uani 1 1 d . . . . .
H41 H 0.433479 0.911272 0.371288 0.096 Uiso 1 1 calc R U . . .
C42 C 0.4853(14) 0.9580(11) 0.4795(8) 0.077(5) Uani 1 1 d . . . . .
C43 C 0.4734(18) 0.8705(13) 0.5080(9) 0.107(7) Uani 1 1 d . . . . .
H43 H 0.448394 0.816639 0.477077 0.129 Uiso 1 1 calc R U . . .
C44 C 0.5011(17) 1.1326(12) 0.4203(8) 0.106(7) Uani 1 1 d . . . . .
H44 H 0.504978 1.190201 0.400672 0.127 Uiso 1 1 calc R U . . .
C57 C 0.2415(10) 0.4253(9) 0.1933(8) 0.062(4) Uani 1 1 d . . . . .
H57 H 0.301508 0.390996 0.214907 0.074 Uiso 1 1 calc R U . . .
O1 O -0.0585(7) 0.4170(6) 0.2582(5) 0.058(2) Uani 1 1 d . . . . .
O2 O -0.0902(8) 0.5681(6) 0.2468(5) 0.068(3) Uani 1 1 d . . . . .
O3 O -0.1130(6) 0.3777(6) 0.0218(4) 0.051(2) Uani 1 1 d . . . . .
O4 O -0.1019(6) 0.2879(6) 0.1133(4) 0.049(2) Uani 1 1 d . . . . .
O5 O -0.1183(8) 0.2211(7) 0.0057(6) 0.075(3) Uani 1 1 d . . . . .
O6 O 0.4154(8) 0.9800(6) 0.2516(4) 0.063(3) Uani 1 1 d . . . . .
O7 O 0.4482(7) 1.1318(7) 0.2666(5) 0.063(2) Uani 1 1 d . . . . .
O8 O 0.3995(7) 1.2330(6) 0.1171(5) 0.056(2) Uani 1 1 d . . . . .
O9 O 0.3872(7) 1.1340(6) 0.0267(5) 0.055(2) Uani 1 1 d . . . . .
O10 O 0.3817(8) 1.2823(7) 0.0078(6) 0.082(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N11 2.287(9) 1_455 ?
Cd1 N1 2.292(8) . ?
Cd1 N7 2.307(9) . ?
Cd1 O1 2.356(8) . ?
Cd1 O3 2.457(8) . ?
Cd1 O2 2.481(8) . ?
Cd1 O4 2.504(8) . ?
Cd1 C31 2.692(12) . ?
Cd2 N9 2.267(9) . ?
Cd2 N3 2.268(9) . ?
Cd2 N5 2.314(9) 1_655 ?
Cd2 O7 2.374(9) . ?
Cd2 O8 2.433(8) . ?
Cd2 O6 2.445(8) . ?
Cd2 O9 2.478(8) . ?
Cd2 C39 2.760(12) . ?
N1 C7 1.277(12) . ?
N1 C8 1.367(14) . ?
N2 C7 1.324(12) . ?
N2 C9 1.366(13) . ?
N2 C2 1.452(13) . ?
N3 C10 1.280(13) . ?
N3 C11 1.329(14) . ?
N4 C10 1.341(13) . ?
N4 C12 1.393(14) . ?
N4 C4 1.472(14) . ?
N5 C13 1.296(13) . ?
N5 C14 1.330(15) . ?
N6 C13 1.323(13) . ?
N6 C15 1.337(15) . ?
N6 C6 1.464(14) . ?
N7 C22 1.298(13) . ?
N7 C23 1.368(14) . ?
N8 C57 1.358(15) . ?
N8 C22 1.381(13) . ?
N8 C17 1.396(13) . ?
N9 C25 1.250(14) . ?
N9 C26 1.361(14) . ?
N10 C25 1.306(13) . ?
N10 C27 1.409(15) . ?
N10 C19 1.420(14) . ?
N11 C29 1.313(15) . ?
N11 C30 1.325(13) . ?
N12 C28 1.327(16) . ?
N12 C30 1.333(14) . ?
N12 C21 1.406(13) . ?
N13 O5 1.248(11) . ?
N13 O4 1.284(12) . ?
N13 O3 1.294(12) . ?
N14 O10 1.227(12) . ?
N14 O9 1.263(13) . ?
N14 O8 1.274(13) . ?
C1 C2 1.369(14) . ?
C1 C6 1.392(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.370(15) . ?
C3 C4 1.347(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(15) . ?
C5 C6 1.374(15) . ?
C5 H5 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.313(16) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.347(16) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.335(17) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C21 1.396(15) . ?
C16 C17 1.412(14) . ?
C16 H16 0.9300 . ?
C17 C18 1.395(14) . ?
C18 C19 1.374(15) . ?
C18 H18 0.9300 . ?
C19 C20 1.376(14) . ?
C20 C21 1.387(15) . ?
C20 H20 0.9300 . ?
C22 H22 0.9300 . ?
C23 C57 1.357(17) . ?
C23 H23 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.373(16) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.333(17) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O2 1.197(15) . ?
C31 O1 1.242(15) . ?
C31 C32 1.546(16) . ?
C32 C33 1.306(19) . ?
C32 C36 1.472(19) . ?
C33 C34 1.415(19) . ?
C33 H33 0.9300 . ?
C34 C35 1.40(2) . ?
C34 C34 1.46(3) 2_566 ?
C35 C36 1.333(18) 2_566 ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C39 O7 1.238(15) . ?
C39 O6 1.259(15) . ?
C39 C40 1.487(16) . ?
C40 C41 1.38(2) . ?
C40 C44 1.43(2) . ?
C41 C42 1.432(19) . ?
C41 H41 0.9300 . ?
C42 C42 1.37(3) 2_676 ?
C42 C43 1.42(2) . ?
C43 C44 1.32(2) 2_676 ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C57 H57 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N11 Cd1 N1 92.5(3) 1_455 . ?
N11 Cd1 N7 175.0(3) 1_455 . ?
N1 Cd1 N7 91.9(3) . . ?
N11 Cd1 O1 90.6(3) 1_455 . ?
N1 Cd1 O1 137.5(3) . . ?
N7 Cd1 O1 87.7(3) . . ?
N11 Cd1 O3 92.2(3) 1_455 . ?
N1 Cd1 O3 89.3(3) . . ?
N7 Cd1 O3 85.5(3) . . ?
O1 Cd1 O3 133.0(3) . . ?
N11 Cd1 O2 88.8(3) 1_455 . ?
N1 Cd1 O2 83.9(3) . . ?
N7 Cd1 O2 93.9(3) . . ?
O1 Cd1 O2 53.8(3) . . ?
O3 Cd1 O2 173.1(3) . . ?
N11 Cd1 O4 83.7(3) 1_455 . ?
N1 Cd1 O4 141.8(3) . . ?
N7 Cd1 O4 91.4(3) . . ?
O1 Cd1 O4 80.7(3) . . ?
O3 Cd1 O4 53.1(3) . . ?
O2 Cd1 O4 133.8(3) . . ?
N11 Cd1 C31 90.5(4) 1_455 . ?
N1 Cd1 C31 110.1(4) . . ?
N7 Cd1 C31 90.1(4) . . ?
O1 Cd1 C31 27.5(3) . . ?
O3 Cd1 C31 160.3(4) . . ?
O2 Cd1 C31 26.3(3) . . ?
O4 Cd1 C31 108.0(4) . . ?
N9 Cd2 N3 93.0(3) . . ?
N9 Cd2 N5 91.6(3) . 1_655 ?
N3 Cd2 N5 175.2(3) . 1_655 ?
N9 Cd2 O7 137.8(3) . . ?
N3 Cd2 O7 90.9(3) . . ?
N5 Cd2 O7 86.7(3) 1_655 . ?
N9 Cd2 O8 139.1(3) . . ?
N3 Cd2 O8 84.5(3) . . ?
N5 Cd2 O8 91.2(3) 1_655 . ?
O7 Cd2 O8 83.1(3) . . ?
N9 Cd2 O6 84.4(3) . . ?
N3 Cd2 O6 88.7(4) . . ?
N5 Cd2 O6 93.1(3) 1_655 . ?
O7 Cd2 O6 53.7(3) . . ?
O8 Cd2 O6 136.1(3) . . ?
N9 Cd2 O9 87.8(3) . . ?
N3 Cd2 O9 93.2(3) . . ?
N5 Cd2 O9 85.6(3) 1_655 . ?
O7 Cd2 O9 133.9(3) . . ?
O8 Cd2 O9 51.8(3) . . ?
O6 Cd2 O9 172.0(3) . . ?
N9 Cd2 C39 111.3(4) . . ?
N3 Cd2 C39 90.5(4) . . ?
N5 Cd2 C39 89.1(4) 1_655 . ?
O7 Cd2 C39 26.6(3) . . ?
O8 Cd2 C39 109.5(4) . . ?
O6 Cd2 C39 27.1(3) . . ?
O9 Cd2 C39 160.3(4) . . ?
C7 N1 C8 103.3(9) . . ?
C7 N1 Cd1 125.1(7) . . ?
C8 N1 Cd1 127.9(7) . . ?
C7 N2 C9 106.3(9) . . ?
C7 N2 C2 127.3(9) . . ?
C9 N2 C2 125.8(9) . . ?
C10 N3 C11 105.4(10) . . ?
C10 N3 Cd2 128.9(8) . . ?
C11 N3 Cd2 123.2(8) . . ?
C10 N4 C12 106.0(9) . . ?
C10 N4 C4 128.0(9) . . ?
C12 N4 C4 125.4(10) . . ?
C13 N5 C14 105.2(10) . . ?
C13 N5 Cd2 132.3(8) . 1_455 ?
C14 N5 Cd2 121.4(8) . 1_455 ?
C13 N6 C15 108.0(10) . . ?
C13 N6 C6 126.0(9) . . ?
C15 N6 C6 125.8(10) . . ?
C22 N7 C23 106.1(10) . . ?
C22 N7 Cd1 131.7(8) . . ?
C23 N7 Cd1 121.7(8) . . ?
C57 N8 C22 105.9(9) . . ?
C57 N8 C17 127.5(10) . . ?
C22 N8 C17 126.6(10) . . ?
C25 N9 C26 102.5(10) . . ?
C25 N9 Cd2 130.6(8) . . ?
C26 N9 Cd2 125.0(8) . . ?
C25 N10 C27 102.6(10) . . ?
C25 N10 C19 131.0(10) . . ?
C27 N10 C19 126.1(9) . . ?
C29 N11 C30 103.8(10) . . ?
C29 N11 Cd1 123.3(8) . 1_655 ?
C30 N11 Cd1 129.6(8) . 1_655 ?
C28 N12 C30 103.7(10) . . ?
C28 N12 C21 129.8(11) . . ?
C30 N12 C21 126.1(10) . . ?
O5 N13 O4 119.8(11) . . ?
O5 N13 O3 121.5(10) . . ?
O4 N13 O3 118.7(9) . . ?
O10 N14 O9 119.5(12) . . ?
O10 N14 O8 124.9(12) . . ?
O9 N14 O8 115.5(9) . . ?
C2 C1 C6 116.8(10) . . ?
C2 C1 H1 121.6 . . ?
C6 C1 H1 121.6 . . ?
C1 C2 C3 122.9(10) . . ?
C1 C2 N2 118.9(9) . . ?
C3 C2 N2 118.1(10) . . ?
C4 C3 C2 117.4(11) . . ?
C4 C3 H3 121.3 . . ?
C2 C3 H3 121.3 . . ?
C3 C4 C5 123.5(11) . . ?
C3 C4 N4 119.9(10) . . ?
C5 C4 N4 116.6(10) . . ?
C4 C5 C6 117.0(11) . . ?
C4 C5 H5 121.5 . . ?
C6 C5 H5 121.5 . . ?
C5 C6 C1 121.9(11) . . ?
C5 C6 N6 119.8(10) . . ?
C1 C6 N6 118.3(10) . . ?
N1 C7 N2 113.5(9) . . ?
N1 C7 H7 123.3 . . ?
N2 C7 H7 123.3 . . ?
C9 C8 N1 112.0(10) . . ?
C9 C8 H8 124.0 . . ?
N1 C8 H8 124.0 . . ?
C8 C9 N2 104.8(11) . . ?
C8 C9 H9 127.6 . . ?
N2 C9 H9 127.6 . . ?
N3 C10 N4 112.7(10) . . ?
N3 C10 H10 123.6 . . ?
N4 C10 H10 123.6 . . ?
N3 C11 C12 112.5(11) . . ?
N3 C11 H11 123.8 . . ?
C12 C11 H11 123.8 . . ?
C11 C12 N4 103.4(11) . . ?
C11 C12 H12 128.3 . . ?
N4 C12 H12 128.3 . . ?
N5 C13 N6 110.9(10) . . ?
N5 C13 H13 124.5 . . ?
N6 C13 H13 124.5 . . ?
N5 C14 C15 111.2(11) . . ?
N5 C14 H14 124.4 . . ?
C15 C14 H14 124.4 . . ?
C14 C15 N6 104.8(11) . . ?
C14 C15 H15 127.6 . . ?
N6 C15 H15 127.6 . . ?
C21 C16 C17 117.4(10) . . ?
C21 C16 H16 121.3 . . ?
C17 C16 H16 121.3 . . ?
N8 C17 C18 120.0(10) . . ?
N8 C17 C16 118.7(10) . . ?
C18 C17 C16 121.3(10) . . ?
C19 C18 C17 118.0(10) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
C20 C19 C18 122.8(11) . . ?
C20 C19 N10 118.1(10) . . ?
C18 C19 N10 118.5(9) . . ?
C19 C20 C21 118.2(10) . . ?
C19 C20 H20 120.9 . . ?
C21 C20 H20 120.9 . . ?
C20 C21 C16 121.8(10) . . ?
C20 C21 N12 121.6(10) . . ?
C16 C21 N12 116.2(10) . . ?
N7 C22 N8 111.4(10) . . ?
N7 C22 H22 124.3 . . ?
N8 C22 H22 124.3 . . ?
C57 C23 N7 109.7(11) . . ?
C57 C23 H23 125.1 . . ?
N7 C23 H23 125.1 . . ?
N9 C25 N10 119.4(11) . . ?
N9 C25 H25 120.3 . . ?
N10 C25 H25 120.3 . . ?
N9 C26 C27 110.5(11) . . ?
N9 C26 H26 124.8 . . ?
C27 C26 H26 124.8 . . ?
C26 C27 N10 104.4(10) . . ?
C26 C27 H27 127.8 . . ?
N10 C27 H27 127.8 . . ?
N12 C28 C29 109.0(12) . . ?
N12 C28 H28 125.5 . . ?
C29 C28 H28 125.5 . . ?
N11 C29 C28 110.3(11) . . ?
N11 C29 H29 124.9 . . ?
C28 C29 H29 124.9 . . ?
N11 C30 N12 113.2(10) . . ?
N11 C30 H30 123.4 . . ?
N12 C30 H30 123.4 . . ?
O2 C31 O1 127.9(12) . . ?
O2 C31 C32 117.0(12) . . ?
O1 C31 C32 114.9(12) . . ?
O2 C31 Cd1 66.9(7) . . ?
O1 C31 Cd1 61.0(6) . . ?
C32 C31 Cd1 175.6(10) . . ?
C33 C32 C36 119.6(13) . . ?
C33 C32 C31 121.9(13) . . ?
C36 C32 C31 118.2(12) . . ?
C32 C33 C34 122.8(15) . . ?
C32 C33 H33 118.6 . . ?
C34 C33 H33 118.6 . . ?
C35 C34 C33 125.9(14) . . ?
C35 C34 C34 115.0(16) . 2_566 ?
C33 C34 C34 119.0(19) . 2_566 ?
C36 C35 C34 125.5(15) 2_566 . ?
C36 C35 H35 117.2 2_566 . ?
C34 C35 H35 117.2 . . ?
C35 C36 C32 117.8(15) 2_566 . ?
C35 C36 H36 121.1 2_566 . ?
C32 C36 H36 121.1 . . ?
O7 C39 O6 121.4(12) . . ?
O7 C39 C40 120.1(13) . . ?
O6 C39 C40 118.5(13) . . ?
O7 C39 Cd2 59.0(6) . . ?
O6 C39 Cd2 62.4(6) . . ?
C40 C39 Cd2 179.1(12) . . ?
C41 C40 C44 118.2(13) . . ?
C41 C40 C39 121.6(14) . . ?
C44 C40 C39 120.1(13) . . ?
C40 C41 C42 122.3(16) . . ?
C40 C41 H41 118.9 . . ?
C42 C41 H41 118.9 . . ?
C42 C42 C43 124.6(18) 2_676 . ?
C42 C42 C41 114.8(19) 2_676 . ?
C43 C42 C41 120.4(14) . . ?
C44 C43 C42 118.3(16) 2_676 . ?
C44 C43 H43 120.8 2_676 . ?
C42 C43 H43 120.8 . . ?
C43 C44 C40 121.6(16) 2_676 . ?
C43 C44 H44 119.2 2_676 . ?
C40 C44 H44 119.2 . . ?
C23 C57 N8 106.9(10) . . ?
C23 C57 H57 126.5 . . ?
N8 C57 H57 126.5 . . ?
C31 O1 Cd1 91.5(7) . . ?
C31 O2 Cd1 86.7(8) . . ?
N13 O3 Cd1 95.0(6) . . ?
N13 O4 Cd1 93.1(6) . . ?
C39 O6 Cd2 90.5(8) . . ?
C39 O7 Cd2 94.4(8) . . ?
N14 O8 Cd2 97.2(7) . . ?
N14 O9 Cd2 95.4(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 2.8(16) . . . . ?
C6 C1 C2 N2 -179.8(9) . . . . ?
C7 N2 C2 C1 -53.0(15) . . . . ?
C9 N2 C2 C1 136.7(12) . . . . ?
C7 N2 C2 C3 124.4(11) . . . . ?
C9 N2 C2 C3 -45.9(15) . . . . ?
C1 C2 C3 C4 -0.1(17) . . . . ?
N2 C2 C3 C4 -177.4(10) . . . . ?
C2 C3 C4 C5 -5.8(18) . . . . ?
C2 C3 C4 N4 174.9(10) . . . . ?
C10 N4 C4 C3 3.5(18) . . . . ?
C12 N4 C4 C3 -165.9(12) . . . . ?
C10 N4 C4 C5 -175.8(11) . . . . ?
C12 N4 C4 C5 14.8(17) . . . . ?
C3 C4 C5 C6 8.2(18) . . . . ?
N4 C4 C5 C6 -172.4(10) . . . . ?
C4 C5 C6 C1 -5.1(17) . . . . ?
C4 C5 C6 N6 176.0(10) . . . . ?
C2 C1 C6 C5 -0.1(17) . . . . ?
C2 C1 C6 N6 178.8(9) . . . . ?
C13 N6 C6 C5 156.0(11) . . . . ?
C15 N6 C6 C5 -17.9(18) . . . . ?
C13 N6 C6 C1 -23.0(16) . . . . ?
C15 N6 C6 C1 163.1(13) . . . . ?
C8 N1 C7 N2 2.4(12) . . . . ?
Cd1 N1 C7 N2 162.0(7) . . . . ?
C9 N2 C7 N1 -3.0(13) . . . . ?
C2 N2 C7 N1 -174.8(9) . . . . ?
C7 N1 C8 C9 -0.8(14) . . . . ?
Cd1 N1 C8 C9 -159.7(9) . . . . ?
N1 C8 C9 N2 -0.9(15) . . . . ?
C7 N2 C9 C8 2.2(14) . . . . ?
C2 N2 C9 C8 174.2(10) . . . . ?
C11 N3 C10 N4 -1.6(14) . . . . ?
Cd2 N3 C10 N4 160.4(8) . . . . ?
C12 N4 C10 N3 0.2(14) . . . . ?
C4 N4 C10 N3 -170.8(11) . . . . ?
C10 N3 C11 C12 2.5(16) . . . . ?
Cd2 N3 C11 C12 -160.9(9) . . . . ?
N3 C11 C12 N4 -2.3(16) . . . . ?
C10 N4 C12 C11 1.3(14) . . . . ?
C4 N4 C12 C11 172.6(11) . . . . ?
C14 N5 C13 N6 2.1(13) . . . . ?
Cd2 N5 C13 N6 169.7(7) 1_455 . . . ?
C15 N6 C13 N5 -2.2(14) . . . . ?
C6 N6 C13 N5 -177.0(10) . . . . ?
C13 N5 C14 C15 -1.2(16) . . . . ?
Cd2 N5 C14 C15 -170.5(10) 1_455 . . . ?
N5 C14 C15 N6 -0.1(17) . . . . ?
C13 N6 C15 C14 1.4(16) . . . . ?
C6 N6 C15 C14 176.2(11) . . . . ?
C57 N8 C17 C18 -158.5(12) . . . . ?
C22 N8 C17 C18 24.9(15) . . . . ?
C57 N8 C17 C16 20.6(17) . . . . ?
C22 N8 C17 C16 -155.9(10) . . . . ?
C21 C16 C17 N8 178.4(9) . . . . ?
C21 C16 C17 C18 -2.5(15) . . . . ?
N8 C17 C18 C19 -175.6(9) . . . . ?
C16 C17 C18 C19 5.2(15) . . . . ?
C17 C18 C19 C20 -7.6(15) . . . . ?
C17 C18 C19 N10 -178.0(8) . . . . ?
C25 N10 C19 C20 -128.0(12) . . . . ?
C27 N10 C19 C20 44.8(15) . . . . ?
C25 N10 C19 C18 42.8(15) . . . . ?
C27 N10 C19 C18 -144.4(11) . . . . ?
C18 C19 C20 C21 7.1(16) . . . . ?
N10 C19 C20 C21 177.5(9) . . . . ?
C19 C20 C21 C16 -4.1(16) . . . . ?
C19 C20 C21 N12 -176.4(9) . . . . ?
C17 C16 C21 C20 1.9(16) . . . . ?
C17 C16 C21 N12 174.6(9) . . . . ?
C28 N12 C21 C20 166.1(13) . . . . ?
C30 N12 C21 C20 -5.9(17) . . . . ?
C28 N12 C21 C16 -6.6(18) . . . . ?
C30 N12 C21 C16 -178.7(10) . . . . ?
C23 N7 C22 N8 0.7(12) . . . . ?
Cd1 N7 C22 N8 -171.3(7) . . . . ?
C57 N8 C22 N7 -1.4(13) . . . . ?
C17 N8 C22 N7 175.8(9) . . . . ?
C22 N7 C23 C57 0.2(15) . . . . ?
Cd1 N7 C23 C57 173.2(9) . . . . ?
C26 N9 C25 N10 6.6(14) . . . . ?
Cd2 N9 C25 N10 -157.7(7) . . . . ?
C27 N10 C25 N9 -2.3(13) . . . . ?
C19 N10 C25 N9 171.8(10) . . . . ?
C25 N9 C26 C27 -8.3(14) . . . . ?
Cd2 N9 C26 C27 157.2(9) . . . . ?
N9 C26 C27 N10 7.2(15) . . . . ?
C25 N10 C27 C26 -3.2(13) . . . . ?
C19 N10 C27 C26 -177.6(10) . . . . ?
C30 N12 C28 C29 0.7(16) . . . . ?
C21 N12 C28 C29 -172.7(12) . . . . ?
C30 N11 C29 C28 -1.3(17) . . . . ?
Cd1 N11 C29 C28 159.8(10) 1_655 . . . ?
N12 C28 C29 N11 0.4(19) . . . . ?
C29 N11 C30 N12 1.8(14) . . . . ?
Cd1 N11 C30 N12 -157.7(7) 1_655 . . . ?
C28 N12 C30 N11 -1.6(14) . . . . ?
C21 N12 C30 N11 172.2(10) . . . . ?
O2 C31 C32 C33 -176.3(16) . . . . ?
O1 C31 C32 C33 9(2) . . . . ?
O2 C31 C32 C36 -2(2) . . . . ?
O1 C31 C32 C36 -177.3(14) . . . . ?
C36 C32 C33 C34 6(3) . . . . ?
C31 C32 C33 C34 179.6(16) . . . . ?
C32 C33 C34 C35 177.7(19) . . . . ?
C32 C33 C34 C34 -4(4) . . . 2_566 ?
C33 C34 C35 C36 179(2) . . . 2_566 ?
C34 C34 C35 C36 1(4) 2_566 . . 2_566 ?
C33 C32 C36 C35 -4(3) . . . 2_566 ?
C31 C32 C36 C35 -178.5(16) . . . 2_566 ?
O7 C39 C40 C41 176.7(14) . . . . ?
O6 C39 C40 C41 -1(2) . . . . ?
O7 C39 C40 C44 -3(2) . . . . ?
O6 C39 C40 C44 179.4(15) . . . . ?
C44 C40 C41 C42 -3(3) . . . . ?
C39 C40 C41 C42 177.3(14) . . . . ?
C40 C41 C42 C42 4(3) . . . 2_676 ?
C40 C41 C42 C43 179.3(17) . . . . ?
C42 C42 C43 C44 -5(4) 2_676 . . 2_676 ?
C41 C42 C43 C44 -179.6(19) . . . 2_676 ?
C41 C40 C44 C43 3(3) . . . 2_676 ?
C39 C40 C44 C43 -177.6(18) . . . 2_676 ?
N7 C23 C57 N8 -1.1(16) . . . . ?
C22 N8 C57 C23 1.4(15) . . . . ?
C17 N8 C57 C23 -175.7(11) . . . . ?
O2 C31 O1 Cd1 3.7(16) . . . . ?
C32 C31 O1 Cd1 178.1(10) . . . . ?
O1 C31 O2 Cd1 -3.6(15) . . . . ?
C32 C31 O2 Cd1 -177.9(11) . . . . ?
O5 N13 O3 Cd1 179.3(9) . . . . ?
O4 N13 O3 Cd1 -3.0(10) . . . . ?
O5 N13 O4 Cd1 -179.3(9) . . . . ?
O3 N13 O4 Cd1 3.0(10) . . . . ?
O7 C39 O6 Cd2 2.9(13) . . . . ?
C40 C39 O6 Cd2 -179.6(11) . . . . ?
O6 C39 O7 Cd2 -3.0(14) . . . . ?
C40 C39 O7 Cd2 179.6(11) . . . . ?
O10 N14 O8 Cd2 178.8(10) . . . . ?
O9 N14 O8 Cd2 -2.1(10) . . . . ?
O10 N14 O9 Cd2 -178.8(9) . . . . ?
O8 N14 O9 Cd2 2.1(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C28 H28 O8 0.93 2.55 3.317(16) 140.0 1_545
C27 H27 O10 0.93 2.65 3.301(17) 127.1 2_675
C22 H22 O3 0.93 2.65 3.313(14) 128.5 2_565
C12 H12 O4 0.93 2.62 3.285(14) 129.2 1_565
C7 H7 O2 0.93 2.53 3.107(13) 120.1 .
C5 H5 O4 0.93 2.61 3.491(15) 157.3 1_565
C5 H5 O4 0.93 2.61 3.491(15) 157.3 1_565
C7 H7 O2 0.93 2.53 3.107(13) 120.1 .
C12 H12 O4 0.93 2.62 3.285(14) 129.2 1_565
C22 H22 O3 0.93 2.65 3.313(14) 128.5 2_565
C27 H27 O10 0.93 2.65 3.301(17) 127.1 2_675
C28 H28 O8 0.93 2.55 3.317(16) 140.0 1_545

_refine_diff_density_max         1.725
_refine_diff_density_min         -1.914
_refine_diff_density_rms         0.150


####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1564038'
_audit_update_record             
;
2017-09-09 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H14 N4 O4 Zn'
_chemical_formula_weight         463.74

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   19.1253(9)
_cell_length_b                   19.1253(9)
_cell_length_c                   8.5716(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2715.2(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4126
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      25.60

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.399
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5736
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14072
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.130
_diffrn_reflns_theta_max         25.716
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3463
_reflns_number_gt                2814
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0479P)²+2.1932P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3463
_refine_ls_number_parameters     416
_refine_ls_number_restraints     166
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.36967(2) 0.33827(2) 0.07096(4) 0.02827(12) Uani 1 1 d D . . . .
N1 N 0.32658(13) 0.40715(13) -0.0075(3) 0.0267(5) Uani 1 1 d . . . . .
N2 N 0.31036(13) 0.51010(12) -0.0583(3) 0.0249(5) Uani 1 1 d . . . . .
N3 N 0.27630(14) 0.23628(14) 0.1739(3) 0.0345(6) Uani 1 1 d . . . . .
N4 N 0.16174(15) 0.12401(15) 0.2221(3) 0.0408(6) Uani 1 1 d . . . . .
C1 C 0.40003(15) 0.65526(15) -0.0558(3) 0.0268(6) Uani 1 1 d . . . . .
H1 H 0.444403 0.647656 -0.055563 0.032 Uiso 1 1 calc R U . . .
C2 C 0.32206(16) 0.58981(15) -0.0560(3) 0.0252(6) Uani 1 1 d . . . . .
C3 C 0.35532(16) 0.48475(16) 0.0166(3) 0.0267(6) Uani 1 1 d . . . . .
H3 H 0.400436 0.517462 0.077115 0.032 Uiso 1 1 calc R U . . .
C4 C 0.26049(17) 0.38207(16) -0.1034(4) 0.0310(6) Uani 1 1 d . . . . .
H4 H 0.228454 0.329718 -0.140359 0.037 Uiso 1 1 calc R U . . .
C5 C 0.24914(16) 0.44450(16) -0.1356(4) 0.0301(6) Uani 1 1 d . . . . .
H5 H 0.208670 0.443754 -0.196993 0.036 Uiso 1 1 calc R U . . .
C6 C 0.06227(19) -0.01849(19) 0.2139(4) 0.0405(8) Uani 1 1 d . . . . .
H6 H 0.103572 -0.030770 0.213968 0.049 Uiso 1 1 calc R U . . .
C7 C 0.07937(18) 0.06115(18) 0.2138(4) 0.0392(7) Uani 1 1 d . . . . .
C8 C 0.20186(19) 0.18961(19) 0.1285(4) 0.0413(8) Uani 1 1 d . . . . .
H8 H 0.179023 0.200069 0.042227 0.050 Uiso 1 1 calc R U . . .
C9 C 0.2850(2) 0.1996(2) 0.3066(4) 0.0434(8) Uani 1 1 d . . . . .
H9 H 0.331605 0.219674 0.366620 0.052 Uiso 1 1 calc R U . . .
C10 C 0.2152(2) 0.1301(2) 0.3353(4) 0.0484(9) Uani 1 1 d . . . . .
H10 H 0.205408 0.093660 0.415697 0.058 Uiso 1 1 calc R U . . .
C11 C 0.4931(4) 0.4397(3) 0.2643(7) 0.0349(13) Uani 0.814(4) 1 d D . P A 1
C12 C 0.5615(4) 0.4633(3) 0.3793(10) 0.0317(13) Uani 0.814(4) 1 d D . P A 1
C13 C 0.5739(3) 0.4064(3) 0.4588(6) 0.0459(12) Uani 0.814(4) 1 d D . P A 1
H13 H 0.538498 0.351645 0.443049 0.055 Uiso 0.814(4) 1 calc R U P A 1
C14 C 0.6370(3) 0.4303(3) 0.5586(6) 0.0494(12) Uani 0.814(4) 1 d D . P A 1
H14 H 0.643385 0.391263 0.611101 0.059 Uiso 0.814(4) 1 calc R U P A 1
C15 C 0.6927(3) 0.5119(3) 0.5844(6) 0.0338(11) Uani 0.814(4) 1 d D . P A 1
C16 C 0.6805(3) 0.5703(3) 0.5070(6) 0.0307(12) Uani 0.814(4) 1 d D . P A 1
C17 C 0.6127(2) 0.5440(2) 0.4049(5) 0.0342(9) Uani 0.814(4) 1 d D . P A 1
H17 H 0.603336 0.581853 0.355748 0.041 Uiso 0.814(4) 1 calc R U P A 1
C18 C 0.7619(2) 0.5396(3) 0.6839(5) 0.0349(9) Uani 0.814(4) 1 d D . P A 1
H18 H 0.770622 0.501958 0.735732 0.042 Uiso 0.814(4) 1 calc R U P A 1
C19 C 0.8147(3) 0.6191(3) 0.7042(7) 0.0305(11) Uani 0.814(4) 1 d D . P A 1
C20 C 0.8012(3) 0.6758(3) 0.6266(5) 0.0381(10) Uani 0.814(4) 1 d D . P A 1
H20 H 0.837423 0.730565 0.640549 0.046 Uiso 0.814(4) 1 calc R U P A 1
C21 C 0.7365(2) 0.6528(2) 0.5314(5) 0.0411(10) Uani 0.814(4) 1 d D . P A 1
H21 H 0.729071 0.691822 0.481811 0.049 Uiso 0.814(4) 1 calc R U P A 1
C22 C 0.8881(2) 0.6498(2) 0.8085(4) 0.0335(7) Uani 0.814(4) 1 d D . P A 1
O1 O 0.4516(2) 0.3643(2) 0.2322(5) 0.0432(9) Uani 0.814(4) 1 d D . P A 1
O2 O 0.4819(2) 0.4898(2) 0.2030(5) 0.0692(12) Uani 0.814(4) 1 d D . P A 1
O3 O 0.9382(3) 0.7205(2) 0.8109(10) 0.0492(13) Uani 0.814(4) 1 d D . P A 1
O4 O 0.8911(6) 0.5938(4) 0.8900(12) 0.0389(18) Uani 0.814(4) 1 d D . P A 1
C11A C 0.4867(16) 0.4164(12) 0.278(3) 0.038(5) Uani 0.186(4) 1 d D . P A 2
C12A C 0.5573(17) 0.4788(12) 0.373(4) 0.026(4) Uani 0.186(4) 1 d D . P A 2
C13A C 0.5908(9) 0.5640(9) 0.3711(19) 0.030(3) Uani 0.186(4) 1 d D . P A 2
H13A H 0.566987 0.587075 0.311546 0.036 Uiso 0.186(4) 1 calc R U P A 2
C14A C 0.6584(8) 0.6117(9) 0.4573(16) 0.029(3) Uani 0.186(4) 1 d D . P A 2
H14A H 0.678424 0.667129 0.457513 0.035 Uiso 0.186(4) 1 calc R U P A 2
C15A C 0.6989(12) 0.5813(10) 0.545(3) 0.022(4) Uani 0.186(4) 1 d D . P A 2
C16A C 0.6664(10) 0.4961(9) 0.547(2) 0.028(4) Uani 0.186(4) 1 d D . P A 2
C17A C 0.5949(10) 0.4473(11) 0.458(2) 0.037(4) Uani 0.186(4) 1 d D . P A 2
H17A H 0.573212 0.391561 0.458709 0.044 Uiso 0.186(4) 1 calc R U P A 2
C18A C 0.7713(8) 0.6282(9) 0.6341(16) 0.024(3) Uani 0.186(4) 1 d D . P A 2
H18A H 0.793500 0.683907 0.637659 0.028 Uiso 0.186(4) 1 calc R U P A 2
C19A C 0.8086(15) 0.5949(10) 0.713(4) 0.029(4) Uani 0.186(4) 1 d D . P A 2
C20A C 0.7746(10) 0.5105(9) 0.714(2) 0.038(4) Uani 0.186(4) 1 d D . P A 2
H20A H 0.799324 0.487032 0.768997 0.046 Uiso 0.186(4) 1 calc R U P A 2
C21A C 0.7053(9) 0.4635(9) 0.633(2) 0.047(5) Uani 0.186(4) 1 d D . P A 2
H21A H 0.683071 0.407781 0.635721 0.056 Uiso 0.186(4) 1 calc R U P A 2
C22A C 0.880760 0.642050 0.819540 0.0335(7) Uani 0.186(4) 1 d D . P A 2
O1A O 0.4626(11) 0.4430(10) 0.166(2) 0.083(5) Uani 0.186(4) 1 d D . P A 2
O2A O 0.4527(12) 0.3438(10) 0.297(2) 0.061(5) Uani 0.186(4) 1 d D . P A 2
O3A O 0.900(3) 0.6072(19) 0.914(5) 0.033(4) Uani 0.186(4) 1 d D . P A 2
O4A O 0.9150(14) 0.7214(10) 0.805(5) 0.052(7) Uani 0.186(4) 1 d D . P A 2


_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
Zn1 O3A 1.77(2) 2_654 ?
Zn1 O1 1.958(3) . ?
Zn1 N1 1.988(2) . ?
Zn1 O4 2.014(5) 2_654 ?
Zn1 O1A 2.066(15) . ?
Zn1 N3 2.071(2) . ?
Zn1 O2A 2.476(19) . ?
N1 C3 1.316(3) . ?
N1 C4 1.378(4) . ?
N2 C3 1.343(3) . ?
N2 C5 1.384(3) . ?
N2 C2 1.426(3) . ?
N3 C8 1.306(4) . ?
N3 C9 1.389(4) . ?
N4 C8 1.358(4) . ?
N4 C10 1.371(4) . ?
N4 C7 1.428(4) . ?
C1 C2 1.386(4) 2_665 ?
C1 C2 1.387(4) . ?
C1 H1 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.345(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.389(4) . ?
C6 C7 1.390(4) 3 ?
C6 H6 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.355(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 O2 1.202(6) . ?
C11 O1 1.281(5) . ?
C11 C12 1.516(6) . ?
C12 C17 1.370(6) . ?
C12 C13 1.400(7) . ?
C13 C14 1.359(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.399(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.415(5) . ?
C15 C18 1.434(6) . ?
C16 C21 1.411(6) . ?
C16 C17 1.431(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.351(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.402(6) . ?
C19 C22 1.514(5) . ?
C20 C21 1.358(5) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 O3 1.204(6) . ?
C22 O4 1.304(7) . ?
C11A O2A 1.214(18) . ?
C11A O1A 1.278(17) . ?
C11A C12A 1.517(15) . ?
C12A C17A 1.359(17) . ?
C12A C13A 1.422(18) . ?
C13A C14A 1.367(15) . ?
C13A H13A 0.9300 . ?
C14A C15A 1.399(15) . ?
C14A H14A 0.9300 . ?
C15A C16A 1.424(15) . ?
C15A C18A 1.436(16) . ?
C16A C21A 1.398(15) . ?
C16A C17A 1.429(16) . ?
C17A H17A 0.9300 . ?
C18A C19A 1.349(16) . ?
C18A H18A 0.9300 . ?
C19A C20A 1.406(16) . ?
C19A C22A 1.520(13) . ?
C20A C21A 1.359(15) . ?
C20A H20A 0.9300 . ?
C21A H21A 0.9300 . ?
C22A O3A 1.217(18) . ?
C22A O4A 1.324(16) . ?

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
O3A Zn1 N1 111(2) 2_654 . ?
O1 Zn1 N1 127.91(12) . . ?
O1 Zn1 O4 104.7(3) . 2_654 ?
N1 Zn1 O4 109.7(4) . 2_654 ?
O3A Zn1 O1A 117.9(12) 2_654 . ?
N1 Zn1 O1A 86.1(5) . . ?
O3A Zn1 N3 99.9(15) 2_654 . ?
O1 Zn1 N3 98.18(14) . . ?
N1 Zn1 N3 108.69(10) . . ?
O4 Zn1 N3 105.4(3) 2_654 . ?
O1A Zn1 N3 131.6(6) . . ?
O3A Zn1 O2A 107.7(18) 2_654 . ?
N1 Zn1 O2A 134.9(4) . . ?
O1A Zn1 O2A 55.1(5) . . ?
N3 Zn1 O2A 86.5(5) . . ?
C3 N1 C4 106.2(2) . . ?
C3 N1 Zn1 128.06(19) . . ?
C4 N1 Zn1 125.68(17) . . ?
C3 N2 C5 107.8(2) . . ?
C3 N2 C2 126.3(2) . . ?
C5 N2 C2 125.8(2) . . ?
C8 N3 C9 105.3(3) . . ?
C8 N3 Zn1 130.4(2) . . ?
C9 N3 Zn1 124.1(2) . . ?
C8 N4 C10 106.7(3) . . ?
C8 N4 C7 128.7(3) . . ?
C10 N4 C7 124.6(3) . . ?
C2 C1 C2 118.4(3) 2_665 . ?
C2 C1 H1 120.8 2_665 . ?
C2 C1 H1 120.8 . . ?
C1 C2 C1 121.6(3) 3_565 . ?
C1 C2 N2 119.2(2) 3_565 . ?
C1 C2 N2 119.2(2) . . ?
N1 C3 N2 110.5(2) . . ?
N1 C3 H3 124.7 . . ?
N2 C3 H3 124.7 . . ?
C5 C4 N1 109.9(2) . . ?
C5 C4 H4 125.0 . . ?
N1 C4 H4 125.0 . . ?
C4 C5 N2 105.5(2) . . ?
C4 C5 H5 127.2 . . ?
N2 C5 H5 127.2 . . ?
C7 C6 C7 118.3(3) . 3 ?
C7 C6 H6 120.9 . . ?
C7 C6 H6 120.9 3 . ?
C6 C7 C6 121.7(3) . 2 ?
C6 C7 N4 118.6(3) . . ?
C6 C7 N4 119.6(3) 2 . ?
N3 C8 N4 112.0(3) . . ?
N3 C8 H8 124.0 . . ?
N4 C8 H8 124.0 . . ?
C10 C9 N3 109.6(3) . . ?
C10 C9 H9 125.2 . . ?
N3 C9 H9 125.2 . . ?
C9 C10 N4 106.4(3) . . ?
C9 C10 H10 126.8 . . ?
N4 C10 H10 126.8 . . ?
O2 C11 O1 123.1(4) . . ?
O2 C11 C12 121.2(4) . . ?
O1 C11 C12 115.6(4) . . ?
C17 C12 C13 119.6(4) . . ?
C17 C12 C11 117.7(5) . . ?
C13 C12 C11 122.8(4) . . ?
C14 C13 C12 120.8(4) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 121.8(4) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C14 C15 C16 118.2(4) . . ?
C14 C15 C18 123.6(4) . . ?
C16 C15 C18 118.2(4) . . ?
C21 C16 C15 118.7(4) . . ?
C21 C16 C17 122.1(4) . . ?
C15 C16 C17 119.1(4) . . ?
C12 C17 C16 120.4(4) . . ?
C12 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C19 C18 C15 121.7(4) . . ?
C19 C18 H18 119.2 . . ?
C15 C18 H18 119.2 . . ?
C18 C19 C20 119.1(4) . . ?
C18 C19 C22 122.6(4) . . ?
C20 C19 C22 118.3(4) . . ?
C21 C20 C19 121.6(4) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C20 C21 C16 120.7(4) . . ?
C20 C21 H21 119.6 . . ?
C16 C21 H21 119.6 . . ?
O3 C22 O4 125.2(4) . . ?
O3 C22 C19 120.5(4) . . ?
O4 C22 C19 114.3(4) . . ?
C11 O1 Zn1 113.9(3) . . ?
C22 O4 Zn1 117.1(5) . 3_666 ?
O2A C11A O1A 117.7(16) . . ?
O2A C11A C12A 125.7(18) . . ?
O1A C11A C12A 116.6(17) . . ?
C17A C12A C13A 118.7(14) . . ?
C17A C12A C11A 113.5(16) . . ?
C13A C12A C11A 127.5(16) . . ?
C14A C13A C12A 119.5(14) . . ?
C14A C13A H13A 120.3 . . ?
C12A C13A H13A 120.3 . . ?
C13A C14A C15A 123.3(14) . . ?
C13A C14A H14A 118.4 . . ?
C15A C14A H14A 118.4 . . ?
C14A C15A C16A 117.7(12) . . ?
C14A C15A C18A 126.0(14) . . ?
C16A C15A C18A 116.2(12) . . ?
C21A C16A C15A 119.4(12) . . ?
C21A C16A C17A 122.6(14) . . ?
C15A C16A C17A 118.0(13) . . ?
C12A C17A C16A 122.7(15) . . ?
C12A C17A H17A 118.6 . . ?
C16A C17A H17A 118.6 . . ?
C19A C18A C15A 122.9(14) . . ?
C19A C18A H18A 118.6 . . ?
C15A C18A H18A 118.6 . . ?
C18A C19A C20A 119.6(13) . . ?
C18A C19A C22A 124.0(13) . . ?
C20A C19A C22A 116.0(12) . . ?
C21A C20A C19A 119.7(14) . . ?
C21A C20A H20A 120.2 . . ?
C19A C20A H20A 120.2 . . ?
C20A C21A C16A 122.3(14) . . ?
C20A C21A H21A 118.9 . . ?
C16A C21A H21A 118.9 . . ?
O3A C22A O4A 125.3(17) . . ?
O3A C22A C19A 120.6(17) . . ?
O4A C22A C19A 113.9(13) . . ?
C11A O1A Zn1 102.5(12) . . ?
C11A O2A Zn1 84.7(12) . . ?
C22A O3A Zn1 139(2) . 3_666 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C1 -0.2(6) 2_665 . . 3_565 ?
C2 C1 C2 N2 179.01(18) 2_665 . . . ?
C3 N2 C2 C1 -143.2(3) . . . 3_565 ?
C5 N2 C2 C1 35.1(4) . . . 3_565 ?
C3 N2 C2 C1 37.5(4) . . . . ?
C5 N2 C2 C1 -144.1(3) . . . . ?
C4 N1 C3 N2 0.5(3) . . . . ?
Zn1 N1 C3 N2 178.80(18) . . . . ?
C5 N2 C3 N1 -0.2(3) . . . . ?
C2 N2 C3 N1 178.4(2) . . . . ?
C3 N1 C4 C5 -0.6(3) . . . . ?
Zn1 N1 C4 C5 -179.0(2) . . . . ?
N1 C4 C5 N2 0.4(3) . . . . ?
C3 N2 C5 C4 -0.2(3) . . . . ?
C2 N2 C5 C4 -178.7(3) . . . . ?
C7 C6 C7 C6 0.1(7) 3 . . 2 ?
C7 C6 C7 N4 176.8(2) 3 . . . ?
C8 N4 C7 C6 128.7(4) . . . . ?
C10 N4 C7 C6 -54.2(5) . . . . ?
C8 N4 C7 C6 -54.5(5) . . . 2 ?
C10 N4 C7 C6 122.6(4) . . . 2 ?
C9 N3 C8 N4 -0.9(4) . . . . ?
Zn1 N3 C8 N4 174.0(2) . . . . ?
C10 N4 C8 N3 0.1(4) . . . . ?
C7 N4 C8 N3 177.6(3) . . . . ?
C8 N3 C9 C10 1.4(4) . . . . ?
Zn1 N3 C9 C10 -173.9(2) . . . . ?
N3 C9 C10 N4 -1.4(4) . . . . ?
C8 N4 C10 C9 0.8(4) . . . . ?
C7 N4 C10 C9 -176.9(3) . . . . ?
O2 C11 C12 C17 -3.4(12) . . . . ?
O1 C11 C12 C17 173.4(6) . . . . ?
O2 C11 C12 C13 176.7(7) . . . . ?
O1 C11 C12 C13 -6.6(12) . . . . ?
C17 C12 C13 C14 -1.3(11) . . . . ?
C11 C12 C13 C14 178.6(7) . . . . ?
C12 C13 C14 C15 -1.0(9) . . . . ?
C13 C14 C15 C16 1.9(8) . . . . ?
C13 C14 C15 C18 -177.5(5) . . . . ?
C14 C15 C16 C21 -179.6(5) . . . . ?
C18 C15 C16 C21 -0.2(8) . . . . ?
C14 C15 C16 C17 -0.5(8) . . . . ?
C18 C15 C16 C17 178.9(4) . . . . ?
C13 C12 C17 C16 2.7(10) . . . . ?
C11 C12 C17 C16 -177.3(7) . . . . ?
C21 C16 C17 C12 177.3(6) . . . . ?
C15 C16 C17 C12 -1.8(9) . . . . ?
C14 C15 C18 C19 179.3(5) . . . . ?
C16 C15 C18 C19 -0.1(7) . . . . ?
C15 C18 C19 C20 0.3(8) . . . . ?
C15 C18 C19 C22 -179.9(5) . . . . ?
C18 C19 C20 C21 -0.1(8) . . . . ?
C22 C19 C20 C21 -179.9(4) . . . . ?
C19 C20 C21 C16 -0.3(7) . . . . ?
C15 C16 C21 C20 0.4(8) . . . . ?
C17 C16 C21 C20 -178.7(5) . . . . ?
C18 C19 C22 O3 172.1(7) . . . . ?
C20 C19 C22 O3 -8.1(9) . . . . ?
C18 C19 C22 O4 -7.3(10) . . . . ?
C20 C19 C22 O4 172.5(8) . . . . ?
O2 C11 O1 Zn1 1.2(9) . . . . ?
C12 C11 O1 Zn1 -175.4(6) . . . . ?
O3 C22 O4 Zn1 16.3(14) . . . 3_666 ?
C19 C22 O4 Zn1 -164.3(6) . . . 3_666 ?
O2A C11A C12A C17A 16(5) . . . . ?
O1A C11A C12A C17A -162(3) . . . . ?
O2A C11A C12A C13A -169(3) . . . . ?
O1A C11A C12A C13A 12(6) . . . . ?
C17A C12A C13A C14A -2(4) . . . . ?
C11A C12A C13A C14A -176(3) . . . . ?
C12A C13A C14A C15A 2(3) . . . . ?
C13A C14A C15A C16A -2(3) . . . . ?
C13A C14A C15A C18A 178(2) . . . . ?
C14A C15A C16A C21A 180(2) . . . . ?
C18A C15A C16A C21A 0(4) . . . . ?
C14A C15A C16A C17A 0(4) . . . . ?
C18A C15A C16A C17A -179(2) . . . . ?
C13A C12A C17A C16A 1(5) . . . . ?
C11A C12A C17A C16A 175(3) . . . . ?
C21A C16A C17A C12A -179(3) . . . . ?
C15A C16A C17A C12A 0(4) . . . . ?
C14A C15A C18A C19A -178(3) . . . . ?
C16A C15A C18A C19A 2(4) . . . . ?
C15A C18A C19A C20A -2(4) . . . . ?
C15A C18A C19A C22A -174(2) . . . . ?
C18A C19A C20A C21A 1(4) . . . . ?
C22A C19A C20A C21A 174(2) . . . . ?
C19A C20A C21A C16A 1(4) . . . . ?
C15A C16A C21A C20A -1(4) . . . . ?
C17A C16A C21A C20A 178(2) . . . . ?
C18A C19A C22A O3A 163(4) . . . . ?
C20A C19A C22A O3A -9(5) . . . . ?
C18A C19A C22A O4A -13(4) . . . . ?
C20A C19A C22A O4A 175(3) . . . . ?
O2A C11A O1A Zn1 1(3) . . . . ?
C12A C11A O1A Zn1 179(3) . . . . ?
O1A C11A O2A Zn1 0(3) . . . . ?
C12A C11A O2A Zn1 -179(4) . . . . ?
O4A C22A O3A Zn1 3(9) . . . 3_666 ?
C19A C22A O3A Zn1 -172(5) . . . 3_666 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C6 H6 O3 0.93 2.54 3.468(5) 175.0 6_546
C5 H5 O1 0.93 2.42 3.272(5) 152.5 6
C3 H3 O2 0.93 2.17 2.861(4) 130.7 .
C1 H1 O1 0.93 2.60 3.397(5) 144.2 4_665

_refine_diff_density_max         0.814
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.064

