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

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

data_1-sr
_database_code_depnum_ccdc_archive 'CCDC 1444248'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H17 N4 O12 Zn2'
_chemical_formula_weight         732.20

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   13.295(11)
_cell_length_b                   14.652(13)
_cell_length_c                   15.117(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.464(16)
_cell_angle_gamma                90.00
_cell_volume                     2864(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1348
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      19.44

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1476
_exptl_absorpt_coefficient_mu    1.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7212
_exptl_absorpt_correction_T_max  0.7553
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14025
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_sigmaI/netI    0.1230
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         25.10
_reflns_number_total             5051
_reflns_number_gt                2748
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

A water molecule was found disordered,a SQUEEZE procedure was applied 
on it.The result gave missing electron density accounting for 9.5 e per asymmetric 
unit,well consistent with the 10 demanded for a water molecule.

PLAT234_ALERT_4_B Large Hirshfeld Difference O4--N1 ..  0.30 Ang.
this is due to the nitro group disorder.

PLAT230_ALERT_2_B Hirshfeld Test Diff for C24 -- C27 .. 10.8 su
PLAT234_ALERT_4_B Large Hirshfeld Difference C19 -- C28_c .. 0.29 Ang.
PLAT234_ALERT_4_B Large Hirshfeld Difference C27 -- C28 .. 0.28 Ang.
PLAT234_ALERT_4_B Large Hirshfeld Difference C28 -- C19_c .. 0.29 Ang.
PLAT260_ALERT_2_B Short C(sp3)-C(sp3) Bond C27 - C28 .. 1.27 Ang.
These are due to the bpa ligand disorder.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1313P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5051
_refine_ls_number_parameters     415
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.2100
_refine_ls_wR_factor_gt          0.1756
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_restrained_S_all      0.890
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8791(6) 0.3880(5) 0.9208(5) 0.0355(19) Uani 1 1 d . . .
C2 C 0.8579(6) 0.4804(5) 0.8788(6) 0.0357(19) Uani 1 1 d . . .
C3 C 0.7946(7) 0.5403(5) 0.9092(6) 0.045(2) Uani 1 1 d . . .
H3 H 0.7641 0.5245 0.9565 0.055 Uiso 1 1 calc R . .
C4 C 0.7769(7) 0.6255(5) 0.8676(6) 0.044(2) Uani 1 1 d . . .
C5 C 0.8193(6) 0.6534(5) 0.7957(6) 0.0340(19) Uani 1 1 d . . .
C6 C 0.8808(6) 0.5887(5) 0.7635(5) 0.0330(18) Uani 1 1 d . . .
C7 C 0.9006(6) 0.5036(5) 0.8066(5) 0.0307(17) Uani 1 1 d . . .
H7 H 0.9433 0.4621 0.7865 0.037 Uiso 1 1 calc R . .
C8 C 0.9271(6) 0.6058(6) 0.6830(6) 0.039(2) Uani 1 1 d . . .
C9 C 0.8036(6) 0.7489(5) 0.7583(5) 0.0321(18) Uani 1 1 d . . .
C10 C 0.7204(6) 0.7745(6) 0.6879(6) 0.044(2) Uani 1 1 d . . .
C11 C 0.7118(7) 0.8641(6) 0.6564(6) 0.048(2) Uani 1 1 d . . .
H11 H 0.6558 0.8805 0.6096 0.058 Uiso 1 1 calc R . .
C12 C 0.7829(6) 0.9276(5) 0.6924(5) 0.0340(18) Uani 1 1 d . . .
C13 C 0.8633(6) 0.9028(5) 0.7639(5) 0.0352(19) Uani 1 1 d . . .
H13 H 0.9124 0.9465 0.7890 0.042 Uiso 1 1 calc R . .
C14 C 0.8733(6) 0.8168(5) 0.7992(5) 0.0294(17) Uani 1 1 d . . .
C15 C 1.0398(7) 0.2074(5) 1.1198(6) 0.0364(19) Uani 1 1 d . . .
C16 C 0.7745(8) 0.4766(5) 1.1525(6) 0.042(2) Uani 1 1 d . . .
C17 C 0.7502(7) 0.1454(6) 1.1469(7) 0.062(3) Uani 1 1 d . . .
H17 H 0.8184 0.1254 1.1621 0.074 Uiso 1 1 calc R . .
C18 C 0.6748(9) 0.0892(8) 1.1625(9) 0.090(4) Uani 1 1 d . . .
H18 H 0.6923 0.0323 1.1889 0.108 Uiso 1 1 calc R . .
C19 C 0.5726(9) 0.1162(9) 1.1395(12) 0.110(5) Uani 1 1 d . . .
C20 C 0.5508(9) 0.1951(9) 1.0987(13) 0.128(7) Uani 1 1 d . . .
H20 H 0.4820 0.2122 1.0774 0.154 Uiso 1 1 calc R . .
C21 C 0.6298(8) 0.2543(8) 1.0869(11) 0.103(5) Uani 1 1 d . . .
H21 H 0.6123 0.3121 1.0626 0.124 Uiso 1 1 calc R . .
C22 C 0.8468(8) 0.0580(6) 0.9489(7) 0.055(2) Uani 1 1 d . . .
H22 H 0.9101 0.0384 0.9840 0.065 Uiso 1 1 calc R . .
C23 C 0.7635(8) 0.0030(7) 0.9448(8) 0.068(3) Uani 1 1 d . . .
H23 H 0.7693 -0.0518 0.9765 0.081 Uiso 1 1 calc R . .
C24 C 0.6707(9) 0.0317(10) 0.8920(11) 0.100(5) Uani 1 1 d . . .
H24 H 0.6781 -0.0032 0.8386 0.120 Uiso 1 1 calc R . .
C25 C 0.6658(8) 0.1145(8) 0.8487(10) 0.092(4) Uani 1 1 d . . .
H25 H 0.6029 0.1366 0.8151 0.110 Uiso 1 1 calc R . .
C26 C 0.7546(8) 0.1643(7) 0.8552(7) 0.060(3) Uani 1 1 d . . .
H26 H 0.7520 0.2185 0.8228 0.072 Uiso 1 1 calc R . .
C27 C 0.5654(16) -0.0253(15) 0.9033(14) 0.169(8) Uani 1 1 d U . .
H27A H 0.5848 -0.0729 0.9487 0.203 Uiso 1 1 calc R . .
H27B H 0.5180 0.0160 0.9232 0.203 Uiso 1 1 calc R . .
C28 C 0.5216(15) -0.0604(12) 0.8270(11) 0.152(8) Uani 1 1 d . . .
H28A H 0.5672 -0.1014 0.8045 0.182 Uiso 1 1 calc R . .
H28B H 0.4948 -0.0144 0.7815 0.182 Uiso 1 1 calc R . .
N2 N 0.6463(8) 0.7104(7) 0.6462(8) 0.086(3) Uani 1 1 d . . .
N3 N 0.7292(6) 0.2299(4) 1.1097(5) 0.0428(17) Uani 1 1 d . . .
N4 N 0.8447(5) 0.1363(5) 0.9073(5) 0.0399(16) Uani 1 1 d . . .
O1 O 0.9405(5) 0.3373(4) 0.8941(4) 0.0516(17) Uani 1 1 d . . .
O2 O 0.8263(5) 0.3643(4) 0.9765(4) 0.0633(19) Uani 1 1 d . . .
O5 O 0.9426(5) 0.6882(4) 0.6651(4) 0.0517(16) Uani 1 1 d . . .
O6 O 0.9425(5) 0.5388(4) 0.6361(4) 0.0505(16) Uani 1 1 d . . .
O7 O 0.6656(8) 0.6338(7) 0.6381(9) 0.150(5) Uani 1 1 d . . .
O8 O 0.5579(9) 0.7370(8) 0.6194(12) 0.179(7) Uani 1 1 d . . .
O9 O 0.8534(5) 0.4252(4) 1.1768(4) 0.0505(16) Uani 1 1 d . . .
O10 O 0.6952(5) 0.4568(4) 1.0944(4) 0.0538(17) Uani 1 1 d . . .
O11 O 0.9594(5) 0.2409(5) 1.1331(4) 0.068(2) Uani 1 1 d . . .
O12 O 1.0567(5) 0.1895(5) 1.0447(4) 0.0635(19) Uani 1 1 d . . .
Zn1 Zn 0.83833(7) 0.31841(6) 1.09960(6) 0.0337(3) Uani 1 1 d . . .
Zn2 Zn 0.97549(7) 0.20955(6) 0.92192(6) 0.0345(3) Uani 1 1 d . . .
N1 N 0.6991(15) 0.6806(11) 0.9020(13) 0.161(7) Uani 1 1 d U . .
O3 O 0.7225(18) 0.7039(14) 0.9768(16) 0.250(10) Uani 1 1 d U . .
O4 O 0.6487(15) 0.7316(12) 0.8504(13) 0.221(7) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.239(9) . ?
C1 O2 1.263(9) . ?
C1 C2 1.494(10) . ?
C2 C3 1.367(10) . ?
C2 C7 1.385(10) . ?
C3 C4 1.393(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.397(11) . ?
C4 N1 1.498(16) . ?
C5 C6 1.411(10) . ?
C5 C9 1.505(10) . ?
C6 C7 1.403(10) . ?
C6 C8 1.507(10) . ?
C7 H7 0.9300 . ?
C8 O6 1.255(9) . ?
C8 O5 1.264(9) . ?
C9 C10 1.396(11) . ?
C9 C14 1.401(11) . ?
C10 N2 1.401(12) . ?
C10 C11 1.392(11) . ?
C11 C12 1.348(11) . ?
C11 H11 0.9300 . ?
C12 C13 1.380(11) . ?
C12 C16 1.521(10) 4_575 ?
C13 C14 1.363(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.517(11) 3_767 ?
C15 O12 1.236(10) . ?
C15 O11 1.234(10) . ?
C15 C14 1.517(11) 3_767 ?
C16 O10 1.239(10) . ?
C16 O9 1.274(11) . ?
C16 C12 1.521(10) 4_576 ?
C17 C18 1.359(13) . ?
C17 N3 1.362(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.380(16) . ?
C18 H18 0.9300 . ?
C19 C20 1.310(17) . ?
C19 C28 1.671(19) 3_657 ?
C20 C21 1.405(15) . ?
C20 H20 0.9300 . ?
C21 N3 1.335(12) . ?
C21 H21 0.9300 . ?
C22 N4 1.305(11) . ?
C22 C23 1.358(13) . ?
C22 H22 0.9300 . ?
C23 C24 1.371(15) . ?
C23 H23 0.9300 . ?
C24 C25 1.372(16) . ?
C24 C27 1.67(2) . ?
C24 H24 0.9800 . ?
C25 C26 1.371(13) . ?
C25 H25 0.9300 . ?
C26 N4 1.335(11) . ?
C26 H26 0.9300 . ?
C27 C28 1.27(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C19 1.671(19) 3_657 ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
N2 O7 1.164(12) . ?
N2 O8 1.214(13) . ?
N3 Zn1 1.979(7) . ?
N4 Zn2 2.011(7) . ?
O1 Zn2 1.951(6) . ?
O2 Zn1 1.950(6) . ?
O5 Zn2 1.919(6) 2_756 ?
O9 Zn1 1.934(6) . ?
O11 Zn1 1.938(7) . ?
O12 Zn2 1.940(7) . ?
Zn2 O5 1.919(6) 2_746 ?
N1 O3 1.15(2) . ?
N1 O4 1.171(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 124.3(7) . . ?
O1 C1 C2 118.5(7) . . ?
O2 C1 C2 117.0(7) . . ?
C3 C2 C7 120.3(7) . . ?
C3 C2 C1 120.6(7) . . ?
C7 C2 C1 119.1(7) . . ?
C2 C3 C4 118.5(7) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C3 C4 C5 123.9(7) . . ?
C3 C4 N1 112.6(9) . . ?
C5 C4 N1 123.3(10) . . ?
C4 C5 C6 116.3(7) . . ?
C4 C5 C9 121.2(7) . . ?
C6 C5 C9 122.4(7) . . ?
C7 C6 C5 119.9(7) . . ?
C7 C6 C8 117.1(7) . . ?
C5 C6 C8 123.0(7) . . ?
C2 C7 C6 121.2(7) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
O6 C8 O5 124.8(8) . . ?
O6 C8 C6 118.4(7) . . ?
O5 C8 C6 116.7(7) . . ?
C10 C9 C14 118.1(7) . . ?
C10 C9 C5 123.5(7) . . ?
C14 C9 C5 118.4(7) . . ?
N2 C10 C11 119.0(8) . . ?
N2 C10 C9 120.8(8) . . ?
C11 C10 C9 120.2(8) . . ?
C12 C11 C10 121.2(8) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 118.5(7) . . ?
C11 C12 C16 119.8(8) . 4_575 ?
C13 C12 C16 121.7(7) . 4_575 ?
C14 C13 C12 122.5(7) . . ?
C14 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
C13 C14 C9 119.3(7) . . ?
C13 C14 C15 121.2(7) . 3_767 ?
C9 C14 C15 119.4(6) . 3_767 ?
O12 C15 O11 125.7(8) . . ?
O12 C15 C14 115.1(8) . 3_767 ?
O11 C15 C14 119.2(7) . 3_767 ?
O10 C16 O9 125.0(7) . . ?
O10 C16 C12 118.0(8) . 4_576 ?
O9 C16 C12 116.8(8) . 4_576 ?
C18 C17 N3 122.3(9) . . ?
C18 C17 H17 118.9 . . ?
N3 C17 H17 118.9 . . ?
C17 C18 C19 120.3(10) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C20 C19 C18 118.0(10) . . ?
C20 C19 C28 118.4(12) . 3_657 ?
C18 C19 C28 123.2(12) . 3_657 ?
C19 C20 C21 121.0(11) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
N3 C21 C20 121.7(11) . . ?
N3 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
N4 C22 C23 125.0(10) . . ?
N4 C22 H22 117.5 . . ?
C23 C22 H22 117.5 . . ?
C22 C23 C24 117.2(10) . . ?
C22 C23 H23 121.4 . . ?
C24 C23 H23 121.4 . . ?
C25 C24 C23 119.0(10) . . ?
C25 C24 C27 122.8(13) . . ?
C23 C24 C27 116.7(13) . . ?
C25 C24 H24 94.0 . . ?
C23 C24 H24 94.0 . . ?
C27 C24 H24 94.0 . . ?
C24 C25 C26 119.4(11) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
N4 C26 C25 121.2(9) . . ?
N4 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C28 C27 C24 109.0(17) . . ?
C28 C27 H27A 109.9 . . ?
C24 C27 H27A 109.9 . . ?
C28 C27 H27B 109.9 . . ?
C24 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C27 C28 C19 98.0(16) . 3_657 ?
C27 C28 H28A 112.2 . . ?
C19 C28 H28A 112.2 3_657 . ?
C27 C28 H28B 112.2 . . ?
C19 C28 H28B 112.2 3_657 . ?
H28A C28 H28B 109.8 . . ?
O7 N2 O8 119.7(11) . . ?
O7 N2 C10 123.0(11) . . ?
O8 N2 C10 117.4(11) . . ?
C21 N3 C17 116.5(8) . . ?
C21 N3 Zn1 120.3(6) . . ?
C17 N3 Zn1 123.0(6) . . ?
C22 N4 C26 118.0(8) . . ?
C22 N4 Zn2 119.7(6) . . ?
C26 N4 Zn2 122.3(6) . . ?
C1 O1 Zn2 130.3(5) . . ?
C1 O2 Zn1 142.8(6) . . ?
C8 O5 Zn2 116.7(5) . 2_756 ?
C16 O9 Zn1 110.0(5) . . ?
C15 O11 Zn1 152.7(6) . . ?
C15 O12 Zn2 131.8(6) . . ?
O9 Zn1 O11 110.7(3) . . ?
O9 Zn1 O2 105.7(3) . . ?
O11 Zn1 O2 109.2(3) . . ?
O9 Zn1 N3 117.3(3) . . ?
O11 Zn1 N3 100.1(3) . . ?
O2 Zn1 N3 113.6(3) . . ?
O5 Zn2 O12 110.7(3) 2_746 . ?
O5 Zn2 O1 98.8(2) 2_746 . ?
O12 Zn2 O1 113.8(3) . . ?
O5 Zn2 N4 116.9(3) 2_746 . ?
O12 Zn2 N4 107.4(3) . . ?
O1 Zn2 N4 109.4(3) . . ?
O3 N1 O4 116.6(19) . . ?
O3 N1 C4 116.7(18) . . ?
O4 N1 C4 116.6(17) . . ?

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
O1 C1 C2 C3 -176.8(8) . . . . ?
O2 C1 C2 C3 8.7(12) . . . . ?
O1 C1 C2 C7 5.2(12) . . . . ?
O2 C1 C2 C7 -169.3(8) . . . . ?
C7 C2 C3 C4 -1.8(13) . . . . ?
C1 C2 C3 C4 -179.8(8) . . . . ?
C2 C3 C4 C5 0.7(14) . . . . ?
C2 C3 C4 N1 174.9(11) . . . . ?
C3 C4 C5 C6 1.8(13) . . . . ?
N1 C4 C5 C6 -171.8(12) . . . . ?
C3 C4 C5 C9 -175.4(8) . . . . ?
N1 C4 C5 C9 11.1(16) . . . . ?
C4 C5 C6 C7 -3.3(12) . . . . ?
C9 C5 C6 C7 173.9(7) . . . . ?
C4 C5 C6 C8 176.5(7) . . . . ?
C9 C5 C6 C8 -6.4(12) . . . . ?
C3 C2 C7 C6 0.3(12) . . . . ?
C1 C2 C7 C6 178.3(7) . . . . ?
C5 C6 C7 C2 2.3(12) . . . . ?
C8 C6 C7 C2 -177.4(7) . . . . ?
C7 C6 C8 O6 28.7(11) . . . . ?
C5 C6 C8 O6 -151.0(8) . . . . ?
C7 C6 C8 O5 -154.9(8) . . . . ?
C5 C6 C8 O5 25.3(12) . . . . ?
C4 C5 C9 C10 -89.6(11) . . . . ?
C6 C5 C9 C10 93.4(10) . . . . ?
C4 C5 C9 C14 87.2(9) . . . . ?
C6 C5 C9 C14 -89.8(10) . . . . ?
C14 C9 C10 N2 -178.0(9) . . . . ?
C5 C9 C10 N2 -1.3(14) . . . . ?
C14 C9 C10 C11 3.9(12) . . . . ?
C5 C9 C10 C11 -179.4(8) . . . . ?
N2 C10 C11 C12 -177.9(10) . . . . ?
C9 C10 C11 C12 0.3(14) . . . . ?
C10 C11 C12 C13 -2.3(13) . . . . ?
C10 C11 C12 C16 176.3(8) . . . 4_575 ?
C11 C12 C13 C14 0.2(12) . . . . ?
C16 C12 C13 C14 -178.5(7) 4_575 . . . ?
C12 C13 C14 C9 4.0(11) . . . . ?
C12 C13 C14 C15 -177.6(7) . . . 3_767 ?
C10 C9 C14 C13 -5.9(11) . . . . ?
C5 C9 C14 C13 177.1(7) . . . . ?
C10 C9 C14 C15 175.7(7) . . . 3_767 ?
C5 C9 C14 C15 -1.2(10) . . . 3_767 ?
N3 C17 C18 C19 1(2) . . . . ?
C17 C18 C19 C20 3(3) . . . . ?
C17 C18 C19 C28 -168.6(14) . . . 3_657 ?
C18 C19 C20 C21 -6(3) . . . . ?
C28 C19 C20 C21 165.9(16) 3_657 . . . ?
C19 C20 C21 N3 6(3) . . . . ?
N4 C22 C23 C24 0.8(18) . . . . ?
C22 C23 C24 C25 -2(2) . . . . ?
C22 C23 C24 C27 -168.4(13) . . . . ?
C23 C24 C25 C26 3(2) . . . . ?
C27 C24 C25 C26 169.1(15) . . . . ?
C24 C25 C26 N4 -4(2) . . . . ?
C25 C24 C27 C28 74(2) . . . . ?
C23 C24 C27 C28 -120(2) . . . . ?
C24 C27 C28 C19 176.6(13) . . . 3_657 ?
C11 C10 N2 O7 146.6(13) . . . . ?
C9 C10 N2 O7 -31.6(19) . . . . ?
C11 C10 N2 O8 -35.0(18) . . . . ?
C9 C10 N2 O8 146.8(13) . . . . ?
C20 C21 N3 C17 -1(2) . . . . ?
C20 C21 N3 Zn1 -175.8(13) . . . . ?
C18 C17 N3 C21 -1.6(17) . . . . ?
C18 C17 N3 Zn1 172.6(10) . . . . ?
C23 C22 N4 C26 -1.3(15) . . . . ?
C23 C22 N4 Zn2 179.4(8) . . . . ?
C25 C26 N4 C22 2.9(15) . . . . ?
C25 C26 N4 Zn2 -177.9(9) . . . . ?
O2 C1 O1 Zn2 1.9(13) . . . . ?
C2 C1 O1 Zn2 -172.3(6) . . . . ?
O1 C1 O2 Zn1 59.1(14) . . . . ?
C2 C1 O2 Zn1 -126.7(9) . . . . ?
O6 C8 O5 Zn2 -15.2(11) . . . 2_756 ?
C6 C8 O5 Zn2 168.7(5) . . . 2_756 ?
O10 C16 O9 Zn1 7.1(11) . . . . ?
C12 C16 O9 Zn1 -167.6(5) 4_576 . . . ?
O12 C15 O11 Zn1 -32(2) . . . . ?
C14 C15 O11 Zn1 149.4(12) 3_767 . . . ?
O11 C15 O12 Zn2 3.5(14) . . . . ?
C14 C15 O12 Zn2 -177.7(6) 3_767 . . . ?
C16 O9 Zn1 O11 178.3(5) . . . . ?
C16 O9 Zn1 O2 60.1(6) . . . . ?
C16 O9 Zn1 N3 -67.8(6) . . . . ?
C15 O11 Zn1 O9 -108.3(15) . . . . ?
C15 O11 Zn1 O2 7.7(16) . . . . ?
C15 O11 Zn1 N3 127.3(15) . . . . ?
C1 O2 Zn1 O9 86.9(10) . . . . ?
C1 O2 Zn1 O11 -32.3(11) . . . . ?
C1 O2 Zn1 N3 -143.1(10) . . . . ?
C21 N3 Zn1 O9 64.1(10) . . . . ?
C17 N3 Zn1 O9 -109.9(8) . . . . ?
C21 N3 Zn1 O11 -176.2(10) . . . . ?
C17 N3 Zn1 O11 9.8(8) . . . . ?
C21 N3 Zn1 O2 -59.9(10) . . . . ?
C17 N3 Zn1 O2 126.1(8) . . . . ?
C15 O12 Zn2 O5 168.4(8) . . . 2_746 ?
C15 O12 Zn2 O1 58.1(9) . . . . ?
C15 O12 Zn2 N4 -63.0(8) . . . . ?
C1 O1 Zn2 O5 171.0(8) . . . 2_746 ?
C1 O1 Zn2 O12 -71.7(8) . . . . ?
C1 O1 Zn2 N4 48.4(8) . . . . ?
C22 N4 Zn2 O5 90.9(7) . . . 2_746 ?
C26 N4 Zn2 O5 -88.4(8) . . . 2_746 ?
C22 N4 Zn2 O12 -34.1(7) . . . . ?
C26 N4 Zn2 O12 146.7(7) . . . . ?
C22 N4 Zn2 O1 -158.0(7) . . . . ?
C26 N4 Zn2 O1 22.8(8) . . . . ?
C3 C4 N1 O3 66(3) . . . . ?
C5 C4 N1 O3 -119(2) . . . . ?
C3 C4 N1 O4 -149(2) . . . . ?
C5 C4 N1 O4 25(3) . . . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.000 111 19 ' '
2 0.500 1.000 0.500 111 19 ' '
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.118
####################################################################### 
# 
# 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 1444250'
_audit_update_record             
;
2016-03-02 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H12 N4 O12 Zn2'
_chemical_formula_weight         703.14

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P21/c '

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

_cell_length_a                   7.9827(3)
_cell_length_b                   14.5526(5)
_cell_length_c                   22.3790(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.608(5)
_cell_angle_gamma                90.00
_cell_volume                     2537.06(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5705
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      27.95

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    1.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6940
_exptl_absorpt_correction_T_max  0.7700
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11941
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4442
_reflns_number_gt                4032
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+145.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4442
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.1465
_refine_ls_wR_factor_ref         0.3159
_refine_ls_wR_factor_gt          0.2996
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.6883(2) 0.40334(12) 0.37128(8) 0.0275(5) Uani 1 1 d . . .
Zn2 Zn 0.8174(2) 0.23815(13) 0.27342(8) 0.0305(5) Uani 1 1 d . . .
O1 O 0.7109(15) 0.4626(8) 0.2952(5) 0.041(3) Uani 1 1 d . . .
O2 O 0.8001(15) 0.3651(8) 0.2330(5) 0.042(3) Uani 1 1 d . . .
O3 O 0.900(4) 0.601(2) 0.0175(14) 0.048(9) Uani 0.42(3) 1 d P A 1
O4 O 0.799(4) 0.474(2) 0.0226(14) 0.050(9) Uani 0.42(3) 1 d P A 1
O3' O 0.946(3) 0.5029(16) 0.0494(10) 0.051(7) Uani 0.58(3) 1 d P A 2
O4' O 0.743(3) 0.5821(16) -0.0034(10) 0.052(7) Uani 0.58(3) 1 d P A 2
O5 O 0.4999(15) 0.8152(8) 0.1348(5) 0.040(3) Uani 1 1 d . . .
O6 O 0.4291(14) 0.7431(8) 0.2131(5) 0.040(3) Uani 1 1 d . . .
O7 O 0.337(3) 0.6463(19) 0.0454(11) 0.050(7) Uani 0.61(3) 1 d P B 3
O8 O 0.325(3) 0.6471(15) -0.0505(10) 0.050(7) Uani 0.61(3) 1 d P B 3
O7' O 0.255(4) 0.704(2) 0.0003(15) 0.049(11) Uani 0.39(3) 1 d P B 4
O8' O 0.404(5) 0.597(3) 0.0316(16) 0.047(10) Uani 0.39(3) 1 d P B 4
O9 O 0.5116(17) 0.9528(9) -0.1173(6) 0.053(3) Uani 1 1 d . B .
O10 O 0.7406(15) 0.4869(8) 0.4409(5) 0.042(3) Uani 1 1 d . . .
O11 O 1.1044(15) 0.8222(8) 0.0968(5) 0.043(3) Uani 1 1 d . . .
O12 O 0.9729(15) 0.7586(8) 0.1617(5) 0.042(3) Uani 1 1 d . . .
N1 N 0.819(2) 0.5528(11) 0.0473(7) 0.046(4) Uani 1 1 d . . .
N2 N 0.401(2) 0.6696(11) 0.0015(7) 0.045(4) Uani 1 1 d . . .
N3 N 0.8041(18) 0.0929(10) 0.2911(7) 0.041(3) Uani 1 1 d . . .
N4 N 0.8778(18) 0.1784(10) 0.1958(6) 0.039(3) Uani 1 1 d . . .
C1 C 0.750(2) 0.4410(13) 0.2478(8) 0.042(4) Uani 1 1 d . . .
C2 C 0.729(2) 0.5165(13) 0.1982(8) 0.042(4) Uani 1 1 d . A .
C3 C 0.782(2) 0.5049(13) 0.1466(8) 0.043(4) Uani 1 1 d . . .
H3 H 0.8327 0.4492 0.1406 0.051 Uiso 1 1 calc R A .
C4 C 0.766(2) 0.5724(13) 0.1000(8) 0.043(4) Uani 1 1 d . A .
C5 C 0.683(2) 0.6566(13) 0.1104(8) 0.043(4) Uani 1 1 d . . .
C6 C 0.620(2) 0.6663(13) 0.1614(8) 0.042(4) Uani 1 1 d . A .
C7 C 0.649(2) 0.5981(12) 0.2040(8) 0.042(4) Uani 1 1 d . . .
H7 H 0.6103 0.6076 0.2399 0.051 Uiso 1 1 calc R A .
C8 C 0.510(2) 0.7476(13) 0.1696(8) 0.043(4) Uani 1 1 d . . .
C9 C 0.676(2) 0.7303(13) 0.0613(8) 0.042(4) Uani 1 1 d . A .
C10 C 0.535(2) 0.7384(13) 0.0119(8) 0.043(4) Uani 1 1 d . A .
C11 C 0.516(2) 0.8080(13) -0.0288(8) 0.044(4) Uani 1 1 d . . .
H11 H 0.4153 0.8132 -0.0588 0.052 Uiso 1 1 calc R B .
C12 C 0.647(2) 0.8722(13) -0.0259(8) 0.043(4) Uani 1 1 d . B .
C13 C 0.791(2) 0.8619(13) 0.0186(8) 0.043(4) Uani 1 1 d . . .
H13 H 0.8830 0.9017 0.0195 0.051 Uiso 1 1 calc R B .
C14 C 0.806(2) 0.7932(12) 0.0633(8) 0.042(4) Uani 1 1 d . A .
C15 C 0.971(2) 0.7913(13) 0.1127(8) 0.042(4) Uani 1 1 d . . .
C16 C 0.633(2) 0.9518(13) -0.0720(8) 0.044(4) Uani 1 1 d . . .
C17 C 0.768(2) 0.0524(13) 0.3372(8) 0.044(4) Uani 1 1 d . . .
H17 H 0.7659 0.0892 0.3710 0.053 Uiso 1 1 calc R . .
C18 C 0.732(2) -0.0394(13) 0.3431(8) 0.044(4) Uani 1 1 d . . .
H18 H 0.7063 -0.0649 0.3781 0.053 Uiso 1 1 calc R . .
C19 C 0.738(2) -0.0891(13) 0.2913(8) 0.045(4) Uani 1 1 d . . .
H19 H 0.7134 -0.1516 0.2916 0.054 Uiso 1 1 calc R . .
C20 C 0.776(2) -0.0539(13) 0.2401(8) 0.045(4) Uani 1 1 d . . .
H20 H 0.7768 -0.0907 0.2062 0.053 Uiso 1 1 calc R . .
C21 C 0.815(2) 0.0413(13) 0.2399(8) 0.044(4) Uani 1 1 d . . .
C22 C 0.856(2) 0.0876(13) 0.1913(8) 0.043(4) Uani 1 1 d . . .
C23 C 0.883(2) 0.0456(13) 0.1363(8) 0.044(4) Uani 1 1 d . . .
H23 H 0.8700 -0.0176 0.1313 0.053 Uiso 1 1 calc R . .
C24 C 0.925(2) 0.0939(13) 0.0940(8) 0.045(4) Uani 1 1 d . . .
H24 H 0.9348 0.0653 0.0578 0.054 Uiso 1 1 calc R . .
C25 C 0.957(2) 0.1864(13) 0.1005(8) 0.045(4) Uani 1 1 d . . .
H25 H 0.9966 0.2200 0.0711 0.053 Uiso 1 1 calc R . .
C26 C 0.927(2) 0.2263(13) 0.1516(8) 0.044(4) Uani 1 1 d . . .
H26 H 0.9423 0.2895 0.1564 0.053 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O10 1.949(12) . ?
Zn1 O1 1.953(11) . ?
Zn1 O5 1.957(12) 2_645 ?
Zn1 O11 2.031(12) 2_745 ?
Zn1 C16 2.548(19) 4_576 ?
Zn2 O12 1.984(11) 2_745 ?
Zn2 O2 2.049(12) . ?
Zn2 O6 2.056(12) 2_645 ?
Zn2 N4 2.091(14) . ?
Zn2 N3 2.158(15) . ?
O1 C1 1.21(2) . ?
O2 C1 1.24(2) . ?
O3 N1 1.24(3) . ?
O4 N1 1.27(3) . ?
O3' N1 1.24(3) . ?
O4' N1 1.24(3) . ?
O5 C8 1.25(2) . ?
O5 Zn1 1.957(12) 2_655 ?
O6 C8 1.28(2) . ?
O6 Zn2 2.056(12) 2_655 ?
O7 N2 1.25(3) . ?
O8 N2 1.23(2) . ?
O7' N2 1.26(4) . ?
O8' N2 1.25(4) . ?
O9 C16 1.24(2) . ?
O10 C16 1.23(2) 4_576 ?
O11 C15 1.28(2) . ?
O11 Zn1 2.031(12) 2_755 ?
O12 C15 1.19(2) . ?
O12 Zn2 1.984(11) 2_755 ?
N1 C4 1.37(2) . ?
N2 C10 1.45(2) . ?
N3 C17 1.28(2) . ?
N3 C21 1.39(2) . ?
N4 C22 1.33(2) . ?
N4 C26 1.34(2) . ?
C1 C2 1.54(2) . ?
C2 C3 1.32(2) . ?
C2 C7 1.37(3) . ?
C3 C4 1.42(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.44(3) . ?
C5 C6 1.35(3) . ?
C5 C9 1.53(2) . ?
C6 C7 1.36(2) . ?
C6 C8 1.51(3) . ?
C7 H7 0.9300 . ?
C9 C14 1.38(2) . ?
C9 C10 1.40(2) . ?
C10 C11 1.35(2) . ?
C11 C12 1.40(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.35(2) . ?
C12 C16 1.54(2) . ?
C13 C14 1.40(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.52(2) . ?
C16 O10 1.23(2) 4_575 ?
C16 Zn1 2.548(19) 4_575 ?
C17 C18 1.38(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.37(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.35(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.42(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.38(3) . ?
C22 C23 1.43(3) . ?
C23 C24 1.28(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.37(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.35(3) . ?
C25 H25 0.9300 . ?
C26 H26 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
O10 Zn1 O1 112.2(5) . . ?
O10 Zn1 O5 119.4(5) . 2_645 ?
O1 Zn1 O5 116.4(5) . 2_645 ?
O10 Zn1 O11 93.8(5) . 2_745 ?
O1 Zn1 O11 109.9(5) . 2_745 ?
O5 Zn1 O11 101.4(5) 2_645 2_745 ?
O10 Zn1 C16 27.9(5) . 4_576 ?
O1 Zn1 C16 97.4(6) . 4_576 ?
O5 Zn1 C16 111.2(5) 2_645 4_576 ?
O11 Zn1 C16 121.5(5) 2_745 4_576 ?
O12 Zn2 O2 98.8(5) 2_745 . ?
O12 Zn2 O6 124.7(5) 2_745 2_645 ?
O2 Zn2 O6 93.4(5) . 2_645 ?
O12 Zn2 N4 111.1(5) 2_745 . ?
O2 Zn2 N4 90.8(5) . . ?
O6 Zn2 N4 122.6(5) 2_645 . ?
O12 Zn2 N3 94.6(5) 2_745 . ?
O2 Zn2 N3 164.4(5) . . ?
O6 Zn2 N3 85.5(5) 2_645 . ?
N4 Zn2 N3 77.0(6) . . ?
C1 O1 Zn1 137.7(12) . . ?
C1 O2 Zn2 132.7(12) . . ?
C8 O5 Zn1 120.3(12) . 2_655 ?
C8 O6 Zn2 140.3(11) . 2_655 ?
C16 O10 Zn1 104.3(11) 4_576 . ?
C15 O11 Zn1 140.6(12) . 2_755 ?
C15 O12 Zn2 124.9(12) . 2_755 ?
O4' N1 O3' 118(2) . . ?
O4' N1 O3 61.4(18) . . ?
O3' N1 O3 80(2) . . ?
O4' N1 O4 86(2) . . ?
O3' N1 O4 60.5(18) . . ?
O3 N1 O4 108(2) . . ?
O4' N1 C4 122.5(18) . . ?
O3' N1 C4 119.6(18) . . ?
O3 N1 C4 130(2) . . ?
O4 N1 C4 122(2) . . ?
O8 N2 O7 117.8(19) . . ?
O8 N2 O8' 103(2) . . ?
O7 N2 O8' 46.4(18) . . ?
O8 N2 O7' 80(2) . . ?
O7 N2 O7' 66(2) . . ?
O8' N2 O7' 105(3) . . ?
O8 N2 C10 122.2(18) . . ?
O7 N2 C10 118.4(18) . . ?
O8' N2 C10 125(2) . . ?
O7' N2 C10 112(2) . . ?
C17 N3 C21 119.0(16) . . ?
C17 N3 Zn2 129.0(13) . . ?
C21 N3 Zn2 111.3(11) . . ?
C22 N4 C26 121.0(16) . . ?
C22 N4 Zn2 115.1(12) . . ?
C26 N4 Zn2 123.8(12) . . ?
O1 C1 O2 128.6(17) . . ?
O1 C1 C2 115.8(16) . . ?
O2 C1 C2 115.6(16) . . ?
C3 C2 C7 116.0(17) . . ?
C3 C2 C1 122.1(17) . . ?
C7 C2 C1 121.9(16) . . ?
C2 C3 C4 124.0(18) . . ?
C2 C3 H3 118.0 . . ?
C4 C3 H3 118.0 . . ?
N1 C4 C3 119.7(17) . . ?
N1 C4 C5 123.9(16) . . ?
C3 C4 C5 116.3(16) . . ?
C6 C5 C4 119.7(17) . . ?
C6 C5 C9 125.1(17) . . ?
C4 C5 C9 115.2(16) . . ?
C5 C6 C7 118.6(17) . . ?
C5 C6 C8 121.2(16) . . ?
C7 C6 C8 120.1(16) . . ?
C6 C7 C2 125.3(18) . . ?
C6 C7 H7 117.4 . . ?
C2 C7 H7 117.4 . . ?
O5 C8 O6 122.6(17) . . ?
O5 C8 C6 120.3(16) . . ?
O6 C8 C6 117.1(16) . . ?
C14 C9 C10 116.3(17) . . ?
C14 C9 C5 122.4(16) . . ?
C10 C9 C5 121.3(16) . . ?
C11 C10 C9 123.2(17) . . ?
C11 C10 N2 116.1(15) . . ?
C9 C10 N2 120.7(16) . . ?
C10 C11 C12 119.9(17) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 117.9(17) . . ?
C13 C12 C16 120.3(17) . . ?
C11 C12 C16 121.8(16) . . ?
C12 C13 C14 122.1(18) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C9 C14 C13 120.2(17) . . ?
C9 C14 C15 122.5(16) . . ?
C13 C14 C15 117.2(16) . . ?
O12 C15 O11 123.5(17) . . ?
O12 C15 C14 120.7(16) . . ?
O11 C15 C14 115.7(15) . . ?
O10 C16 O9 124.5(17) 4_575 . ?
O10 C16 C12 116.2(15) 4_575 . ?
O9 C16 C12 119.2(16) . . ?
O10 C16 Zn1 47.8(8) 4_575 4_575 ?
O9 C16 Zn1 76.9(11) . 4_575 ?
C12 C16 Zn1 163.9(13) . 4_575 ?
N3 C17 C18 127.8(19) . . ?
N3 C17 H17 116.1 . . ?
C18 C17 H17 116.1 . . ?
C19 C18 C17 112.6(18) . . ?
C19 C18 H18 123.7 . . ?
C17 C18 H18 123.7 . . ?
C20 C19 C18 124.9(19) . . ?
C20 C19 H19 117.6 . . ?
C18 C19 H19 117.6 . . ?
C19 C20 C21 117.6(18) . . ?
C19 C20 H20 121.2 . . ?
C21 C20 H20 121.2 . . ?
C22 C21 N3 117.1(17) . . ?
C22 C21 C20 124.8(18) . . ?
N3 C21 C20 118.1(17) . . ?
N4 C22 C21 118.3(17) . . ?
N4 C22 C23 116.5(16) . . ?
C21 C22 C23 125.1(18) . . ?
C24 C23 C22 120.9(18) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 122.2(19) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C26 C25 C24 116.8(18) . . ?
C26 C25 H25 121.6 . . ?
C24 C25 H25 121.6 . . ?
N4 C26 C25 122.5(18) . . ?
N4 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         2.250
_refine_diff_density_min         -2.250
_refine_diff_density_rms         0.302
####################################################################### 
# 
# 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 1444251'
_audit_update_record             
;
2016-03-02 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H22 N6 O12 Zn'
_chemical_formula_weight         844.01

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   11.5833(5)
_cell_length_b                   11.7884(5)
_cell_length_c                   13.8783(6)
_cell_angle_alpha                96.027(8)
_cell_angle_beta                 92.924(6)
_cell_angle_gamma                107.066(9)
_cell_volume                     1794.92(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1777
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      23.21

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8625
_exptl_absorpt_correction_T_max  0.8813
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9027
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         25.10
_reflns_number_total             6257
_reflns_number_gt                4022
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0009P)²+40.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6257
_refine_ls_number_parameters     808
_refine_ls_number_restraints     9695
_refine_ls_R_factor_all          0.1775
_refine_ls_R_factor_gt           0.1124
_refine_ls_wR_factor_ref         0.3151
_refine_ls_wR_factor_gt          0.2373
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      0.660
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.72825(8) 0.73549(7) 0.74317(6) 0.0418(2) Uani 1 1 d U . .
C1 C 0.6819(6) 0.9340(6) 0.6809(5) 0.0403(8) Uani 1 1 d U . .
C2 C 0.6682(6) 1.0582(6) 0.7098(5) 0.0401(8) Uani 1 1 d U A .
C3 C 0.7698(6) 1.1558(6) 0.6967(5) 0.0407(8) Uani 1 1 d U . .
H3 H 0.8347 1.1408 0.6666 0.049 Uiso 1 1 calc R A .
C4 C 0.7749(6) 1.2726(6) 0.7276(5) 0.0401(8) Uani 1 1 d U A .
C5 C 0.6804(6) 1.2934(6) 0.7708(5) 0.0413(8) Uani 1 1 d U . .
H5 H 0.6843 1.3713 0.7946 0.050 Uiso 1 1 calc R A .
C6 C 0.5775(6) 1.2006(6) 0.7806(5) 0.0415(8) Uani 1 1 d DU A .
C7 C 0.5692(6) 1.0797(6) 0.7489(5) 0.0408(8) Uani 1 1 d U . .
C8 C 0.4586(6) 0.9763(6) 0.7601(5) 0.0396(8) Uani 1 1 d U A .
C9 C 0.3586(6) 0.9377(6) 0.6887(5) 0.0403(8) Uani 1 1 d DU . .
C10 C 0.2637(6) 0.8387(6) 0.7003(5) 0.0411(8) Uani 1 1 d U A .
H10 H 0.2001 0.8128 0.6517 0.049 Uiso 1 1 calc R . .
C11 C 0.2566(6) 0.7755(6) 0.7791(5) 0.0417(8) Uani 1 1 d DU . .
C12 C 0.3541(6) 0.8138(6) 0.8473(5) 0.0415(8) Uani 1 1 d U A .
H12 H 0.3545 0.7730 0.9011 0.050 Uiso 1 1 calc R . .
C13 C 0.4505(6) 0.9105(6) 0.8382(5) 0.0412(8) Uani 1 1 d U . .
C14 C 0.5523(6) 0.9378(6) 0.9120(5) 0.0422(8) Uani 1 1 d U A .
C15 C 0.8896(6) 1.3732(6) 0.7210(5) 0.0411(8) Uani 1 1 d DU . .
C16 C 0.1520(6) 0.6672(6) 0.7889(5) 0.0428(8) Uani 1 1 d DU A .
C17 C 0.9865(12) 0.9712(13) 0.7585(13) 0.0435(9) Uani 0.469(12) 1 d PDU A 11
H17 H 0.9574 0.9946 0.7025 0.052 Uiso 0.469(12) 1 calc PR A 11
C18 C 1.0944(12) 1.0453(13) 0.7996(12) 0.0440(9) Uani 0.469(12) 1 d PDU A 11
H18 H 1.1352 1.1103 0.7691 0.053 Uiso 0.469(12) 1 calc PR A 11
C19 C 1.1328(15) 1.0298(14) 0.8664(12) 0.0432(9) Uani 0.469(12) 1 d PDU A 11
H19 H 1.2063 1.0822 0.8943 0.052 Uiso 0.469(12) 1 calc PR A 11
C20 C 1.0758(15) 0.9345(15) 0.9112(13) 0.0428(9) Uani 0.469(12) 1 d PDU A 11
C21 C 1.1210(14) 0.9137(15) 1.0038(12) 0.0436(9) Uani 0.469(12) 1 d PDU A 11
H21 H 1.1911 0.9676 1.0361 0.052 Uiso 0.469(12) 1 calc PR A 11
C22 C 1.0613(15) 0.8151(16) 1.0442(12) 0.0428(9) Uani 0.469(12) 1 d PDU A 11
H22 H 1.1042 0.7994 1.0971 0.051 Uiso 0.469(12) 1 calc PR A 11
C23 C 0.9331(14) 0.7242(11) 1.0167(13) 0.0435(9) Uani 0.469(12) 1 d PDU A 11
C24 C 0.8871(15) 0.7594(14) 0.9176(14) 0.0424(9) Uani 0.469(12) 1 d PDU A 11
C25 C 0.9630(15) 0.8579(14) 0.8704(13) 0.0425(9) Uani 0.469(12) 1 d PDU A 11
C26 C 0.8822(13) 0.6135(11) 1.0425(12) 0.0436(9) Uani 0.469(12) 1 d PDU A 11
H26 H 0.9228 0.5811 1.0866 0.052 Uiso 0.469(12) 1 calc PR A 11
C27 C 0.7718(14) 0.5536(14) 1.0018(12) 0.0431(9) Uani 0.469(12) 1 d PDU A 11
H27 H 0.7260 0.4851 1.0255 0.052 Uiso 0.469(12) 1 calc PR A 11
C28 C 0.7233(15) 0.5984(15) 0.9177(14) 0.0433(9) Uani 0.469(12) 1 d PDU A 11
H28 H 0.6426 0.5620 0.8950 0.052 Uiso 0.469(12) 1 calc PR A 11
C17' C 0.9678(11) 0.9385(11) 0.7371(12) 0.0430(9) Uani 0.531(12) 1 d PDU A 12
H17' H 0.9356 0.9440 0.6756 0.052 Uiso 0.531(12) 1 calc PR A 12
C18' C 1.0802(11) 1.0092(11) 0.7724(11) 0.0439(9) Uani 0.531(12) 1 d PDU A 12
H18' H 1.1248 1.0688 0.7384 0.053 Uiso 0.531(12) 1 calc PR A 12
C19' C 1.1329(13) 0.9862(13) 0.8741(11) 0.0433(9) Uani 0.531(12) 1 d PDU A 12
H19' H 1.2106 1.0311 0.8998 0.052 Uiso 0.531(12) 1 calc PR A 12
C20' C 1.0613(8) 0.8974(9) 0.9255(7) 0.0428(9) Uani 0.531(12) 1 d PGDU A 12
C21' C 1.1003(7) 0.8669(10) 1.0129(7) 0.0434(9) Uani 0.531(12) 1 d PGDU A 12
H21' H 1.1753 0.9110 1.0445 0.052 Uiso 0.531(12) 1 calc PR A 12
C22' C 1.0273(10) 0.7705(10) 1.0529(6) 0.0441(9) Uani 0.531(12) 1 d PGDU A 12
H22' H 1.0534 0.7501 1.1113 0.053 Uiso 0.531(12) 1 calc PR A 12
C23' C 0.9152(10) 0.7046(9) 1.0057(8) 0.0439(9) Uani 0.531(12) 1 d PGDU A 12
C24' C 0.8762(8) 0.7351(9) 0.9184(8) 0.0421(9) Uani 0.531(12) 1 d PGDU A 12
C25' C 0.9493(9) 0.8315(9) 0.8783(7) 0.0425(9) Uani 0.531(12) 1 d PGU A 12
C26' C 0.8410(11) 0.6270(10) 1.0501(10) 0.0430(9) Uani 0.531(12) 1 d PDU A 12
H26' H 0.8645 0.6155 1.1125 0.052 Uiso 0.531(12) 1 calc PR A 12
C27' C 0.7263(12) 0.5598(12) 1.0070(11) 0.0430(9) Uani 0.531(12) 1 d PDU A 12
H27' H 0.6785 0.4975 1.0367 0.052 Uiso 0.531(12) 1 calc PR A 12
C28' C 0.6853(13) 0.5864(12) 0.9209(12) 0.0430(9) Uani 0.531(12) 1 d PDU A 12
H28' H 0.6096 0.5422 0.8905 0.052 Uiso 0.531(12) 1 calc PR A 12
C29 C 0.8921(13) 0.6915(13) 0.5868(10) 0.0440(8) Uani 0.485(6) 1 d PDU A 9
H29 H 0.9490 0.7620 0.6155 0.053 Uiso 0.485(6) 1 calc PR A 9
C30 C 0.9218(13) 0.6288(12) 0.5060(10) 0.0433(8) Uani 0.485(6) 1 d PDU A 9
H30 H 0.9916 0.6579 0.4746 0.052 Uiso 0.485(6) 1 calc PR A 9
C31 C 0.8359(11) 0.5173(12) 0.4769(11) 0.0430(8) Uani 0.485(6) 1 d PDU A 9
H31 H 0.8547 0.4698 0.4260 0.052 Uiso 0.485(6) 1 calc PR A 9
C32 C 0.7265(7) 0.4691(8) 0.5146(7) 0.0431(8) Uani 0.485(6) 1 d PGDU A 9
C33 C 0.6384(9) 0.3623(8) 0.4795(7) 0.0439(8) Uani 0.485(6) 1 d PGU A 9
H33 H 0.6532 0.3119 0.4287 0.053 Uiso 0.485(6) 1 calc PR A 9
C34 C 0.5280(8) 0.3309(7) 0.5203(7) 0.0431(8) Uani 0.485(6) 1 d PGU A 9
H34 H 0.4690 0.2594 0.4968 0.052 Uiso 0.485(6) 1 calc PR A 9
C35 C 0.5059(8) 0.4062(8) 0.5963(7) 0.0433(8) Uani 0.485(6) 1 d PGDU A 9
C36 C 0.5940(9) 0.5131(8) 0.6314(7) 0.0422(8) Uani 0.485(6) 1 d PGDU A 9
C37 C 0.7044(8) 0.5445(7) 0.5906(8) 0.0420(8) Uani 0.485(6) 1 d PGDU A 9
C38 C 0.3985(12) 0.3791(12) 0.6362(10) 0.0432(8) Uani 0.485(6) 1 d PDU A 9
H38 H 0.3398 0.3071 0.6137 0.052 Uiso 0.485(6) 1 calc PR A 9
C39 C 0.3738(13) 0.4543(12) 0.7087(11) 0.0436(8) Uani 0.485(6) 1 d PDU A 9
H39 H 0.3001 0.4366 0.7363 0.052 Uiso 0.485(6) 1 calc PR A 9
C40 C 0.4674(15) 0.5593(13) 0.7376(14) 0.0435(8) Uani 0.485(6) 1 d PDU A 9
H40 H 0.4505 0.6127 0.7850 0.052 Uiso 0.485(6) 1 calc PR A 9
C29' C 0.8550(12) 0.6423(12) 0.5795(10) 0.0446(13) Uani 0.515(6) 1 d PDU A 10
H29' H 0.9156 0.7135 0.6005 0.054 Uiso 0.515(6) 1 calc PR A 10
C30' C 0.8785(13) 0.5644(11) 0.5046(10) 0.0450(13) Uani 0.515(6) 1 d PDU A 10
H30' H 0.9494 0.5811 0.4730 0.054 Uiso 0.515(6) 1 calc PR A 10
C31' C 0.7824(10) 0.4587(12) 0.4832(10) 0.0454(13) Uani 0.515(6) 1 d PDU A 10
H31' H 0.7908 0.4014 0.4350 0.055 Uiso 0.515(6) 1 calc PR A 10
C32' C 0.6733(7) 0.4325(8) 0.5295(7) 0.0441(13) Uani 0.515(6) 1 d PGDU A 10
C33' C 0.5781(9) 0.3283(7) 0.5022(6) 0.0438(13) Uani 0.515(6) 1 d PGU A 10
H33' H 0.5867 0.2703 0.4547 0.053 Uiso 0.515(6) 1 calc PR A 10
C34' C 0.4699(7) 0.3110(6) 0.5458(7) 0.0447(13) Uani 0.515(6) 1 d PGU A 10
H34' H 0.4061 0.2414 0.5275 0.054 Uiso 0.515(6) 1 calc PR A 10
C35' C 0.4569(7) 0.3978(8) 0.6167(7) 0.0433(13) Uani 0.515(6) 1 d PGDU A 10
C36' C 0.5521(8) 0.5020(7) 0.6440(7) 0.0414(12) Uani 0.515(6) 1 d PGDU A 10
C37' C 0.6603(7) 0.5193(6) 0.6004(7) 0.0408(12) Uani 0.515(6) 1 d PGDU A 10
C38' C 0.3511(11) 0.3902(12) 0.6656(10) 0.0447(13) Uani 0.515(6) 1 d PDU A 10
H38' H 0.2840 0.3229 0.6496 0.054 Uiso 0.515(6) 1 calc PR A 10
C39' C 0.3439(12) 0.4802(11) 0.7371(11) 0.0453(13) Uani 0.515(6) 1 d PDU A 10
H39' H 0.2728 0.4746 0.7671 0.054 Uiso 0.515(6) 1 calc PR A 10
C40' C 0.4457(11) 0.5774(13) 0.7616(12) 0.0450(13) Uani 0.515(6) 1 d PDU A 10
H40' H 0.4438 0.6365 0.8109 0.054 Uiso 0.515(6) 1 calc PR A 10
N1 N 0.4792(5) 1.2310(5) 0.8270(5) 0.0606(19) Uani 1 1 d D . .
N2 N 0.3558(6) 0.9957(5) 0.5999(5) 0.0594(17) Uani 1 1 d DU A .
N3 N 0.902(2) 0.8522(15) 0.7894(19) 0.044(2) Uani 0.469(12) 1 d PDU A 11
N4 N 0.7858(14) 0.6851(15) 0.8734(13) 0.041(2) Uani 0.469(12) 1 d PDU A 11
N3' N 0.9137(19) 0.8724(14) 0.7846(17) 0.0434(14) Uani 0.531(12) 1 d PDU A 12
N4' N 0.7578(9) 0.6792(13) 0.8807(11) 0.0412(14) Uani 0.531(12) 1 d PDU A 12
N5 N 0.7839(14) 0.6550(13) 0.6262(15) 0.042(2) Uani 0.485(6) 1 d PDU A 9
N6 N 0.574(3) 0.593(3) 0.708(3) 0.043(2) Uani 0.485(6) 1 d PU A 9
N5' N 0.7510(11) 0.6210(10) 0.6231(12) 0.042(3) Uani 0.515(6) 1 d PD A 10
N6' N 0.5484(19) 0.589(2) 0.716(2) 0.043(5) Uani 0.515(6) 1 d PD A 10
O1 O 0.6510(4) 0.8652(4) 0.7457(4) 0.0442(10) Uani 1 1 d U A .
O2 O 0.7279(5) 0.9148(4) 0.6060(4) 0.0489(13) Uani 1 1 d . A .
O3 O 0.9771(5) 1.3454(5) 0.6903(4) 0.0577(14) Uani 1 1 d D A .
O4 O 0.8857(5) 1.4750(4) 0.7476(4) 0.0577(14) Uani 1 1 d D A .
H4 H 0.9430 1.5241 0.7282 0.087 Uiso 1 1 calc R . .
O5 O 0.483(4) 1.3336(18) 0.857(2) 0.065(7) Uani 0.35(3) 1 d PDU A 5
O6 O 0.3875(17) 1.1600(17) 0.845(2) 0.065(6) Uani 0.35(3) 1 d PDU A 5
O5' O 0.505(2) 1.3188(12) 0.8917(12) 0.065(4) Uani 0.65(3) 1 d PDU A 6
O6' O 0.3752(9) 1.1724(10) 0.7901(13) 0.065(4) Uani 0.65(3) 1 d PDU A 6
O7 O 0.4168(10) 1.1033(9) 0.6046(9) 0.059(4) Uani 0.459(13) 1 d PDU A 1
O8 O 0.2718(15) 0.9498(16) 0.5367(11) 0.059(4) Uani 0.459(13) 1 d PDU A 1
O8' O 0.2590(12) 0.9800(14) 0.5487(10) 0.059(4) Uani 0.541(13) 1 d PDU A 2
O7' O 0.4549(8) 1.0329(9) 0.5568(7) 0.059(3) Uani 0.541(13) 1 d PDU A 2
O9 O 0.068(2) 0.641(3) 0.7236(19) 0.058(5) Uani 0.53(8) 1 d PDU A 3
O10 O 0.153(3) 0.623(3) 0.8656(17) 0.058(6) Uani 0.53(8) 1 d PDU A 3
H10A H 0.0929 0.5649 0.8641 0.087 Uiso 0.53(8) 1 calc PR A 3
O9' O 0.059(2) 0.653(3) 0.737(3) 0.058(6) Uani 0.47(8) 1 d PDU A 4
O10' O 0.170(3) 0.594(3) 0.841(3) 0.058(7) Uani 0.47(8) 1 d PDU A 4
H10' H 0.1074 0.5394 0.8418 0.087 Uiso 0.47(8) 1 calc PR A 4
O11 O 0.6080(5) 1.0441(5) 0.9367(4) 0.0603(15) Uani 1 1 d . . .
O12 O 0.5769(5) 0.8573(5) 0.9463(4) 0.0603(15) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.983(5) . ?
Zn1 N5 2.023(16) . ?
Zn1 N6 2.06(3) . ?
Zn1 N4 2.098(17) . ?
Zn1 N3 2.10(2) . ?
Zn1 N5' 2.109(13) . ?
Zn1 N4' 2.130(15) . ?
Zn1 N6' 2.266(18) . ?
Zn1 N3' 2.28(2) . ?
C1 O2 1.222(8) . ?
C1 O1 1.269(8) . ?
C1 C2 1.533(9) . ?
C2 C7 1.371(10) . ?
C2 C3 1.419(9) . ?
C3 C4 1.382(9) . ?
C4 C5 1.346(10) . ?
C4 C15 1.514(9) . ?
C5 C6 1.384(9) . ?
C6 C7 1.421(9) . ?
C6 N1 1.451(9) . ?
C7 C8 1.516(9) . ?
C8 C13 1.389(9) . ?
C8 C9 1.418(9) . ?
C9 C10 1.378(9) . ?
C9 N2 1.475(9) . ?
C10 C11 1.379(10) . ?
C11 C12 1.370(10) . ?
C11 C16 1.504(9) . ?
C12 C13 1.364(9) . ?
C13 C14 1.458(10) . ?
C14 O12 1.204(8) . ?
C14 O11 1.232(8) . ?
C15 O4 1.233(7) . ?
C15 O3 1.235(7) . ?
C16 O9' 1.226(11) . ?
C16 O10 1.231(11) . ?
C16 O10' 1.239(11) . ?
C16 O9 1.242(11) . ?
C17 C18 1.353(11) . ?
C17 N3 1.57(2) . ?
C18 C19 1.06(2) . ?
C19 C20 1.36(2) . ?
C20 C25 1.40(2) . ?
C20 C21 1.43(2) . ?
C21 C22 1.36(2) . ?
C22 C23 1.56(2) . ?
C23 C26 1.359(11) . ?
C23 C24 1.59(2) . ?
C24 N4 1.32(2) . ?
C24 C25 1.47(2) . ?
C25 N3 1.28(3) . ?
C26 C27 1.329(11) . ?
C27 C28 1.48(2) . ?
C28 N4 1.30(2) . ?
C17' N3' 1.14(2) . ?
C17' C18' 1.358(11) . ?
C18' C19' 1.59(2) . ?
C19' C20' 1.415(15) . ?
C20' C21' 1.3900 . ?
C20' C25' 1.3900 . ?
C21' C22' 1.3900 . ?
C22' C23' 1.3900 . ?
C23' C26' 1.291(13) . ?
C23' C24' 1.3900 . ?
C24' N4' 1.383(8) . ?
C24' C25' 1.3900 . ?
C25' N3' 1.51(3) . ?
C26' C27' 1.396(11) . ?
C27' C28' 1.36(2) . ?
C28' N4' 1.360(9) . ?
C29 N5 1.363(12) . ?
C29 C30 1.392(10) . ?
C30 C31 1.401(11) . ?
C31 C32 1.381(10) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C38 1.352(10) . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C36 N6 1.42(2) . ?
C37 N5 1.379(11) . ?
C38 C39 1.367(11) . ?
C39 C40 1.390(10) . ?
C40 N6 1.28(3) . ?
C29' N5' 1.345(11) . ?
C29' C30' 1.405(10) . ?
C30' C31' 1.398(11) . ?
C31' C32' 1.414(10) . ?
C32' C33' 1.3900 . ?
C32' C37' 1.3900 . ?
C33' C34' 1.3900 . ?
C34' C35' 1.3900 . ?
C35' C36' 1.3900 . ?
C35' C38' 1.415(10) . ?
C36' N6' 1.363(13) . ?
C36' C37' 1.3900 . ?
C37' N5' 1.337(10) . ?
C38' C39' 1.398(11) . ?
C39' C40' 1.380(10) . ?
C40' N6' 1.358(12) . ?
N1 O6 1.202(12) . ?
N1 O5 1.226(12) . ?
N1 O5' 1.250(10) . ?
N1 O6' 1.252(9) . ?
N2 O8 1.230(10) . ?
N2 O8' 1.250(10) . ?
N2 O7 1.251(9) . ?
N2 O7' 1.304(9) . ?

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 Zn1 N5 127.3(7) . . ?
O1 Zn1 N6 97.9(12) . . ?
N5 Zn1 N6 81.9(8) . . ?
O1 Zn1 N4 120.4(5) . . ?
N5 Zn1 N4 111.7(8) . . ?
N6 Zn1 N4 97.8(15) . . ?
O1 Zn1 N3 94.1(6) . . ?
N5 Zn1 N3 94.1(8) . . ?
N6 Zn1 N3 167.3(15) . . ?
N4 Zn1 N3 72.3(8) . . ?
O1 Zn1 N5' 129.0(5) . . ?
N5 Zn1 N5' 12.6(4) . . ?
N6 Zn1 N5' 69.5(7) . . ?
N4 Zn1 N5' 110.4(7) . . ?
N3 Zn1 N5' 105.9(7) . . ?
O1 Zn1 N4' 115.2(5) . . ?
N5 Zn1 N4' 117.4(8) . . ?
N6 Zn1 N4' 91.5(14) . . ?
N4 Zn1 N4' 9.0(6) . . ?
N3 Zn1 N4' 79.5(7) . . ?
N5' Zn1 N4' 114.4(7) . . ?
O1 Zn1 N6' 93.2(8) . . ?
N5 Zn1 N6' 87.8(5) . . ?
N6 Zn1 N6' 6.1(9) . . ?
N4 Zn1 N6' 96.9(12) . . ?
N3 Zn1 N6' 169.0(13) . . ?
N5' Zn1 N6' 75.5(4) . . ?
N4' Zn1 N6' 90.0(11) . . ?
O1 Zn1 N3' 90.7(5) . . ?
N5 Zn1 N3' 93.7(6) . . ?
N6 Zn1 N3' 171.4(13) . . ?
N4 Zn1 N3' 76.9(7) . . ?
N3 Zn1 N3' 4.7(11) . . ?
N5' Zn1 N3' 105.7(6) . . ?
N4' Zn1 N3' 83.9(6) . . ?
N6' Zn1 N3' 173.8(12) . . ?
O2 C1 O1 127.8(6) . . ?
O2 C1 C2 119.5(6) . . ?
O1 C1 C2 112.5(6) . . ?
C7 C2 C3 119.6(6) . . ?
C7 C2 C1 125.2(6) . . ?
C3 C2 C1 115.2(6) . . ?
C4 C3 C2 121.7(7) . . ?
C5 C4 C3 118.7(6) . . ?
C5 C4 C15 121.1(6) . . ?
C3 C4 C15 120.0(6) . . ?
C4 C5 C6 121.1(7) . . ?
C5 C6 C7 121.5(7) . . ?
C5 C6 N1 117.5(6) . . ?
C7 C6 N1 121.0(6) . . ?
C2 C7 C6 117.3(6) . . ?
C2 C7 C8 120.0(6) . . ?
C6 C7 C8 122.6(6) . . ?
C13 C8 C9 115.9(6) . . ?
C13 C8 C7 122.5(6) . . ?
C9 C8 C7 121.6(6) . . ?
C10 C9 C8 118.8(6) . . ?
C10 C9 N2 118.9(6) . . ?
C8 C9 N2 122.2(5) . . ?
C9 C10 C11 124.5(7) . . ?
C12 C11 C10 115.9(6) . . ?
C12 C11 C16 121.0(6) . . ?
C10 C11 C16 123.0(6) . . ?
C13 C12 C11 121.5(7) . . ?
C12 C13 C8 123.4(7) . . ?
C12 C13 C14 116.4(6) . . ?
C8 C13 C14 120.1(6) . . ?
O12 C14 O11 123.4(7) . . ?
O12 C14 C13 119.5(6) . . ?
O11 C14 C13 117.1(6) . . ?
O4 C15 O3 126.8(6) . . ?
O4 C15 C4 116.0(6) . . ?
O3 C15 C4 117.2(6) . . ?
O9' C16 O10 122.5(18) . . ?
O9' C16 O10' 125(2) . . ?
O10 C16 O9 127(2) . . ?
O10' C16 O9 122.9(18) . . ?
O9' C16 C11 116.9(17) . . ?
O10 C16 C11 116.5(12) . . ?
O10' C16 C11 117.7(15) . . ?
O9 C16 C11 115.8(13) . . ?
C18 C17 N3 130.9(18) . . ?
C19 C18 C17 120.5(18) . . ?
C18 C19 C20 120.8(18) . . ?
C19 C20 C25 119.4(15) . . ?
C19 C20 C21 122.6(15) . . ?
C25 C20 C21 117.8(14) . . ?
C22 C21 C20 120.0(14) . . ?
C21 C22 C23 130.7(15) . . ?
C26 C23 C22 131.0(14) . . ?
C26 C23 C24 120.2(13) . . ?
C22 C23 C24 104.8(11) . . ?
N4 C24 C25 121.8(16) . . ?
N4 C24 C23 115.9(13) . . ?
C25 C24 C23 121.7(12) . . ?
N3 C25 C20 132.0(16) . . ?
N3 C25 C24 103.9(15) . . ?
C20 C25 C24 124.1(15) . . ?
C27 C26 C23 116.9(14) . . ?
C26 C27 C28 118.5(14) . . ?
N4 C28 C27 124.6(15) . . ?
N3' C17' C18' 118.4(19) . . ?
C17' C18' C19' 117.5(13) . . ?
C20' C19' C18' 119.9(12) . . ?
C21' C20' C25' 120.0 . . ?
C21' C20' C19' 124.5(9) . . ?
C25' C20' C19' 115.3(9) . . ?
C20' C21' C22' 120.0 . . ?
C23' C22' C21' 120.0 . . ?
C26' C23' C22' 119.3(9) . . ?
C26' C23' C24' 119.9(9) . . ?
C22' C23' C24' 120.0 . . ?
N4' C24' C25' 121.0(8) . . ?
N4' C24' C23' 118.3(9) . . ?
C25' C24' C23' 120.0 . . ?
C24' C25' C20' 120.0 . . ?
C24' C25' N3' 123.7(9) . . ?
C20' C25' N3' 116.2(9) . . ?
C23' C26' C27' 121.8(13) . . ?
C28' C27' C26' 119.4(13) . . ?
N4' C28' C27' 118.2(13) . . ?
N5 C29 C30 123.4(14) . . ?
C29 C30 C31 113.0(13) . . ?
C32 C31 C30 127.9(13) . . ?
C31 C32 C33 126.8(9) . . ?
C31 C32 C37 113.0(9) . . ?
C33 C32 C37 120.0 . . ?
C32 C33 C34 120.0 . . ?
C35 C34 C33 120.0 . . ?
C38 C35 C34 121.3(8) . . ?
C38 C35 C36 118.7(8) . . ?
C34 C35 C36 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 N6 118.7(14) . . ?
C35 C36 N6 121.3(14) . . ?
N5 C37 C36 116.1(9) . . ?
N5 C37 C32 123.8(9) . . ?
C36 C37 C32 120.0 . . ?
C35 C38 C39 122.0(12) . . ?
C38 C39 C40 114.7(14) . . ?
N6 C40 C39 128.9(19) . . ?
N5' C29' C30' 124.6(13) . . ?
C31' C30' C29' 111.7(12) . . ?
C30' C31' C32' 124.9(12) . . ?
C33' C32' C37' 120.0 . . ?
C33' C32' C31' 122.6(8) . . ?
C37' C32' C31' 117.3(8) . . ?
C32' C33' C34' 120.0 . . ?
C35' C34' C33' 120.0 . . ?
C36' C35' C34' 120.0 . . ?
C36' C35' C38' 115.1(8) . . ?
C34' C35' C38' 124.9(8) . . ?
N6' C36' C35' 123.6(9) . . ?
N6' C36' C37' 116.4(9) . . ?
C35' C36' C37' 120.0 . . ?
N5' C37' C36' 120.7(8) . . ?
N5' C37' C32' 119.3(8) . . ?
C36' C37' C32' 120.0 . . ?
C39' C38' C35' 122.3(12) . . ?
C40' C39' C38' 117.8(13) . . ?
N6' C40' C39' 121.7(14) . . ?
O6 N1 O5 111(3) . . ?
O6 N1 O5' 108.1(17) . . ?
O5 N1 O6' 111(2) . . ?
O5' N1 O6' 126.4(14) . . ?
O6 N1 C6 125.0(12) . . ?
O5 N1 C6 124(2) . . ?
O5' N1 C6 118.2(12) . . ?
O6' N1 C6 115.0(9) . . ?
O8 N2 O7 121.5(12) . . ?
O8' N2 O7 108.4(10) . . ?
O8 N2 O7' 108.0(12) . . ?
O8' N2 O7' 115.8(10) . . ?
O7 N2 O7' 56.3(7) . . ?
O8 N2 C9 118.4(10) . . ?
O8' N2 C9 121.5(9) . . ?
O7 N2 C9 117.0(7) . . ?
O7' N2 C9 119.4(6) . . ?
C25 N3 C17 96.0(18) . . ?
C25 N3 Zn1 126.6(14) . . ?
C17 N3 Zn1 136.1(17) . . ?
C28 N4 C24 119.2(17) . . ?
C28 N4 Zn1 125.6(13) . . ?
C24 N4 Zn1 114.5(12) . . ?
C17' N3' C25' 132(2) . . ?
C17' N3' Zn1 126.8(19) . . ?
C25' N3' Zn1 100.3(9) . . ?
C28' N4' C24' 121.2(13) . . ?
C28' N4' Zn1 127.9(10) . . ?
C24' N4' Zn1 109.7(8) . . ?
C29 N5 C37 118.5(13) . . ?
C29 N5 Zn1 127.9(10) . . ?
C37 N5 Zn1 113.3(9) . . ?
C40 N6 C36 114(2) . . ?
C40 N6 Zn1 136.4(17) . . ?
C36 N6 Zn1 109.3(17) . . ?
C37' N5' C29' 122.1(12) . . ?
C37' N5' Zn1 115.3(8) . . ?
C29' N5' Zn1 122.3(8) . . ?
C40' N6' C36' 119.4(15) . . ?
C40' N6' Zn1 129.0(11) . . ?
C36' N6' Zn1 111.5(9) . . ?
C1 O1 Zn1 114.4(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C7 139.7(8) . . . . ?
O1 C1 C2 C7 -45.9(10) . . . . ?
O2 C1 C2 C3 -42.6(9) . . . . ?
O1 C1 C2 C3 131.9(7) . . . . ?
C7 C2 C3 C4 3.7(11) . . . . ?
C1 C2 C3 C4 -174.1(6) . . . . ?
C2 C3 C4 C5 -0.1(11) . . . . ?
C2 C3 C4 C15 174.2(7) . . . . ?
C3 C4 C5 C6 -2.9(11) . . . . ?
C15 C4 C5 C6 -177.2(7) . . . . ?
C4 C5 C6 C7 2.5(11) . . . . ?
C4 C5 C6 N1 -179.2(6) . . . . ?
C3 C2 C7 C6 -4.1(10) . . . . ?
C1 C2 C7 C6 173.6(7) . . . . ?
C3 C2 C7 C8 177.9(6) . . . . ?
C1 C2 C7 C8 -4.4(11) . . . . ?
C5 C6 C7 C2 1.1(11) . . . . ?
N1 C6 C7 C2 -177.1(6) . . . . ?
C5 C6 C7 C8 179.0(7) . . . . ?
N1 C6 C7 C8 0.8(11) . . . . ?
C2 C7 C8 C13 82.3(9) . . . . ?
C6 C7 C8 C13 -95.5(9) . . . . ?
C2 C7 C8 C9 -95.0(8) . . . . ?
C6 C7 C8 C9 87.2(9) . . . . ?
C13 C8 C9 C10 -1.2(10) . . . . ?
C7 C8 C9 C10 176.2(6) . . . . ?
C13 C8 C9 N2 -177.7(6) . . . . ?
C7 C8 C9 N2 -0.3(10) . . . . ?
C8 C9 C10 C11 2.2(11) . . . . ?
N2 C9 C10 C11 178.9(6) . . . . ?
C9 C10 C11 C12 -2.3(11) . . . . ?
C9 C10 C11 C16 -179.5(7) . . . . ?
C10 C11 C12 C13 1.4(11) . . . . ?
C16 C11 C12 C13 178.7(7) . . . . ?
C11 C12 C13 C8 -0.6(12) . . . . ?
C11 C12 C13 C14 -176.0(7) . . . . ?
C9 C8 C13 C12 0.5(11) . . . . ?
C7 C8 C13 C12 -177.0(7) . . . . ?
C9 C8 C13 C14 175.7(6) . . . . ?
C7 C8 C13 C14 -1.7(11) . . . . ?
C12 C13 C14 O12 34.1(11) . . . . ?
C8 C13 C14 O12 -141.5(8) . . . . ?
C12 C13 C14 O11 -145.1(7) . . . . ?
C8 C13 C14 O11 39.3(10) . . . . ?
C5 C4 C15 O4 -7.6(10) . . . . ?
C3 C4 C15 O4 178.2(7) . . . . ?
C5 C4 C15 O3 172.0(7) . . . . ?
C3 C4 C15 O3 -2.2(10) . . . . ?
C12 C11 C16 O9' 165(2) . . . . ?
C10 C11 C16 O9' -18(3) . . . . ?
C12 C11 C16 O10 7(2) . . . . ?
C10 C11 C16 O10 -176(2) . . . . ?
C12 C11 C16 O10' -21(3) . . . . ?
C10 C11 C16 O10' 156(3) . . . . ?
C12 C11 C16 O9 179(2) . . . . ?
C10 C11 C16 O9 -4(2) . . . . ?
N3 C17 C18 C19 -4.0(12) . . . . ?
C17 C18 C19 C20 1.1(10) . . . . ?
C18 C19 C20 C25 -2.1(19) . . . . ?
C18 C19 C20 C21 -176.6(12) . . . . ?
C19 C20 C21 C22 -178.6(15) . . . . ?
C25 C20 C21 C22 7(2) . . . . ?
C20 C21 C22 C23 -12(3) . . . . ?
C21 C22 C23 C26 164.5(19) . . . . ?
C21 C22 C23 C24 8(2) . . . . ?
C26 C23 C24 N4 12(2) . . . . ?
C22 C23 C24 N4 171.8(17) . . . . ?
C26 C23 C24 C25 -158.6(17) . . . . ?
C22 C23 C24 C25 1.4(18) . . . . ?
C19 C20 C25 N3 7(3) . . . . ?
C21 C20 C25 N3 -178(2) . . . . ?
C19 C20 C25 C24 -173.3(15) . . . . ?
C21 C20 C25 C24 1(2) . . . . ?
N4 C24 C25 N3 4(2) . . . . ?
C23 C24 C25 N3 174.0(17) . . . . ?
N4 C24 C25 C20 -175.4(18) . . . . ?
C23 C24 C25 C20 -5(2) . . . . ?
C22 C23 C26 C27 -175.8(17) . . . . ?
C24 C23 C26 C27 -22(2) . . . . ?
C23 C26 C27 C28 13(2) . . . . ?
C26 C27 C28 N4 8(3) . . . . ?
N3' C17' C18' C19' 5.3(12) . . . . ?
C17' C18' C19' C20' -2.0(6) . . . . ?
C18' C19' C20' C21' 177.3(6) . . . . ?
C18' C19' C20' C25' 3.2(9) . . . . ?
C25' C20' C21' C22' 0.0 . . . . ?
C19' C20' C21' C22' -173.8(10) . . . . ?
C20' C21' C22' C23' 0.0 . . . . ?
C21' C22' C23' C26' -169.9(12) . . . . ?
C21' C22' C23' C24' 0.0 . . . . ?
C26' C23' C24' N4' -0.9(14) . . . . ?
C22' C23' C24' N4' -170.7(13) . . . . ?
C26' C23' C24' C25' 169.9(12) . . . . ?
C22' C23' C24' C25' 0.0 . . . . ?
N4' C24' C25' C20' 170.5(14) . . . . ?
C23' C24' C25' C20' 0.0 . . . . ?
N4' C24' C25' N3' -8.6(15) . . . . ?
C23' C24' C25' N3' -179.0(13) . . . . ?
C21' C20' C25' C24' 0.0 . . . . ?
C19' C20' C25' C24' 174.4(9) . . . . ?
C21' C20' C25' N3' 179.1(12) . . . . ?
C19' C20' C25' N3' -6.5(12) . . . . ?
C22' C23' C26' C27' 178.8(10) . . . . ?
C24' C23' C26' C27' 8.9(17) . . . . ?
C23' C26' C27' C28' -8(2) . . . . ?
C26' C27' C28' N4' -1(2) . . . . ?
N5 C29 C30 C31 -8(2) . . . . ?
C29 C30 C31 C32 4(2) . . . . ?
C30 C31 C32 C33 174.5(12) . . . . ?
C30 C31 C32 C37 -0.2(19) . . . . ?
C31 C32 C33 C34 -174.4(13) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C38 178.7(12) . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C38 C35 C36 C37 -178.7(12) . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C38 C35 C36 N6 0(3) . . . . ?
C34 C35 C36 N6 179(3) . . . . ?
C35 C36 C37 N5 176.5(15) . . . . ?
N6 C36 C37 N5 -3(3) . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
N6 C36 C37 C32 -179(3) . . . . ?
C31 C32 C37 N5 -1.2(17) . . . . ?
C33 C32 C37 N5 -176.3(17) . . . . ?
C31 C32 C37 C36 175.1(11) . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C34 C35 C38 C39 -177.6(12) . . . . ?
C36 C35 C38 C39 1.1(19) . . . . ?
C35 C38 C39 C40 0(2) . . . . ?
C38 C39 C40 N6 -3(4) . . . . ?
N5' C29' C30' C31' -3(2) . . . . ?
C29' C30' C31' C32' 1(2) . . . . ?
C30' C31' C32' C33' 176.8(11) . . . . ?
C30' C31' C32' C37' 1.1(18) . . . . ?
C37' C32' C33' C34' 0.0 . . . . ?
C31' C32' C33' C34' -175.6(11) . . . . ?
C32' C33' C34' C35' 0.0 . . . . ?
C33' C34' C35' C36' 0.0 . . . . ?
C33' C34' C35' C38' 179.7(11) . . . . ?
C34' C35' C36' N6' -177(2) . . . . ?
C38' C35' C36' N6' 3(2) . . . . ?
C34' C35' C36' C37' 0.0 . . . . ?
C38' C35' C36' C37' -179.7(10) . . . . ?
N6' C36' C37' N5' -5(2) . . . . ?
C35' C36' C37' N5' 177.3(13) . . . . ?
N6' C36' C37' C32' 177(2) . . . . ?
C35' C36' C37' C32' 0.0 . . . . ?
C33' C32' C37' N5' -177.3(13) . . . . ?
C31' C32' C37' N5' -1.5(14) . . . . ?
C33' C32' C37' C36' 0.0 . . . . ?
C31' C32' C37' C36' 175.9(10) . . . . ?
C36' C35' C38' C39' -0.9(17) . . . . ?
C34' C35' C38' C39' 179.4(11) . . . . ?
C35' C38' C39' C40' -2(2) . . . . ?
C38' C39' C40' N6' 3(3) . . . . ?
C5 C6 N1 O6 -176(2) . . . . ?
C7 C6 N1 O6 3(2) . . . . ?
C5 C6 N1 O5 0(2) . . . . ?
C7 C6 N1 O5 178(2) . . . . ?
C5 C6 N1 O5' -31.9(13) . . . . ?
C7 C6 N1 O5' 146.4(12) . . . . ?
C5 C6 N1 O6' 141.1(10) . . . . ?
C7 C6 N1 O6' -40.5(12) . . . . ?
C10 C9 N2 O8 -3.9(14) . . . . ?
C8 C9 N2 O8 172.7(13) . . . . ?
C10 C9 N2 O8' 19.7(13) . . . . ?
C8 C9 N2 O8' -163.8(11) . . . . ?
C10 C9 N2 O7 156.4(9) . . . . ?
C8 C9 N2 O7 -27.1(11) . . . . ?
C10 C9 N2 O7' -138.9(8) . . . . ?
C8 C9 N2 O7' 37.6(10) . . . . ?
C20 C25 N3 C17 -8(3) . . . . ?
C24 C25 N3 C17 172.6(13) . . . . ?
C20 C25 N3 Zn1 -176.5(14) . . . . ?
C24 C25 N3 Zn1 4(2) . . . . ?
C18 C17 N3 C25 7(2) . . . . ?
C18 C17 N3 Zn1 173.5(12) . . . . ?
O1 Zn1 N3 C25 113.5(19) . . . . ?
N5 Zn1 N3 C25 -119(2) . . . . ?
N6 Zn1 N3 C25 -47(6) . . . . ?
N4 Zn1 N3 C25 -7.1(19) . . . . ?
N5' Zn1 N3 C25 -114(2) . . . . ?
N4' Zn1 N3 C25 -1.4(19) . . . . ?
N6' Zn1 N3 C25 -19(5) . . . . ?
N3' Zn1 N3 C25 157(15) . . . . ?
O1 Zn1 N3 C17 -50.0(19) . . . . ?
N5 Zn1 N3 C17 78(2) . . . . ?
N6 Zn1 N3 C17 149(4) . . . . ?
N4 Zn1 N3 C17 -171(2) . . . . ?
N5' Zn1 N3 C17 83(2) . . . . ?
N4' Zn1 N3 C17 -165(2) . . . . ?
N6' Zn1 N3 C17 178(2) . . . . ?
N3' Zn1 N3 C17 -7(12) . . . . ?
C27 C28 N4 C24 -18(3) . . . . ?
C27 C28 N4 Zn1 171.1(13) . . . . ?
C25 C24 N4 C28 178.7(16) . . . . ?
C23 C24 N4 C28 8(2) . . . . ?
C25 C24 N4 Zn1 -10(2) . . . . ?
C23 C24 N4 Zn1 179.8(11) . . . . ?
O1 Zn1 N4 C28 94.6(16) . . . . ?
N5 Zn1 N4 C28 -93.7(16) . . . . ?
N6 Zn1 N4 C28 -9.4(18) . . . . ?
N3 Zn1 N4 C28 178.9(19) . . . . ?
N5' Zn1 N4 C28 -80.3(17) . . . . ?
N4' Zn1 N4 C28 37(5) . . . . ?
N6' Zn1 N4 C28 -3.3(17) . . . . ?
N3' Zn1 N4 C28 177.5(18) . . . . ?
O1 Zn1 N4 C24 -76.3(15) . . . . ?
N5 Zn1 N4 C24 95.4(15) . . . . ?
N6 Zn1 N4 C24 179.8(16) . . . . ?
N3 Zn1 N4 C24 8.0(15) . . . . ?
N5' Zn1 N4 C24 108.8(14) . . . . ?
N4' Zn1 N4 C24 -134(6) . . . . ?
N6' Zn1 N4 C24 -174.2(14) . . . . ?
N3' Zn1 N4 C24 6.7(14) . . . . ?
C18' C17' N3' C25' -11(2) . . . . ?
C18' C17' N3' Zn1 -176.4(9) . . . . ?
C24' C25' N3' C17' -169.1(16) . . . . ?
C20' C25' N3' C17' 12(3) . . . . ?
C24' C25' N3' Zn1 -0.7(13) . . . . ?
C20' C25' N3' Zn1 -179.8(6) . . . . ?
O1 Zn1 N3' C17' -70.0(16) . . . . ?
N5 Zn1 N3' C17' 57.5(18) . . . . ?
N4 Zn1 N3' C17' 169.0(18) . . . . ?
N3 Zn1 N3' C17' 153(14) . . . . ?
N5' Zn1 N3' C17' 61.1(18) . . . . ?
N4' Zn1 N3' C17' 174.7(17) . . . . ?
O1 Zn1 N3' C25' 120.9(10) . . . . ?
N5 Zn1 N3' C25' -111.6(12) . . . . ?
N4 Zn1 N3' C25' -0.2(10) . . . . ?
N3 Zn1 N3' C25' -16(12) . . . . ?
N5' Zn1 N3' C25' -108.1(11) . . . . ?
N4' Zn1 N3' C25' 5.6(10) . . . . ?
C27' C28' N4' C24' 9(2) . . . . ?
C27' C28' N4' Zn1 174.7(11) . . . . ?
C25' C24' N4' C28' -178.7(12) . . . . ?
C23' C24' N4' C28' -8(2) . . . . ?
C25' C24' N4' Zn1 13.0(14) . . . . ?
C23' C24' N4' Zn1 -176.4(6) . . . . ?
O1 Zn1 N4' C28' 94.9(15) . . . . ?
N5 Zn1 N4' C28' -86.3(15) . . . . ?
N6 Zn1 N4' C28' -4.6(17) . . . . ?
N4 Zn1 N4' C28' -138(7) . . . . ?
N3 Zn1 N4' C28' -175.5(16) . . . . ?
N5' Zn1 N4' C28' -72.7(15) . . . . ?
N6' Zn1 N4' C28' 1.3(15) . . . . ?
N3' Zn1 N4' C28' -177.3(16) . . . . ?
O1 Zn1 N4' C24' -97.8(11) . . . . ?
N5 Zn1 N4' C24' 81.1(12) . . . . ?
N6 Zn1 N4' C24' 162.8(14) . . . . ?
N4 Zn1 N4' C24' 29(5) . . . . ?
N3 Zn1 N4' C24' -8.1(12) . . . . ?
N5' Zn1 N4' C24' 94.6(11) . . . . ?
N6' Zn1 N4' C24' 168.6(12) . . . . ?
N3' Zn1 N4' C24' -9.9(12) . . . . ?
C30 C29 N5 C37 7(3) . . . . ?
C30 C29 N5 Zn1 179.6(14) . . . . ?
C36 C37 N5 C29 -178.3(15) . . . . ?
C32 C37 N5 C29 -2(3) . . . . ?
C36 C37 N5 Zn1 7.8(19) . . . . ?
C32 C37 N5 Zn1 -175.8(7) . . . . ?
O1 Zn1 N5 C29 85(2) . . . . ?
N6 Zn1 N5 C29 179(2) . . . . ?
N4 Zn1 N5 C29 -86(2) . . . . ?
N3 Zn1 N5 C29 -13(2) . . . . ?
N5' Zn1 N5 C29 -172(7) . . . . ?
N4' Zn1 N5 C29 -93.2(19) . . . . ?
N6' Zn1 N5 C29 178(2) . . . . ?
N3' Zn1 N5 C29 -8(2) . . . . ?
O1 Zn1 N5 C37 -101.3(15) . . . . ?
N6 Zn1 N5 C37 -8(2) . . . . ?
N4 Zn1 N5 C37 87.7(16) . . . . ?
N3 Zn1 N5 C37 160.3(16) . . . . ?
N5' Zn1 N5 C37 1(4) . . . . ?
N4' Zn1 N5 C37 80.0(16) . . . . ?
N6' Zn1 N5 C37 -8.9(18) . . . . ?
N3' Zn1 N5 C37 165.0(16) . . . . ?
C39 C40 N6 C36 4(6) . . . . ?
C39 C40 N6 Zn1 -176(3) . . . . ?
C37 C36 N6 C40 176(3) . . . . ?
C35 C36 N6 C40 -3(5) . . . . ?
C37 C36 N6 Zn1 -4(4) . . . . ?
C35 C36 N6 Zn1 177.2(11) . . . . ?
O1 Zn1 N6 C40 -47(6) . . . . ?
N5 Zn1 N6 C40 -174(6) . . . . ?
N4 Zn1 N6 C40 75(5) . . . . ?
N3 Zn1 N6 C40 113(5) . . . . ?
N5' Zn1 N6 C40 -176(6) . . . . ?
N4' Zn1 N6 C40 68(5) . . . . ?
N6' Zn1 N6 C40 -7(19) . . . . ?
O1 Zn1 N6 C36 133(3) . . . . ?
N5 Zn1 N6 C36 6(3) . . . . ?
N4 Zn1 N6 C36 -105(3) . . . . ?
N3 Zn1 N6 C36 -67(7) . . . . ?
N5' Zn1 N6 C36 4(2) . . . . ?
N4' Zn1 N6 C36 -112(3) . . . . ?
N6' Zn1 N6 C36 173(27) . . . . ?
C36' C37' N5' C29' -177.5(13) . . . . ?
C32' C37' N5' C29' 0(2) . . . . ?
C36' C37' N5' Zn1 9.9(16) . . . . ?
C32' C37' N5' Zn1 -172.8(6) . . . . ?
C30' C29' N5' C37' 2(3) . . . . ?
C30' C29' N5' Zn1 174.6(12) . . . . ?
O1 Zn1 N5' C37' -89.8(13) . . . . ?
N5 Zn1 N5' C37' -177(6) . . . . ?
N6 Zn1 N5' C37' -6.4(19) . . . . ?
N4 Zn1 N5' C37' 84.5(13) . . . . ?
N3 Zn1 N5' C37' 161.1(13) . . . . ?
N4' Zn1 N5' C37' 75.7(13) . . . . ?
N6' Zn1 N5' C37' -7.6(16) . . . . ?
N3' Zn1 N5' C37' 166.1(13) . . . . ?
O1 Zn1 N5' C29' 97.5(14) . . . . ?
N5 Zn1 N5' C29' 10(4) . . . . ?
N6 Zn1 N5' C29' -179(2) . . . . ?
N4 Zn1 N5' C29' -88.2(15) . . . . ?
N3 Zn1 N5' C29' -11.5(17) . . . . ?
N4' Zn1 N5' C29' -96.9(14) . . . . ?
N6' Zn1 N5' C29' 179.8(19) . . . . ?
N3' Zn1 N5' C29' -6.6(16) . . . . ?
C39' C40' N6' C36' -1(5) . . . . ?
C39' C40' N6' Zn1 -178(2) . . . . ?
C35' C36' N6' C40' -2(5) . . . . ?
C37' C36' N6' C40' -180(3) . . . . ?
C35' C36' N6' Zn1 175.7(8) . . . . ?
C37' C36' N6' Zn1 -2(3) . . . . ?
O1 Zn1 N6' C40' -48(4) . . . . ?
N5 Zn1 N6' C40' -175(4) . . . . ?
N6 Zn1 N6' C40' 172(27) . . . . ?
N4 Zn1 N6' C40' 73(4) . . . . ?
N3 Zn1 N6' C40' 84(5) . . . . ?
N5' Zn1 N6' C40' -177(4) . . . . ?
N4' Zn1 N6' C40' 67(4) . . . . ?
O1 Zn1 N6' C36' 134(2) . . . . ?
N5 Zn1 N6' C36' 7(2) . . . . ?
N6 Zn1 N6' C36' -6(22) . . . . ?
N4 Zn1 N6' C36' -104(2) . . . . ?
N3 Zn1 N6' C36' -93(4) . . . . ?
N5' Zn1 N6' C36' 5(2) . . . . ?
N4' Zn1 N6' C36' -110(2) . . . . ?
O2 C1 O1 Zn1 18.9(10) . . . . ?
C2 C1 O1 Zn1 -155.0(4) . . . . ?
N5 Zn1 O1 C1 -29.5(7) . . . . ?
N6 Zn1 O1 C1 -115.3(12) . . . . ?
N4 Zn1 O1 C1 140.8(6) . . . . ?
N3 Zn1 O1 C1 68.9(8) . . . . ?
N5' Zn1 O1 C1 -45.3(6) . . . . ?
N4' Zn1 O1 C1 149.2(5) . . . . ?
N6' Zn1 O1 C1 -119.2(9) . . . . ?
N3' Zn1 O1 C1 65.7(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.225
####################################################################### 
# 
# 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-sr
_database_code_depnum_ccdc_archive 'CCDC 1444252'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H8 Cd3 N4 O27'
_chemical_formula_weight         1217.62

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.0719(6)
_cell_length_b                   22.5340(11)
_cell_length_c                   16.8938(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.9080(10)
_cell_angle_gamma                90.00
_cell_volume                     4902.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8885
_cell_measurement_theta_min      2.402
_cell_measurement_theta_max      26.365

_exptl_crystal_description       columnar
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6829
_exptl_absorpt_correction_T_max  0.7161
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26827
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         26.37
_reflns_number_total             9923
_reflns_number_gt                8050
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0800P)²+0.1684P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9923
_refine_ls_number_parameters     595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.1204
_refine_ls_wR_factor_gt          0.1145
_refine_ls_goodness_of_fit_ref   1.008
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7183(3) 0.10971(19) 0.0804(2) 0.0250(9) Uani 1 1 d . . .
C2 C 0.7871(3) 0.05569(17) 0.0899(2) 0.0215(8) Uani 1 1 d . . .
C3 C 0.7994(3) 0.02291(19) 0.0207(2) 0.0264(9) Uani 1 1 d . . .
H3 H 0.7665 0.0358 -0.0295 0.032 Uiso 1 1 calc R . .
C4 C 0.8591(3) -0.0274(2) 0.0265(3) 0.0274(9) Uani 1 1 d . . .
C5 C 0.9177(4) -0.0434(2) 0.1008(3) 0.0339(10) Uani 1 1 d . . .
H5 H 0.9638 -0.0751 0.1049 0.041 Uiso 1 1 calc R . .
C6 C 0.9053(4) -0.0107(2) 0.1681(3) 0.0316(10) Uani 1 1 d . . .
C7 C 0.8393(3) 0.03723(18) 0.1655(3) 0.0244(9) Uani 1 1 d . . .
C8 C -0.1786(3) 0.07259(18) 0.2372(2) 0.0221(8) Uani 1 1 d . . .
C9 C -0.2613(3) 0.06321(17) 0.2776(2) 0.0233(8) Uani 1 1 d . . .
C10 C -0.2801(3) 0.09855(18) 0.3408(2) 0.0246(9) Uani 1 1 d . . .
H10 H -0.3351 0.0900 0.3673 0.030 Uiso 1 1 calc R . .
C11 C -0.2163(3) 0.14647(19) 0.3638(2) 0.0267(9) Uani 1 1 d . . .
C12 C -0.1374(3) 0.15989(19) 0.3224(3) 0.0283(9) Uani 1 1 d . . .
H12 H -0.0983 0.1941 0.3352 0.034 Uiso 1 1 calc R . .
C13 C -0.1152(3) 0.12266(19) 0.2614(2) 0.0244(9) Uani 1 1 d . . .
C14 C -0.0218(3) 0.1336(2) 0.2227(2) 0.0270(9) Uani 1 1 d . . .
C15 C 0.1383(3) 0.0670(2) 0.0445(3) 0.0280(9) Uani 1 1 d . . .
C16 C 0.7624(3) 0.3141(2) -0.0690(3) 0.0289(9) Uani 1 1 d . . .
C17 C 0.5702(3) 0.2878(2) 0.1567(2) 0.0275(9) Uani 1 1 d . . .
C18 C 0.4894(3) 0.30034(18) 0.2081(2) 0.0223(8) Uani 1 1 d . . .
C19 C 0.5144(3) 0.2916(2) 0.2900(2) 0.0274(9) Uani 1 1 d . . .
H19 H 0.5783 0.2751 0.3116 0.033 Uiso 1 1 calc R . .
C20 C 0.4457(3) 0.19292(18) -0.1591(2) 0.0242(9) Uani 1 1 d . . .
C21 C 0.3487(3) 0.17104(19) -0.1923(2) 0.0252(9) Uani 1 1 d . . .
H21 H 0.3015 0.1605 -0.1593 0.030 Uiso 1 1 calc R . .
C22 C 0.3227(3) 0.33498(18) 0.2253(2) 0.0238(8) Uani 1 1 d . . .
C23 C 0.3926(3) 0.32218(18) 0.1728(2) 0.0223(8) Uani 1 1 d . . .
C24 C 0.3648(3) 0.32483(19) 0.0835(2) 0.0233(8) Uani 1 1 d . . .
C25 C 0.4012(3) 0.1315(2) 0.5347(3) 0.0283(9) Uani 1 1 d . . .
C26 C 0.3726(4) 0.1303(2) 0.4531(2) 0.0304(10) Uani 1 1 d . . .
H26 H 0.3984 0.1009 0.4233 0.036 Uiso 1 1 calc R . .
C27 C 0.3048(3) 0.17279(19) 0.4147(2) 0.0246(9) Uani 1 1 d . . .
C28 C 0.2694(3) 0.28288(19) -0.0397(2) 0.0241(8) Uani 1 1 d . . .
H28 H 0.2239 0.2542 -0.0648 0.029 Uiso 1 1 calc R . .
C29 C 0.3008(3) 0.28096(18) 0.0427(2) 0.0224(8) Uani 1 1 d . . .
C30 C 0.2605(3) 0.23145(18) 0.0893(2) 0.0208(8) Uani 1 1 d . . .
C31 C 0.4807(3) 0.1980(2) -0.0701(3) 0.0301(10) Uani 1 1 d . . .
C32 C 0.2635(3) 0.1688(2) 0.3261(2) 0.0269(9) Uani 1 1 d . . .
Cd1 Cd 0.48088(2) 0.154030(14) 0.104540(17) 0.02385(10) Uani 1 1 d . . .
Cd2 Cd 0.16613(2) 0.146487(13) 0.171284(16) 0.01999(9) Uani 1 1 d . . .
Cd3 Cd 0.69401(2) 0.248146(13) 0.047196(17) 0.02279(9) Uani 1 1 d . . .
N1 N 0.9673(4) -0.0297(2) 0.2445(2) 0.0434(11) Uani 1 1 d . . .
N2 N -0.3352(3) 0.01545(17) 0.2514(2) 0.0328(9) Uani 1 1 d . . .
N3 N 0.4701(4) 0.0836(2) 0.5714(3) 0.0479(12) Uani 1 1 d . . .
N4 N 0.2175(3) 0.3589(2) 0.1949(2) 0.0392(10) Uani 1 1 d . . .
O1 O 0.7511(3) 0.15436(15) 0.0497(2) 0.0438(9) Uani 1 1 d . . .
O2 O 0.6346(2) 0.10485(15) 0.1057(2) 0.0413(8) Uani 1 1 d . . .
O3 O 0.9390(3) -0.01663(17) 0.3075(2) 0.0507(10) Uani 1 1 d . . .
O4 O 1.0473(4) -0.0591(2) 0.2416(3) 0.0743(15) Uani 1 1 d . . .
O5 O 0.0720(3) 0.10553(17) 0.0405(2) 0.0485(10) Uani 1 1 d . . .
O6 O 0.2094(2) 0.06079(15) 0.10478(19) 0.0373(8) Uani 1 1 d . . .
O7 O -0.0184(2) 0.18019(16) 0.1815(2) 0.0386(8) Uani 1 1 d . . .
O8 O 0.0490(2) 0.09645(16) 0.2347(2) 0.0379(8) Uani 1 1 d . . .
O9 O -0.3036(3) -0.02942(15) 0.2219(2) 0.0485(9) Uani 1 1 d . . .
O10 O -0.4263(3) 0.02362(16) 0.2583(2) 0.0478(9) Uani 1 1 d . . .
O11 O 0.7156(3) 0.33645(15) -0.0179(2) 0.0408(8) Uani 1 1 d . . .
O12 O 0.7914(3) 0.26202(15) -0.0660(2) 0.0416(9) Uani 1 1 d . . .
O13 O 0.5835(3) 0.23406(16) 0.1376(2) 0.0431(9) Uani 1 1 d . . .
O14 O 0.6192(3) 0.32780(18) 0.1335(3) 0.0596(11) Uani 1 1 d . . .
O15 O 0.2014(3) 0.3821(2) 0.1292(2) 0.0652(13) Uani 1 1 d . . .
O16 O 0.1524(3) 0.35388(19) 0.2369(3) 0.0573(11) Uani 1 1 d . . .
O17 O 0.4347(3) 0.16735(18) -0.02655(19) 0.0467(9) Uani 1 1 d . . .
O18 O 0.5536(3) 0.2330(2) -0.0470(2) 0.0603(12) Uani 1 1 d . . .
O19 O 0.3210(2) 0.19253(14) 0.12226(18) 0.0311(7) Uani 1 1 d . . .
O20 O 0.1658(2) 0.23099(16) 0.0925(2) 0.0385(8) Uani 1 1 d . . .
O21 O 0.4632(4) 0.0672(2) 0.6385(2) 0.0732(14) Uani 1 1 d . . .
O22 O 0.5286(4) 0.0619(2) 0.5317(3) 0.0707(13) Uani 1 1 d . . .
O23 O 0.1976(3) 0.20498(15) 0.29463(18) 0.0372(8) Uani 1 1 d . . .
O24 O 0.2954(2) 0.12664(15) 0.28603(17) 0.0321(7) Uani 1 1 d . . .
O1W O 0.4107(3) 0.06131(16) 0.0823(3) 0.0549(11) Uani 1 1 d . . .
O2W O 0.4881(3) 0.13930(18) 0.2406(2) 0.0453(9) Uani 1 1 d . . .
O3W O 0.8354(3) 0.2662(2) 0.1503(3) 0.0612(12) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.241(5) . ?
C1 O2 1.247(5) . ?
C1 C2 1.506(6) . ?
C2 C7 1.403(6) . ?
C2 C3 1.415(5) . ?
C3 C4 1.369(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.401(6) . ?
C4 C15 1.501(5) 3_655 ?
C5 C6 1.388(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.378(6) . ?
C6 N1 1.465(6) . ?
C7 C8 1.501(5) 1_655 ?
C8 C9 1.389(6) . ?
C8 C13 1.418(6) . ?
C8 C7 1.501(5) 1_455 ?
C9 C10 1.388(5) . ?
C9 N2 1.463(5) . ?
C10 C11 1.378(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.375(6) . ?
C11 C16 1.505(5) 4_466 ?
C12 C13 1.398(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.502(6) . ?
C14 O8 1.238(5) . ?
C14 O7 1.264(6) . ?
C14 Cd2 2.758(4) . ?
C15 O5 1.220(5) . ?
C15 O6 1.263(5) . ?
C15 C4 1.501(5) 3_655 ?
C16 O12 1.231(6) . ?
C16 O11 1.248(5) . ?
C16 C11 1.505(5) 4_665 ?
C16 Cd3 2.732(4) . ?
C17 O14 1.210(6) . ?
C17 O13 1.273(6) . ?
C17 C18 1.504(5) . ?
C18 C19 1.380(6) . ?
C18 C23 1.393(6) . ?
C19 C20 1.390(6) 4_566 ?
C19 H19 0.9300 . ?
C20 C21 1.386(6) . ?
C20 C19 1.390(6) 4_565 ?
C20 C31 1.500(6) . ?
C21 C22 1.383(6) 4_565 ?
C21 H21 0.9300 . ?
C22 C21 1.383(6) 4_566 ?
C22 C23 1.408(6) . ?
C22 N4 1.483(6) . ?
C23 C24 1.491(5) . ?
C24 C29 1.398(6) . ?
C24 C25 1.418(6) 4_565 ?
C25 C26 1.364(6) . ?
C25 C24 1.418(6) 4_566 ?
C25 N3 1.472(6) . ?
C26 C27 1.389(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.389(6) 4_566 ?
C27 C32 1.504(6) . ?
C28 C29 1.382(6) . ?
C28 C27 1.389(6) 4_565 ?
C28 H28 0.9300 . ?
C29 C30 1.511(6) . ?
C30 O19 1.246(5) . ?
C30 O20 1.249(5) . ?
C31 O17 1.238(6) . ?
C31 O18 1.246(6) . ?
C32 O23 1.238(5) . ?
C32 O24 1.276(5) . ?
C32 Cd2 2.751(4) . ?
Cd1 O17 2.213(3) . ?
Cd1 O13 2.260(3) . ?
Cd1 O1W 2.287(4) . ?
Cd1 O2 2.291(3) . ?
Cd1 O2W 2.308(3) . ?
Cd1 O19 2.330(3) . ?
Cd2 O8 2.308(3) . ?
Cd2 O20 2.323(3) . ?
Cd2 O6 2.352(3) . ?
Cd2 O24 2.384(3) . ?
Cd2 O23 2.440(3) . ?
Cd2 O5 2.512(3) . ?
Cd2 O19 2.537(3) . ?
Cd2 O7 2.564(3) . ?
Cd3 O18 2.239(4) . ?
Cd3 O1 2.239(3) . ?
Cd3 O13 2.298(3) . ?
Cd3 O11 2.314(3) . ?
Cd3 O3W 2.347(4) . ?
Cd3 O12 2.493(3) . ?
Cd3 O14 2.607(4) . ?
N1 O3 1.221(5) . ?
N1 O4 1.246(6) . ?
N2 O9 1.229(5) . ?
N2 O10 1.230(5) . ?
N3 O22 1.205(6) . ?
N3 O21 1.211(6) . ?
N4 O16 1.203(6) . ?
N4 O15 1.213(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 127.0(4) . . ?
O1 C1 C2 117.2(4) . . ?
O2 C1 C2 115.8(4) . . ?
C7 C2 C3 119.4(4) . . ?
C7 C2 C1 121.7(3) . . ?
C3 C2 C1 119.0(4) . . ?
C4 C3 C2 121.2(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 119.6(4) . . ?
C3 C4 C15 121.8(4) . 3_655 ?
C5 C4 C15 118.6(4) . 3_655 ?
C6 C5 C4 118.3(4) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
C7 C6 C5 123.4(4) . . ?
C7 C6 N1 120.4(4) . . ?
C5 C6 N1 116.2(4) . . ?
C6 C7 C2 117.7(4) . . ?
C6 C7 C8 125.0(4) . 1_655 ?
C2 C7 C8 117.3(4) . 1_655 ?
C9 C8 C13 116.4(3) . . ?
C9 C8 C7 123.9(4) . 1_455 ?
C13 C8 C7 119.4(4) . 1_455 ?
C10 C9 C8 123.1(4) . . ?
C10 C9 N2 117.4(4) . . ?
C8 C9 N2 119.5(4) . . ?
C11 C10 C9 119.2(4) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C12 C11 C10 120.0(4) . . ?
C12 C11 C16 120.3(4) . 4_466 ?
C10 C11 C16 119.6(4) . 4_466 ?
C11 C12 C13 120.7(4) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C8 120.4(4) . . ?
C12 C13 C14 120.7(4) . . ?
C8 C13 C14 118.9(3) . . ?
O8 C14 O7 123.8(4) . . ?
O8 C14 C13 117.3(4) . . ?
O7 C14 C13 118.9(4) . . ?
O8 C14 Cd2 56.1(2) . . ?
O7 C14 Cd2 67.8(2) . . ?
C13 C14 Cd2 171.8(3) . . ?
O5 C15 O6 122.7(4) . . ?
O5 C15 C4 119.6(4) . 3_655 ?
O6 C15 C4 117.6(4) . 3_655 ?
O12 C16 O11 122.7(4) . . ?
O12 C16 C11 119.9(4) . 4_665 ?
O11 C16 C11 117.4(4) . 4_665 ?
O12 C16 Cd3 65.7(2) . . ?
O11 C16 Cd3 57.5(2) . . ?
C11 C16 Cd3 171.5(3) 4_665 . ?
O14 C17 O13 121.6(4) . . ?
O14 C17 C18 120.7(4) . . ?
O13 C17 C18 117.7(4) . . ?
C19 C18 C23 121.3(4) . . ?
C19 C18 C17 118.9(4) . . ?
C23 C18 C17 119.7(3) . . ?
C18 C19 C20 121.2(4) . 4_566 ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 4_566 . ?
C21 C20 C19 118.9(4) . 4_565 ?
C21 C20 C31 122.2(4) . . ?
C19 C20 C31 118.9(4) 4_565 . ?
C22 C21 C20 119.4(4) 4_565 . ?
C22 C21 H21 120.3 4_565 . ?
C20 C21 H21 120.3 . . ?
C21 C22 C23 122.7(4) 4_566 . ?
C21 C22 N4 115.9(4) 4_566 . ?
C23 C22 N4 121.3(4) . . ?
C18 C23 C22 116.3(3) . . ?
C18 C23 C24 119.5(4) . . ?
C22 C23 C24 123.9(4) . . ?
C29 C24 C25 115.9(4) . 4_565 ?
C29 C24 C23 119.4(4) . . ?
C25 C24 C23 124.7(4) 4_565 . ?
C26 C25 C24 122.7(4) . 4_566 ?
C26 C25 N3 116.9(4) . . ?
C24 C25 N3 120.4(4) 4_566 . ?
C25 C26 C27 120.0(4) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C28 118.9(4) . 4_566 ?
C26 C27 C32 121.0(4) . . ?
C28 C27 C32 120.0(4) 4_566 . ?
C29 C28 C27 120.8(4) . 4_565 ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 4_565 . ?
C28 C29 C24 121.5(4) . . ?
C28 C29 C30 118.5(4) . . ?
C24 C29 C30 119.9(3) . . ?
O19 C30 O20 122.1(4) . . ?
O19 C30 C29 120.1(4) . . ?
O20 C30 C29 117.7(3) . . ?
O17 C31 O18 126.3(4) . . ?
O17 C31 C20 117.2(4) . . ?
O18 C31 C20 116.6(4) . . ?
O23 C32 O24 121.9(4) . . ?
O23 C32 C27 119.4(4) . . ?
O24 C32 C27 118.6(4) . . ?
O23 C32 Cd2 62.5(2) . . ?
O24 C32 Cd2 60.0(2) . . ?
C27 C32 Cd2 170.2(3) . . ?
O17 Cd1 O13 100.81(14) . . ?
O17 Cd1 O1W 85.80(15) . . ?
O13 Cd1 O1W 166.92(14) . . ?
O17 Cd1 O2 99.33(14) . . ?
O13 Cd1 O2 84.36(13) . . ?
O1W Cd1 O2 83.44(13) . . ?
O17 Cd1 O2W 166.71(13) . . ?
O13 Cd1 O2W 86.99(14) . . ?
O1W Cd1 O2W 88.79(15) . . ?
O2 Cd1 O2W 92.08(13) . . ?
O17 Cd1 O19 88.95(13) . . ?
O13 Cd1 O19 100.28(12) . . ?
O1W Cd1 O19 91.04(12) . . ?
O2 Cd1 O19 169.65(11) . . ?
O2W Cd1 O19 79.02(11) . . ?
O8 Cd2 O20 136.93(12) . . ?
O8 Cd2 O6 93.09(12) . . ?
O20 Cd2 O6 112.10(13) . . ?
O8 Cd2 O24 87.98(11) . . ?
O20 Cd2 O24 123.42(12) . . ?
O6 Cd2 O24 92.26(11) . . ?
O8 Cd2 O23 83.99(12) . . ?
O20 Cd2 O23 91.72(12) . . ?
O6 Cd2 O23 146.36(11) . . ?
O24 Cd2 O23 54.21(11) . . ?
O8 Cd2 O5 88.01(13) . . ?
O20 Cd2 O5 81.07(13) . . ?
O6 Cd2 O5 53.11(11) . . ?
O24 Cd2 O5 144.83(11) . . ?
O23 Cd2 O5 159.17(11) . . ?
O8 Cd2 O19 168.95(11) . . ?
O20 Cd2 O19 53.17(10) . . ?
O6 Cd2 O19 84.78(11) . . ?
O24 Cd2 O19 81.29(10) . . ?
O23 Cd2 O19 91.77(11) . . ?
O5 Cd2 O19 99.25(12) . . ?
O8 Cd2 O7 53.58(11) . . ?
O20 Cd2 O7 83.51(11) . . ?
O6 Cd2 O7 125.59(11) . . ?
O24 Cd2 O7 122.96(10) . . ?
O23 Cd2 O7 78.74(11) . . ?
O5 Cd2 O7 81.03(11) . . ?
O19 Cd2 O7 135.56(11) . . ?
O8 Cd2 C32 83.29(12) . . ?
O20 Cd2 C32 110.50(13) . . ?
O6 Cd2 C32 119.61(13) . . ?
O24 Cd2 C32 27.62(12) . . ?
O23 Cd2 C32 26.75(12) . . ?
O5 Cd2 C32 168.43(13) . . ?
O19 Cd2 C32 88.33(11) . . ?
O7 Cd2 C32 99.71(12) . . ?
O8 Cd2 C14 26.43(13) . . ?
O20 Cd2 C14 110.67(13) . . ?
O6 Cd2 C14 111.36(12) . . ?
O24 Cd2 C14 105.61(12) . . ?
O23 Cd2 C14 79.43(12) . . ?
O5 Cd2 C14 84.85(12) . . ?
O19 Cd2 C14 161.76(12) . . ?
O7 Cd2 C14 27.18(12) . . ?
C32 Cd2 C14 90.66(12) . . ?
O18 Cd3 O1 95.73(17) . . ?
O18 Cd3 O13 85.37(14) . . ?
O1 Cd3 O13 95.89(13) . . ?
O18 Cd3 O11 86.86(15) . . ?
O1 Cd3 O11 138.86(12) . . ?
O13 Cd3 O11 125.21(13) . . ?
O18 Cd3 O3W 176.92(16) . . ?
O1 Cd3 O3W 86.14(16) . . ?
O13 Cd3 O3W 92.01(15) . . ?
O11 Cd3 O3W 93.34(15) . . ?
O18 Cd3 O12 86.45(14) . . ?
O1 Cd3 O12 85.43(12) . . ?
O13 Cd3 O12 171.80(13) . . ?
O11 Cd3 O12 53.67(11) . . ?
O3W Cd3 O12 96.15(15) . . ?
O18 Cd3 O14 99.30(17) . . ?
O1 Cd3 O14 142.68(13) . . ?
O13 Cd3 O14 51.98(12) . . ?
O11 Cd3 O14 76.21(12) . . ?
O3W Cd3 O14 77.78(16) . . ?
O12 Cd3 O14 129.28(12) . . ?
O18 Cd3 C16 84.35(14) . . ?
O1 Cd3 C16 112.17(13) . . ?
O13 Cd3 C16 150.89(14) . . ?
O11 Cd3 C16 27.05(13) . . ?
O3W Cd3 C16 97.23(15) . . ?
O12 Cd3 C16 26.75(12) . . ?
O14 Cd3 C16 103.19(13) . . ?
O3 N1 O4 123.1(4) . . ?
O3 N1 C6 119.5(4) . . ?
O4 N1 C6 117.5(4) . . ?
O9 N2 O10 124.0(4) . . ?
O9 N2 C9 118.5(4) . . ?
O10 N2 C9 117.4(4) . . ?
O22 N3 O21 123.7(5) . . ?
O22 N3 C25 117.6(4) . . ?
O21 N3 C25 118.7(5) . . ?
O16 N4 O15 123.5(4) . . ?
O16 N4 C22 118.0(4) . . ?
O15 N4 C22 118.5(4) . . ?
C1 O1 Cd3 129.4(3) . . ?
C1 O2 Cd1 140.8(3) . . ?
C15 O5 Cd2 88.7(3) . . ?
C15 O6 Cd2 95.2(3) . . ?
C14 O7 Cd2 85.0(3) . . ?
C14 O8 Cd2 97.5(3) . . ?
C16 O11 Cd3 95.5(3) . . ?
C16 O12 Cd3 87.5(3) . . ?
C17 O13 Cd1 136.1(3) . . ?
C17 O13 Cd3 99.5(3) . . ?
Cd1 O13 Cd3 111.10(13) . . ?
C17 O14 Cd3 86.5(3) . . ?
C31 O17 Cd1 126.3(3) . . ?
C31 O18 Cd3 143.8(4) . . ?
C30 O19 Cd1 135.9(3) . . ?
C30 O19 Cd2 87.3(2) . . ?
Cd1 O19 Cd2 132.34(13) . . ?
C30 O20 Cd2 97.3(3) . . ?
C32 O23 Cd2 90.8(3) . . ?
C32 O24 Cd2 92.4(3) . . ?

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
O1 C1 C2 C7 107.8(5) . . . . ?
O2 C1 C2 C7 -71.0(5) . . . . ?
O1 C1 C2 C3 -72.1(5) . . . . ?
O2 C1 C2 C3 109.1(5) . . . . ?
C7 C2 C3 C4 1.8(6) . . . . ?
C1 C2 C3 C4 -178.3(4) . . . . ?
C2 C3 C4 C5 -6.8(7) . . . . ?
C2 C3 C4 C15 171.8(4) . . . 3_655 ?
C3 C4 C5 C6 6.3(7) . . . . ?
C15 C4 C5 C6 -172.3(4) 3_655 . . . ?
C4 C5 C6 C7 -0.9(8) . . . . ?
C4 C5 C6 N1 179.2(4) . . . . ?
C5 C6 C7 C2 -4.0(7) . . . . ?
N1 C6 C7 C2 175.9(4) . . . . ?
C5 C6 C7 C8 178.1(4) . . . 1_655 ?
N1 C6 C7 C8 -1.9(7) . . . 1_655 ?
C3 C2 C7 C6 3.6(6) . . . . ?
C1 C2 C7 C6 -176.3(4) . . . . ?
C3 C2 C7 C8 -178.4(4) . . . 1_655 ?
C1 C2 C7 C8 1.7(6) . . . 1_655 ?
C13 C8 C9 C10 -2.8(6) . . . . ?
C7 C8 C9 C10 -176.0(4) 1_455 . . . ?
C13 C8 C9 N2 174.8(4) . . . . ?
C7 C8 C9 N2 1.6(6) 1_455 . . . ?
C8 C9 C10 C11 2.0(7) . . . . ?
N2 C9 C10 C11 -175.7(4) . . . . ?
C9 C10 C11 C12 2.2(7) . . . . ?
C9 C10 C11 C16 178.6(4) . . . 4_466 ?
C10 C11 C12 C13 -5.4(7) . . . . ?
C16 C11 C12 C13 178.3(4) 4_466 . . . ?
C11 C12 C13 C8 4.5(7) . . . . ?
C11 C12 C13 C14 -173.1(4) . . . . ?
C9 C8 C13 C12 -0.4(6) . . . . ?
C7 C8 C13 C12 173.1(4) 1_455 . . . ?
C9 C8 C13 C14 177.2(4) . . . . ?
C7 C8 C13 C14 -9.3(6) 1_455 . . . ?
C12 C13 C14 O8 112.6(5) . . . . ?
C8 C13 C14 O8 -64.9(5) . . . . ?
C12 C13 C14 O7 -65.8(6) . . . . ?
C8 C13 C14 O7 116.6(5) . . . . ?
C12 C13 C14 Cd2 77(2) . . . . ?
C8 C13 C14 Cd2 -100(2) . . . . ?
O14 C17 C18 C19 -100.5(6) . . . . ?
O13 C17 C18 C19 80.6(5) . . . . ?
O14 C17 C18 C23 77.5(6) . . . . ?
O13 C17 C18 C23 -101.3(5) . . . . ?
C23 C18 C19 C20 -3.3(7) . . . 4_566 ?
C17 C18 C19 C20 174.7(4) . . . 4_566 ?
C19 C20 C21 C22 0.1(6) 4_565 . . 4_565 ?
C31 C20 C21 C22 -177.2(4) . . . 4_565 ?
C19 C18 C23 C22 0.4(6) . . . . ?
C17 C18 C23 C22 -177.6(4) . . . . ?
C19 C18 C23 C24 -173.5(4) . . . . ?
C17 C18 C23 C24 8.5(6) . . . . ?
C21 C22 C23 C18 2.7(6) 4_566 . . . ?
N4 C22 C23 C18 179.5(4) . . . . ?
C21 C22 C23 C24 176.3(4) 4_566 . . . ?
N4 C22 C23 C24 -6.9(6) . . . . ?
C18 C23 C24 C29 100.8(5) . . . . ?
C22 C23 C24 C29 -72.5(6) . . . . ?
C18 C23 C24 C25 -77.3(6) . . . 4_565 ?
C22 C23 C24 C25 109.3(5) . . . 4_565 ?
C24 C25 C26 C27 -0.2(7) 4_566 . . . ?
N3 C25 C26 C27 177.7(4) . . . . ?
C25 C26 C27 C28 1.7(7) . . . 4_566 ?
C25 C26 C27 C32 -173.7(4) . . . . ?
C27 C28 C29 C24 3.2(6) 4_565 . . . ?
C27 C28 C29 C30 -179.5(4) 4_565 . . . ?
C25 C24 C29 C28 -4.5(6) 4_565 . . . ?
C23 C24 C29 C28 177.2(4) . . . . ?
C25 C24 C29 C30 178.2(4) 4_565 . . . ?
C23 C24 C29 C30 -0.1(6) . . . . ?
C28 C29 C30 O19 112.3(5) . . . . ?
C24 C29 C30 O19 -70.3(5) . . . . ?
C28 C29 C30 O20 -67.0(5) . . . . ?
C24 C29 C30 O20 110.3(5) . . . . ?
C21 C20 C31 O17 20.1(7) . . . . ?
C19 C20 C31 O17 -157.3(4) 4_565 . . . ?
C21 C20 C31 O18 -159.8(5) . . . . ?
C19 C20 C31 O18 22.9(6) 4_565 . . . ?
C26 C27 C32 O23 174.9(4) . . . . ?
C28 C27 C32 O23 -0.4(6) 4_566 . . . ?
C26 C27 C32 O24 -2.8(6) . . . . ?
C28 C27 C32 O24 -178.1(4) 4_566 . . . ?
C26 C27 C32 Cd2 76(2) . . . . ?
C28 C27 C32 Cd2 -99.0(19) 4_566 . . . ?
O23 C32 Cd2 O8 -90.0(3) . . . . ?
O24 C32 Cd2 O8 98.5(3) . . . . ?
C27 C32 Cd2 O8 13.8(19) . . . . ?
O23 C32 Cd2 O20 47.9(3) . . . . ?
O24 C32 Cd2 O20 -123.6(2) . . . . ?
C27 C32 Cd2 O20 151.7(19) . . . . ?
O23 C32 Cd2 O6 -179.7(2) . . . . ?
O24 C32 Cd2 O6 8.8(3) . . . . ?
C27 C32 Cd2 O6 -75.9(19) . . . . ?
O23 C32 Cd2 O24 171.5(4) . . . . ?
C27 C32 Cd2 O24 -84.7(19) . . . . ?
O24 C32 Cd2 O23 -171.5(4) . . . . ?
C27 C32 Cd2 O23 103.8(19) . . . . ?
O23 C32 Cd2 O5 -131.5(6) . . . . ?
O24 C32 Cd2 O5 57.0(7) . . . . ?
C27 C32 Cd2 O5 -28(2) . . . . ?
O23 C32 Cd2 O19 97.3(3) . . . . ?
O24 C32 Cd2 O19 -74.3(2) . . . . ?
C27 C32 Cd2 O19 -158.9(19) . . . . ?
O23 C32 Cd2 O7 -38.8(3) . . . . ?
O24 C32 Cd2 O7 149.7(2) . . . . ?
C27 C32 Cd2 O7 65.0(19) . . . . ?
O23 C32 Cd2 C14 -64.5(3) . . . . ?
O24 C32 Cd2 C14 124.0(3) . . . . ?
C27 C32 Cd2 C14 39.3(19) . . . . ?
O7 C14 Cd2 O8 -176.3(4) . . . . ?
C13 C14 Cd2 O8 38(2) . . . . ?
O8 C14 Cd2 O20 174.3(3) . . . . ?
O7 C14 Cd2 O20 -1.9(3) . . . . ?
C13 C14 Cd2 O20 -147(2) . . . . ?
O8 C14 Cd2 O6 48.9(3) . . . . ?
O7 C14 Cd2 O6 -127.3(2) . . . . ?
C13 C14 Cd2 O6 87(2) . . . . ?
O8 C14 Cd2 O24 -49.9(3) . . . . ?
O7 C14 Cd2 O24 133.8(2) . . . . ?
C13 C14 Cd2 O24 -12(2) . . . . ?
O8 C14 Cd2 O23 -97.8(3) . . . . ?
O7 C14 Cd2 O23 85.9(3) . . . . ?
C13 C14 Cd2 O23 -60(2) . . . . ?
O8 C14 Cd2 O5 95.9(3) . . . . ?
O7 C14 Cd2 O5 -80.4(3) . . . . ?
C13 C14 Cd2 O5 134(2) . . . . ?
O8 C14 Cd2 O19 -160.1(3) . . . . ?
O7 C14 Cd2 O19 23.6(5) . . . . ?
C13 C14 Cd2 O19 -122(2) . . . . ?
O8 C14 Cd2 O7 176.3(4) . . . . ?
C13 C14 Cd2 O7 -145(2) . . . . ?
O8 C14 Cd2 C32 -73.4(3) . . . . ?
O7 C14 Cd2 C32 110.3(3) . . . . ?
C13 C14 Cd2 C32 -35(2) . . . . ?
O12 C16 Cd3 O18 -93.3(3) . . . . ?
O11 C16 Cd3 O18 94.2(3) . . . . ?
C11 C16 Cd3 O18 40(2) 4_665 . . . ?
O12 C16 Cd3 O1 0.6(3) . . . . ?
O11 C16 Cd3 O1 -171.9(3) . . . . ?
C11 C16 Cd3 O1 134(2) 4_665 . . . ?
O12 C16 Cd3 O13 -163.2(3) . . . . ?
O11 C16 Cd3 O13 24.3(4) . . . . ?
C11 C16 Cd3 O13 -30(2) 4_665 . . . ?
O12 C16 Cd3 O11 172.5(5) . . . . ?
C11 C16 Cd3 O11 -55(2) 4_665 . . . ?
O12 C16 Cd3 O3W 89.3(3) . . . . ?
O11 C16 Cd3 O3W -83.2(3) . . . . ?
C11 C16 Cd3 O3W -138(2) 4_665 . . . ?
O11 C16 Cd3 O12 -172.5(5) . . . . ?
C11 C16 Cd3 O12 133(2) 4_665 . . . ?
O12 C16 Cd3 O14 168.4(3) . . . . ?
O11 C16 Cd3 O14 -4.1(3) . . . . ?
C11 C16 Cd3 O14 -59(2) 4_665 . . . ?
C7 C6 N1 O3 22.8(7) . . . . ?
C5 C6 N1 O3 -157.3(5) . . . . ?
C7 C6 N1 O4 -157.5(5) . . . . ?
C5 C6 N1 O4 22.4(8) . . . . ?
C10 C9 N2 O9 -150.8(4) . . . . ?
C8 C9 N2 O9 31.5(6) . . . . ?
C10 C9 N2 O10 31.3(6) . . . . ?
C8 C9 N2 O10 -146.4(4) . . . . ?
C26 C25 N3 O22 29.2(7) . . . . ?
C24 C25 N3 O22 -152.9(5) 4_566 . . . ?
C26 C25 N3 O21 -149.0(5) . . . . ?
C24 C25 N3 O21 29.0(7) 4_566 . . . ?
C21 C22 N4 O16 -22.8(6) 4_566 . . . ?
C23 C22 N4 O16 160.1(4) . . . . ?
C21 C22 N4 O15 157.5(5) 4_566 . . . ?
C23 C22 N4 O15 -19.6(7) . . . . ?
O2 C1 O1 Cd3 13.0(7) . . . . ?
C2 C1 O1 Cd3 -165.7(3) . . . . ?
O18 Cd3 O1 C1 -75.7(4) . . . . ?
O13 Cd3 O1 C1 10.2(4) . . . . ?
O11 Cd3 O1 C1 -167.5(4) . . . . ?
O3W Cd3 O1 C1 101.8(4) . . . . ?
O12 Cd3 O1 C1 -161.7(4) . . . . ?
O14 Cd3 O1 C1 37.8(5) . . . . ?
C16 Cd3 O1 C1 -161.9(4) . . . . ?
O1 C1 O2 Cd1 11.0(8) . . . . ?
C2 C1 O2 Cd1 -170.3(3) . . . . ?
O17 Cd1 O2 C1 52.9(5) . . . . ?
O13 Cd1 O2 C1 -47.2(5) . . . . ?
O1W Cd1 O2 C1 137.5(5) . . . . ?
O2W Cd1 O2 C1 -133.9(5) . . . . ?
O19 Cd1 O2 C1 -164.4(6) . . . . ?
O6 C15 O5 Cd2 5.5(5) . . . . ?
C4 C15 O5 Cd2 -170.4(4) 3_655 . . . ?
O8 Cd2 O5 C15 -98.5(3) . . . . ?
O20 Cd2 O5 C15 123.3(3) . . . . ?
O6 Cd2 O5 C15 -3.1(3) . . . . ?
O24 Cd2 O5 C15 -14.8(4) . . . . ?
O23 Cd2 O5 C15 -165.8(3) . . . . ?
O19 Cd2 O5 C15 73.2(3) . . . . ?
O7 Cd2 O5 C15 -151.9(3) . . . . ?
C32 Cd2 O5 C15 -57.3(7) . . . . ?
C14 Cd2 O5 C15 -124.8(3) . . . . ?
O5 C15 O6 Cd2 -5.9(5) . . . . ?
C4 C15 O6 Cd2 170.1(3) 3_655 . . . ?
O8 Cd2 O6 C15 88.2(3) . . . . ?
O20 Cd2 O6 C15 -56.0(3) . . . . ?
O24 Cd2 O6 C15 176.3(3) . . . . ?
O23 Cd2 O6 C15 172.0(2) . . . . ?
O5 Cd2 O6 C15 3.0(3) . . . . ?
O19 Cd2 O6 C15 -102.7(3) . . . . ?
O7 Cd2 O6 C15 42.0(3) . . . . ?
C32 Cd2 O6 C15 172.2(2) . . . . ?
C14 Cd2 O6 C15 68.6(3) . . . . ?
O8 C14 O7 Cd2 -3.7(4) . . . . ?
C13 C14 O7 Cd2 174.7(3) . . . . ?
O8 Cd2 O7 C14 2.1(2) . . . . ?
O20 Cd2 O7 C14 178.2(3) . . . . ?
O6 Cd2 O7 C14 65.6(3) . . . . ?
O24 Cd2 O7 C14 -55.9(3) . . . . ?
O23 Cd2 O7 C14 -88.8(3) . . . . ?
O5 Cd2 O7 C14 96.2(3) . . . . ?
O19 Cd2 O7 C14 -169.7(2) . . . . ?
C32 Cd2 O7 C14 -72.1(3) . . . . ?
O7 C14 O8 Cd2 4.1(5) . . . . ?
C13 C14 O8 Cd2 -174.3(3) . . . . ?
O20 Cd2 O8 C14 -7.8(3) . . . . ?
O6 Cd2 O8 C14 -135.3(3) . . . . ?
O24 Cd2 O8 C14 132.5(3) . . . . ?
O23 Cd2 O8 C14 78.3(3) . . . . ?
O5 Cd2 O8 C14 -82.4(3) . . . . ?
O19 Cd2 O8 C14 146.2(5) . . . . ?
O7 Cd2 O8 C14 -2.1(2) . . . . ?
C32 Cd2 O8 C14 105.2(3) . . . . ?
O12 C16 O11 Cd3 -8.1(5) . . . . ?
C11 C16 O11 Cd3 172.2(3) 4_665 . . . ?
O18 Cd3 O11 C16 -83.7(3) . . . . ?
O1 Cd3 O11 C16 11.4(4) . . . . ?
O13 Cd3 O11 C16 -165.8(3) . . . . ?
O3W Cd3 O11 C16 99.4(3) . . . . ?
O12 Cd3 O11 C16 4.2(3) . . . . ?
O14 Cd3 O11 C16 175.9(3) . . . . ?
O11 C16 O12 Cd3 7.5(5) . . . . ?
C11 C16 O12 Cd3 -172.8(4) 4_665 . . . ?
O18 Cd3 O12 C16 84.5(3) . . . . ?
O1 Cd3 O12 C16 -179.5(3) . . . . ?
O13 Cd3 O12 C16 80.9(9) . . . . ?
O11 Cd3 O12 C16 -4.2(3) . . . . ?
O3W Cd3 O12 C16 -93.9(3) . . . . ?
O14 Cd3 O12 C16 -14.6(4) . . . . ?
O14 C17 O13 Cd1 -141.5(4) . . . . ?
C18 C17 O13 Cd1 37.3(6) . . . . ?
O14 C17 O13 Cd3 -6.9(5) . . . . ?
C18 C17 O13 Cd3 171.9(3) . . . . ?
O17 Cd1 O13 C17 86.9(5) . . . . ?
O1W Cd1 O13 C17 -153.6(6) . . . . ?
O2 Cd1 O13 C17 -174.6(5) . . . . ?
O2W Cd1 O13 C17 -82.3(5) . . . . ?
O19 Cd1 O13 C17 -4.0(5) . . . . ?
O17 Cd1 O13 Cd3 -44.21(19) . . . . ?
O1W Cd1 O13 Cd3 75.3(7) . . . . ?
O2 Cd1 O13 Cd3 54.24(17) . . . . ?
O2W Cd1 O13 Cd3 146.63(18) . . . . ?
O19 Cd1 O13 Cd3 -135.11(16) . . . . ?
O18 Cd3 O13 C17 -102.1(3) . . . . ?
O1 Cd3 O13 C17 162.6(3) . . . . ?
O11 Cd3 O13 C17 -19.3(3) . . . . ?
O3W Cd3 O13 C17 76.2(3) . . . . ?
O12 Cd3 O13 C17 -98.5(8) . . . . ?
O14 Cd3 O13 C17 3.5(3) . . . . ?
C16 Cd3 O13 C17 -32.5(4) . . . . ?
O18 Cd3 O13 Cd1 45.9(2) . . . . ?
O1 Cd3 O13 Cd1 -49.41(19) . . . . ?
O11 Cd3 O13 Cd1 128.74(16) . . . . ?
O3W Cd3 O13 Cd1 -135.74(19) . . . . ?
O12 Cd3 O13 Cd1 49.5(9) . . . . ?
O14 Cd3 O13 Cd1 151.5(3) . . . . ?
C16 Cd3 O13 Cd1 115.5(3) . . . . ?
O13 C17 O14 Cd3 6.0(5) . . . . ?
C18 C17 O14 Cd3 -172.7(4) . . . . ?
O18 Cd3 O14 C17 73.0(3) . . . . ?
O1 Cd3 O14 C17 -39.5(4) . . . . ?
O13 Cd3 O14 C17 -3.6(3) . . . . ?
O11 Cd3 O14 C17 157.4(3) . . . . ?
O3W Cd3 O14 C17 -106.0(3) . . . . ?
O12 Cd3 O14 C17 166.0(3) . . . . ?
C16 Cd3 O14 C17 159.3(3) . . . . ?
O18 C31 O17 Cd1 -9.9(8) . . . . ?
C20 C31 O17 Cd1 170.3(3) . . . . ?
O13 Cd1 O17 C31 21.0(4) . . . . ?
O1W Cd1 O17 C31 -147.6(4) . . . . ?
O2 Cd1 O17 C31 -65.0(4) . . . . ?
O2W Cd1 O17 C31 146.2(6) . . . . ?
O19 Cd1 O17 C31 121.3(4) . . . . ?
O17 C31 O18 Cd3 34.7(10) . . . . ?
C20 C31 O18 Cd3 -145.5(5) . . . . ?
O1 Cd3 O18 C31 41.8(7) . . . . ?
O13 Cd3 O18 C31 -53.7(6) . . . . ?
O11 Cd3 O18 C31 -179.4(7) . . . . ?
O3W Cd3 O18 C31 -86(3) . . . . ?
O12 Cd3 O18 C31 126.8(7) . . . . ?
O14 Cd3 O18 C31 -103.9(6) . . . . ?
C16 Cd3 O18 C31 153.6(7) . . . . ?
O20 C30 O19 Cd1 156.1(3) . . . . ?
C29 C30 O19 Cd1 -23.1(6) . . . . ?
O20 C30 O19 Cd2 -1.0(4) . . . . ?
C29 C30 O19 Cd2 179.7(3) . . . . ?
O17 Cd1 O19 C30 -34.6(4) . . . . ?
O13 Cd1 O19 C30 66.2(4) . . . . ?
O1W Cd1 O19 C30 -120.3(4) . . . . ?
O2 Cd1 O19 C30 -177.9(6) . . . . ?
O2W Cd1 O19 C30 151.1(4) . . . . ?
O17 Cd1 O19 Cd2 113.8(2) . . . . ?
O13 Cd1 O19 Cd2 -145.36(19) . . . . ?
O1W Cd1 O19 Cd2 28.1(2) . . . . ?
O2 Cd1 O19 Cd2 -29.5(8) . . . . ?
O2W Cd1 O19 Cd2 -60.50(19) . . . . ?
O8 Cd2 O19 C30 -157.4(5) . . . . ?
O20 Cd2 O19 C30 0.6(2) . . . . ?
O6 Cd2 O19 C30 123.3(2) . . . . ?
O24 Cd2 O19 C30 -143.6(3) . . . . ?
O23 Cd2 O19 C30 -90.2(2) . . . . ?
O5 Cd2 O19 C30 72.0(2) . . . . ?
O7 Cd2 O19 C30 -14.6(3) . . . . ?
C32 Cd2 O19 C30 -116.8(3) . . . . ?
C14 Cd2 O19 C30 -29.7(5) . . . . ?
O8 Cd2 O19 Cd1 44.0(7) . . . . ?
O20 Cd2 O19 Cd1 -158.0(3) . . . . ?
O6 Cd2 O19 Cd1 -35.30(18) . . . . ?
O24 Cd2 O19 Cd1 57.80(18) . . . . ?
O23 Cd2 O19 Cd1 111.17(19) . . . . ?
O5 Cd2 O19 Cd1 -86.58(19) . . . . ?
O7 Cd2 O19 Cd1 -173.16(14) . . . . ?
C32 Cd2 O19 Cd1 84.6(2) . . . . ?
C14 Cd2 O19 Cd1 171.7(3) . . . . ?
O19 C30 O20 Cd2 1.1(5) . . . . ?
C29 C30 O20 Cd2 -179.6(3) . . . . ?
O8 Cd2 O20 C30 173.4(2) . . . . ?
O6 Cd2 O20 C30 -65.3(3) . . . . ?
O24 Cd2 O20 C30 43.3(3) . . . . ?
O23 Cd2 O20 C30 90.3(3) . . . . ?
O5 Cd2 O20 C30 -109.3(3) . . . . ?
O19 Cd2 O20 C30 -0.6(2) . . . . ?
O7 Cd2 O20 C30 168.8(3) . . . . ?
C32 Cd2 O20 C30 70.8(3) . . . . ?
C14 Cd2 O20 C30 169.7(3) . . . . ?
O24 C32 O23 Cd2 8.7(4) . . . . ?
C27 C32 O23 Cd2 -169.0(3) . . . . ?
O8 Cd2 O23 C32 87.0(3) . . . . ?
O20 Cd2 O23 C32 -136.0(3) . . . . ?
O6 Cd2 O23 C32 0.5(4) . . . . ?
O24 Cd2 O23 C32 -4.8(2) . . . . ?
O5 Cd2 O23 C32 155.0(3) . . . . ?
O19 Cd2 O23 C32 -82.8(3) . . . . ?
O7 Cd2 O23 C32 141.0(3) . . . . ?
C14 Cd2 O23 C32 113.3(3) . . . . ?
O23 C32 O24 Cd2 -8.9(4) . . . . ?
C27 C32 O24 Cd2 168.8(3) . . . . ?
O8 Cd2 O24 C32 -79.4(3) . . . . ?
O20 Cd2 O24 C32 69.1(3) . . . . ?
O6 Cd2 O24 C32 -172.4(3) . . . . ?
O23 Cd2 O24 C32 4.7(2) . . . . ?
O5 Cd2 O24 C32 -163.0(3) . . . . ?
O19 Cd2 O24 C32 103.3(3) . . . . ?
O7 Cd2 O24 C32 -36.3(3) . . . . ?
C14 Cd2 O24 C32 -59.4(3) . . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.386 -0.105 1391 464 ' '
_platon_squeeze_details          
;
;
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.126
####################################################################### 
# 
# 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_6-sr
_database_code_depnum_ccdc_archive 'CCDC 1444253'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H13 Cd2 N5 O12'
_chemical_formula_weight         812.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P21/c   '

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

_cell_length_a                   7.520(7)
_cell_length_b                   15.850(15)
_cell_length_c                   22.80(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.031(17)
_cell_angle_gamma                90.00
_cell_volume                     2718(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2535
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      23.05

_exptl_crystal_description       columnar
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7565
_exptl_absorpt_correction_T_max  0.8530
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13263
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_sigmaI/netI    0.0991
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4786
_reflns_number_gt                3214
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

half of one water molecule was found disordered, and a SQUEEZE
procedure was applied on it. The result gave missing electron density 
accounting for 5 e per asymmetric 
unit,well consistent with the 5 demanded for half of one water molecule.


PLAT230_ALERT_2_B Hirshfeld Test Diff for    N1     --  C6      ..       13.3 su    
PLAT241_ALERT_2_B High      Ueq as Compared to Neighbors for .....         N2 Check
these are the nitro groups disorder.
 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0897P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4786
_refine_ls_number_parameters     416
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1652
_refine_ls_wR_factor_gt          0.1481
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O8 O 0.166(4) 0.9769(9) 0.0288(8) 0.050(7) Uani 0.50(5) 1 d PU A 1
O8' O 0.081(4) 0.9825(9) 0.0370(8) 0.050(7) Uani 0.50(5) 1 d PU A 2
C1 C 0.0830(11) 0.6394(5) 0.1056(4) 0.0326(19) Uani 1 1 d . . .
C2 C 0.2276(11) 0.6580(5) 0.0615(4) 0.0324(19) Uani 1 1 d . . .
C3 C 0.2633(11) 0.5953(5) 0.0179(4) 0.0314(19) Uani 1 1 d . . .
H3 H 0.1995 0.5451 0.0187 0.038 Uiso 1 1 calc R . .
C4 C 0.3861(11) 0.6067(5) -0.0243(4) 0.035(2) Uani 1 1 d . . .
C5 C 0.4880(12) 0.6812(6) -0.0243(4) 0.044(2) Uani 1 1 d . . .
H5 H 0.5791 0.6880 -0.0515 0.053 Uiso 1 1 calc R . .
C6 C 0.4532(13) 0.7438(5) 0.0156(4) 0.045(2) Uani 1 1 d . . .
C7 C 0.3197(11) 0.7341(5) 0.0602(4) 0.036(2) Uani 1 1 d . . .
C8 C 0.2975(11) 0.8000(5) 0.1078(4) 0.0338(19) Uani 1 1 d . . .
C9 C 0.2219(13) 0.8789(5) 0.0996(4) 0.041(2) Uani 1 1 d . A .
C10 C 0.2130(13) 0.9384(5) 0.1423(4) 0.041(2) Uani 1 1 d . . .
H10 H 0.1653 0.9913 0.1343 0.050 Uiso 1 1 calc R . .
C11 C 0.2766(11) 0.9192(5) 0.1985(4) 0.0331(19) Uani 1 1 d . . .
C12 C 0.3544(11) 0.8411(5) 0.2075(4) 0.036(2) Uani 1 1 d . . .
H12 H 0.3996 0.8280 0.2444 0.043 Uiso 1 1 calc R . .
C13 C 0.3663(11) 0.7821(5) 0.1631(4) 0.0312(18) Uani 1 1 d . . .
C14 C 0.4574(12) 0.6988(5) 0.1748(4) 0.035(2) Uani 1 1 d . . .
C15 C 0.4197(12) 0.5400(6) -0.0696(4) 0.038(2) Uani 1 1 d . . .
C16 C 0.2635(11) 0.9818(5) 0.2482(4) 0.033(2) Uani 1 1 d . . .
C17 C 0.0696(15) 0.3604(6) 0.1199(5) 0.059(3) Uani 1 1 d . . .
H17 H 0.0764 0.4020 0.0912 0.071 Uiso 1 1 calc R . .
C18 C 0.0044(18) 0.2854(7) 0.1040(6) 0.082(4) Uani 1 1 d . . .
H18 H -0.0357 0.2750 0.0660 0.099 Uiso 1 1 calc R . .
C19 C 0.000(3) 0.2240(9) 0.1471(10) 0.146(9) Uani 1 1 d . . .
H19 H -0.0289 0.1691 0.1365 0.176 Uiso 1 1 calc R . .
C20 C 0.038(2) 0.2417(8) 0.2080(9) 0.126(7) Uani 1 1 d . . .
H20 H 0.0163 0.2027 0.2376 0.152 Uiso 1 1 calc R . .
C21 C 0.1110(14) 0.3226(6) 0.2196(5) 0.057(3) Uani 1 1 d . . .
C22 C 0.2251(14) 0.4100(7) 0.3051(5) 0.052(3) Uani 1 1 d . . .
C23 C 0.2325(17) 0.4026(9) 0.3669(6) 0.080(4) Uani 1 1 d . . .
H23 H 0.2045 0.3512 0.3842 0.096 Uiso 1 1 calc R . .
C24 C 0.280(2) 0.4693(10) 0.4017(6) 0.090(4) Uani 1 1 d . . .
H24 H 0.2789 0.4660 0.4424 0.107 Uiso 1 1 calc R . .
C25 C 0.331(2) 0.5442(9) 0.3713(6) 0.092(4) Uani 1 1 d . . .
H25 H 0.3712 0.5909 0.3922 0.110 Uiso 1 1 calc R . .
C26 C 0.3214(19) 0.5469(8) 0.3122(5) 0.072(4) Uani 1 1 d . . .
H26 H 0.3514 0.5969 0.2933 0.087 Uiso 1 1 calc R . .
Cd1 Cd 0.31123(9) 0.49868(4) 0.17992(3) 0.0363(2) Uani 1 1 d . . .
Cd2 Cd 0.78087(8) 0.58150(3) 0.15707(3) 0.0306(2) Uani 1 1 d . . .
N1 N 0.557(2) 0.8164(9) 0.0080(6) 0.111(4) Uani 1 1 d U . .
N3 N 0.1281(10) 0.3812(5) 0.1759(4) 0.0458(19) Uani 1 1 d . . .
N4 N 0.1691(13) 0.3386(6) 0.2748(4) 0.068(3) Uani 1 1 d . . .
H4 H 0.1721 0.2939 0.2962 0.082 Uiso 1 1 calc R . .
N5 N 0.2698(11) 0.4803(5) 0.2793(3) 0.046(2) Uani 1 1 d . . .
O1 O 0.0733(7) 0.5636(3) 0.1246(3) 0.0369(14) Uani 1 1 d . . .
O2 O -0.0217(9) 0.6947(4) 0.1198(3) 0.0552(18) Uani 1 1 d . . .
O3 O 0.3072(10) 0.4826(4) -0.0751(3) 0.0491(17) Uani 1 1 d . . .
O4 O 0.5633(9) 0.5476(4) -0.0994(3) 0.0549(18) Uani 1 1 d . . .
O5 O 0.728(2) 0.8063(11) 0.0063(8) 0.213(9) Uani 1 1 d . . .
O6 O 0.4799(19) 0.8928(10) 0.0071(7) 0.154(5) Uani 1 1 d U . .
O7 O 0.100(2) 0.8510(7) 0.0077(5) 0.141(5) Uani 1 1 d . A .
O9 O 0.1538(9) 1.0413(4) 0.2456(3) 0.0479(16) Uani 1 1 d . . .
O10 O 0.3633(8) 0.9716(4) 0.2925(3) 0.0435(15) Uani 1 1 d . . .
O11 O 0.3638(9) 0.6384(4) 0.1915(3) 0.0530(18) Uani 1 1 d . . .
O12 O 0.6163(9) 0.6953(4) 0.1652(4) 0.067(2) Uani 1 1 d . . .
N2 N 0.151(2) 0.9023(7) 0.0440(6) 0.130(6) 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
O8 N2 1.237(17) . ?
O8' N2 1.38(2) . ?
C1 O2 1.221(10) . ?
C1 O1 1.279(9) . ?
C1 C2 1.510(12) . ?
C1 Cd2 2.718(9) 1_455 ?
C2 C7 1.392(11) . ?
C2 C3 1.432(11) . ?
C3 C4 1.346(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.407(12) . ?
C4 C15 1.499(12) . ?
C5 C6 1.372(13) . ?
C5 H5 0.9300 . ?
C6 N1 1.402(17) . ?
C6 C7 1.438(13) . ?
C7 C8 1.515(12) . ?
C8 C9 1.385(12) . ?
C8 C13 1.393(12) . ?
C9 C10 1.357(12) . ?
C9 N2 1.425(15) . ?
C10 C11 1.402(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.384(11) . ?
C11 C16 1.509(11) . ?
C12 C13 1.381(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.511(11) . ?
C14 O12 1.216(11) . ?
C14 O11 1.248(10) . ?
C15 O3 1.249(11) . ?
C15 O4 1.282(11) . ?
C16 O9 1.255(10) . ?
C16 O10 1.269(10) . ?
C16 Cd2 2.697(9) 2_655 ?
C17 C18 1.336(14) . ?
C17 N3 1.391(13) . ?
C17 H17 0.9300 . ?
C18 C19 1.38(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.44(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.419(16) . ?
C20 H20 0.9300 . ?
C21 N4 1.356(13) . ?
C21 N3 1.367(12) . ?
C22 N5 1.303(12) . ?
C22 N4 1.392(13) . ?
C22 C23 1.414(17) . ?
C23 C24 1.368(18) . ?
C23 H23 0.9300 . ?
C24 C25 1.43(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.350(17) . ?
C25 H25 0.9300 . ?
C26 N5 1.352(14) . ?
C26 H26 0.9300 . ?
Cd1 O4 2.191(7) 3_665 ?
Cd1 O11 2.265(7) . ?
Cd1 N5 2.306(8) . ?
Cd1 N3 2.318(8) . ?
Cd1 O1 2.419(6) . ?
Cd1 O10 2.563(7) 2_645 ?
Cd2 O12 2.196(6) . ?
Cd2 O3 2.228(6) 3_665 ?
Cd2 O1 2.338(6) 1_655 ?
Cd2 O10 2.352(6) 2_645 ?
Cd2 O9 2.359(6) 2_645 ?
Cd2 O2 2.479(7) 1_655 ?
Cd2 C16 2.697(9) 2_645 ?
Cd2 C1 2.718(9) 1_655 ?
N1 O5 1.295(18) . ?
N1 O6 1.343(18) . ?
N4 H4 0.8600 . ?
O1 Cd2 2.338(6) 1_455 ?
O2 Cd2 2.479(7) 1_455 ?
O3 Cd2 2.228(6) 3_665 ?
O4 Cd1 2.191(7) 3_665 ?
O7 N2 1.223(15) . ?
O9 Cd2 2.359(6) 2_655 ?
O10 Cd2 2.352(6) 2_655 ?
O10 Cd1 2.563(6) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 123.2(8) . . ?
O2 C1 C2 120.0(8) . . ?
O1 C1 C2 116.7(7) . . ?
O2 C1 Cd2 65.7(5) . 1_455 ?
O1 C1 Cd2 59.3(4) . 1_455 ?
C2 C1 Cd2 162.9(5) . 1_455 ?
C7 C2 C3 119.5(8) . . ?
C7 C2 C1 122.9(7) . . ?
C3 C2 C1 117.6(7) . . ?
C4 C3 C2 122.2(7) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 119.1(8) . . ?
C3 C4 C15 120.9(8) . . ?
C5 C4 C15 120.0(8) . . ?
C6 C5 C4 120.2(9) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 N1 113.9(10) . . ?
C5 C6 C7 121.7(8) . . ?
N1 C6 C7 124.4(10) . . ?
C2 C7 C6 117.2(8) . . ?
C2 C7 C8 121.7(8) . . ?
C6 C7 C8 120.7(7) . . ?
C9 C8 C13 117.2(7) . . ?
C9 C8 C7 124.8(8) . . ?
C13 C8 C7 117.8(7) . . ?
C10 C9 C8 123.4(8) . . ?
C10 C9 N2 116.0(9) . . ?
C8 C9 N2 120.6(9) . . ?
C9 C10 C11 119.3(8) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C12 C11 C10 118.2(8) . . ?
C12 C11 C16 120.3(8) . . ?
C10 C11 C16 121.4(7) . . ?
C13 C12 C11 121.7(8) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 C13 C8 120.1(8) . . ?
C12 C13 C14 119.5(8) . . ?
C8 C13 C14 120.4(7) . . ?
O12 C14 O11 125.1(8) . . ?
O12 C14 C13 117.0(8) . . ?
O11 C14 C13 117.9(8) . . ?
O3 C15 O4 125.9(8) . . ?
O3 C15 C4 117.9(8) . . ?
O4 C15 C4 116.2(8) . . ?
O9 C16 O10 121.5(7) . . ?
O9 C16 C11 120.2(8) . . ?
O10 C16 C11 118.3(7) . . ?
O9 C16 Cd2 61.0(4) . 2_655 ?
O10 C16 Cd2 60.7(4) . 2_655 ?
C11 C16 Cd2 174.0(6) . 2_655 ?
C18 C17 N3 125.2(11) . . ?
C18 C17 H17 117.4 . . ?
N3 C17 H17 117.4 . . ?
C17 C18 C19 116.2(13) . . ?
C17 C18 H18 121.9 . . ?
C19 C18 H18 121.9 . . ?
C18 C19 C20 122.8(12) . . ?
C18 C19 H19 118.6 . . ?
C20 C19 H19 118.6 . . ?
C21 C20 C19 115.5(14) . . ?
C21 C20 H20 122.3 . . ?
C19 C20 H20 122.3 . . ?
N4 C21 N3 121.2(9) . . ?
N4 C21 C20 117.8(11) . . ?
N3 C21 C20 121.0(12) . . ?
N5 C22 N4 123.3(10) . . ?
N5 C22 C23 120.7(11) . . ?
N4 C22 C23 116.0(10) . . ?
C24 C23 C22 121.6(12) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C25 115.5(13) . . ?
C23 C24 H24 122.2 . . ?
C25 C24 H24 122.2 . . ?
C26 C25 C24 119.7(13) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 N5 122.9(12) . . ?
C25 C26 H26 118.5 . . ?
N5 C26 H26 118.5 . . ?
O4 Cd1 O11 110.5(3) 3_665 . ?
O4 Cd1 N5 147.1(3) 3_665 . ?
O11 Cd1 N5 91.9(3) . . ?
O4 Cd1 N3 87.4(3) 3_665 . ?
O11 Cd1 N3 153.3(3) . . ?
N5 Cd1 N3 81.7(3) . . ?
O4 Cd1 O1 91.4(2) 3_665 . ?
O11 Cd1 O1 76.9(2) . . ?
N5 Cd1 O1 117.8(2) . . ?
N3 Cd1 O1 83.2(2) . . ?
O4 Cd1 O10 74.8(2) 3_665 2_645 ?
O11 Cd1 O10 88.2(2) . 2_645 ?
N5 Cd1 O10 82.4(2) . 2_645 ?
N3 Cd1 O10 116.2(2) . 2_645 ?
O1 Cd1 O10 154.86(19) . 2_645 ?
O12 Cd2 O3 106.2(3) . 3_665 ?
O12 Cd2 O1 131.1(2) . 1_655 ?
O3 Cd2 O1 87.6(2) 3_665 1_655 ?
O12 Cd2 O10 107.9(3) . 2_645 ?
O3 Cd2 O10 86.3(2) 3_665 2_645 ?
O1 Cd2 O10 119.9(2) 1_655 2_645 ?
O12 Cd2 O9 105.0(3) . 2_645 ?
O3 Cd2 O9 136.7(2) 3_665 2_645 ?
O1 Cd2 O9 94.0(2) 1_655 2_645 ?
O10 Cd2 O9 55.7(2) 2_645 2_645 ?
O12 Cd2 O2 76.8(2) . 1_655 ?
O3 Cd2 O2 102.7(2) 3_665 1_655 ?
O1 Cd2 O2 54.2(2) 1_655 1_655 ?
O10 Cd2 O2 168.4(2) 2_645 1_655 ?
O9 Cd2 O2 113.2(2) 2_645 1_655 ?
O12 Cd2 C16 110.1(3) . 2_645 ?
O3 Cd2 C16 111.6(3) 3_665 2_645 ?
O1 Cd2 C16 107.4(2) 1_655 2_645 ?
O10 Cd2 C16 28.1(2) 2_645 2_645 ?
O9 Cd2 C16 27.7(2) 2_645 2_645 ?
O2 Cd2 C16 140.6(3) 1_655 2_645 ?
O12 Cd2 C1 103.3(3) . 1_655 ?
O3 Cd2 C1 92.3(2) 3_665 1_655 ?
O1 Cd2 C1 28.1(2) 1_655 1_655 ?
O10 Cd2 C1 147.9(2) 2_645 1_655 ?
O9 Cd2 C1 108.9(2) 2_645 1_655 ?
O2 Cd2 C1 26.7(2) 1_655 1_655 ?
C16 Cd2 C1 130.3(3) 2_645 1_655 ?
O5 N1 O6 122.7(16) . . ?
O5 N1 C6 117.1(14) . . ?
O6 N1 C6 120.0(15) . . ?
C21 N3 C17 118.6(8) . . ?
C21 N3 Cd1 125.0(7) . . ?
C17 N3 Cd1 114.4(6) . . ?
C21 N4 C22 135.3(9) . . ?
C21 N4 H4 112.4 . . ?
C22 N4 H4 112.4 . . ?
C22 N5 C26 119.4(10) . . ?
C22 N5 Cd1 125.9(7) . . ?
C26 N5 Cd1 114.0(7) . . ?
C1 O1 Cd2 92.7(5) . 1_455 ?
C1 O1 Cd1 122.2(5) . . ?
Cd2 O1 Cd1 125.6(3) 1_455 . ?
C1 O2 Cd2 87.6(5) . 1_455 ?
C15 O3 Cd2 128.1(6) . 3_665 ?
C15 O4 Cd1 140.9(6) . 3_665 ?
C16 O9 Cd2 91.3(5) . 2_655 ?
C16 O10 Cd2 91.2(5) . 2_655 ?
C16 O10 Cd1 137.6(6) . 2_655 ?
Cd2 O10 Cd1 101.3(2) 2_655 2_655 ?
C14 O11 Cd1 144.3(7) . . ?
C14 O12 Cd2 127.3(6) . . ?
O7 N2 O8 118.3(14) . . ?
O7 N2 O8' 114.4(14) . . ?
O8 N2 O8' 29.0(9) . . ?
O7 N2 C9 123.1(11) . . ?
O8 N2 C9 117.7(13) . . ?
O8' N2 C9 119.0(12) . . ?

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
O2 C1 C2 C7 38.9(12) . . . . ?
O1 C1 C2 C7 -144.0(8) . . . . ?
Cd2 C1 C2 C7 144.1(17) 1_455 . . . ?
O2 C1 C2 C3 -138.0(8) . . . . ?
O1 C1 C2 C3 39.1(10) . . . . ?
Cd2 C1 C2 C3 -33(2) 1_455 . . . ?
C7 C2 C3 C4 1.2(12) . . . . ?
C1 C2 C3 C4 178.2(8) . . . . ?
C2 C3 C4 C5 2.6(13) . . . . ?
C2 C3 C4 C15 -179.7(7) . . . . ?
C3 C4 C5 C6 -4.8(14) . . . . ?
C15 C4 C5 C6 177.5(8) . . . . ?
C4 C5 C6 N1 -176.0(10) . . . . ?
C4 C5 C6 C7 3.3(15) . . . . ?
C3 C2 C7 C6 -2.7(12) . . . . ?
C1 C2 C7 C6 -179.5(8) . . . . ?
C3 C2 C7 C8 -175.4(7) . . . . ?
C1 C2 C7 C8 7.8(12) . . . . ?
C5 C6 C7 C2 0.5(14) . . . . ?
N1 C6 C7 C2 179.7(11) . . . . ?
C5 C6 C7 C8 173.3(9) . . . . ?
N1 C6 C7 C8 -7.5(16) . . . . ?
C2 C7 C8 C9 -113.7(10) . . . . ?
C6 C7 C8 C9 73.8(12) . . . . ?
C2 C7 C8 C13 69.9(11) . . . . ?
C6 C7 C8 C13 -102.5(10) . . . . ?
C13 C8 C9 C10 0.3(13) . . . . ?
C7 C8 C9 C10 -176.1(9) . . . . ?
C13 C8 C9 N2 179.2(11) . . . . ?
C7 C8 C9 N2 2.8(16) . . . . ?
C8 C9 C10 C11 -2.6(15) . . . . ?
N2 C9 C10 C11 178.5(11) . . . . ?
C9 C10 C11 C12 3.1(13) . . . . ?
C9 C10 C11 C16 -177.6(9) . . . . ?
C10 C11 C12 C13 -1.5(12) . . . . ?
C16 C11 C12 C13 179.2(8) . . . . ?
C11 C12 C13 C8 -0.8(12) . . . . ?
C11 C12 C13 C14 178.2(8) . . . . ?
C9 C8 C13 C12 1.4(12) . . . . ?
C7 C8 C13 C12 178.0(8) . . . . ?
C9 C8 C13 C14 -177.5(8) . . . . ?
C7 C8 C13 C14 -0.9(11) . . . . ?
C12 C13 C14 O12 -90.2(11) . . . . ?
C8 C13 C14 O12 88.7(10) . . . . ?
C12 C13 C14 O11 92.0(10) . . . . ?
C8 C13 C14 O11 -89.1(10) . . . . ?
C3 C4 C15 O3 15.2(12) . . . . ?
C5 C4 C15 O3 -167.1(8) . . . . ?
C3 C4 C15 O4 -164.9(8) . . . . ?
C5 C4 C15 O4 12.8(12) . . . . ?
C12 C11 C16 O9 -160.5(8) . . . . ?
C10 C11 C16 O9 20.2(13) . . . . ?
C12 C11 C16 O10 18.3(12) . . . . ?
C10 C11 C16 O10 -161.0(8) . . . . ?
N3 C17 C18 C19 -2(2) . . . . ?
C17 C18 C19 C20 9(3) . . . . ?
C18 C19 C20 C21 -11(3) . . . . ?
C19 C20 C21 N4 -172.2(14) . . . . ?
C19 C20 C21 N3 5(2) . . . . ?
N5 C22 C23 C24 2.5(19) . . . . ?
N4 C22 C23 C24 -177.9(12) . . . . ?
C22 C23 C24 C25 -4(2) . . . . ?
C23 C24 C25 C26 3(2) . . . . ?
C24 C25 C26 N5 -2(2) . . . . ?
C5 C6 N1 O5 -53.6(18) . . . . ?
C7 C6 N1 O5 127.1(16) . . . . ?
C5 C6 N1 O6 131.3(14) . . . . ?
C7 C6 N1 O6 -48.0(18) . . . . ?
N4 C21 N3 C17 178.6(10) . . . . ?
C20 C21 N3 C17 1.1(17) . . . . ?
N4 C21 N3 Cd1 15.7(14) . . . . ?
C20 C21 N3 Cd1 -161.9(10) . . . . ?
C18 C17 N3 C21 -3.3(17) . . . . ?
C18 C17 N3 Cd1 161.4(10) . . . . ?
O4 Cd1 N3 C21 123.3(8) 3_665 . . . ?
O11 Cd1 N3 C21 -103.1(9) . . . . ?
N5 Cd1 N3 C21 -25.6(8) . . . . ?
O1 Cd1 N3 C21 -145.0(8) . . . . ?
O10 Cd1 N3 C21 51.7(9) 2_645 . . . ?
O4 Cd1 N3 C17 -40.3(7) 3_665 . . . ?
O11 Cd1 N3 C17 93.4(9) . . . . ?
N5 Cd1 N3 C17 170.9(7) . . . . ?
O1 Cd1 N3 C17 51.4(7) . . . . ?
O10 Cd1 N3 C17 -111.9(7) 2_645 . . . ?
N3 C21 N4 C22 12(2) . . . . ?
C20 C21 N4 C22 -169.9(13) . . . . ?
N5 C22 N4 C21 -16(2) . . . . ?
C23 C22 N4 C21 164.5(12) . . . . ?
N4 C22 N5 C26 179.5(10) . . . . ?
C23 C22 N5 C26 -0.9(16) . . . . ?
N4 C22 N5 Cd1 -10.3(15) . . . . ?
C23 C22 N5 Cd1 169.3(8) . . . . ?
C25 C26 N5 C22 0.8(19) . . . . ?
C25 C26 N5 Cd1 -170.5(11) . . . . ?
O4 Cd1 N5 C22 -49.0(11) 3_665 . . . ?
O11 Cd1 N5 C22 177.0(8) . . . . ?
N3 Cd1 N5 C22 23.0(8) . . . . ?
O1 Cd1 N5 C22 100.8(8) . . . . ?
O10 Cd1 N5 C22 -95.1(8) 2_645 . . . ?
O4 Cd1 N5 C26 121.7(8) 3_665 . . . ?
O11 Cd1 N5 C26 -12.3(8) . . . . ?
N3 Cd1 N5 C26 -166.3(8) . . . . ?
O1 Cd1 N5 C26 -88.5(8) . . . . ?
O10 Cd1 N5 C26 75.6(8) 2_645 . . . ?
O2 C1 O1 Cd2 16.0(9) . . . 1_455 ?
C2 C1 O1 Cd2 -161.0(6) . . . 1_455 ?
O2 C1 O1 Cd1 -119.8(8) . . . . ?
C2 C1 O1 Cd1 63.1(8) . . . . ?
Cd2 C1 O1 Cd1 -135.9(5) 1_455 . . . ?
O4 Cd1 O1 C1 -89.7(6) 3_665 . . . ?
O11 Cd1 O1 C1 21.1(6) . . . . ?
N5 Cd1 O1 C1 106.2(6) . . . . ?
N3 Cd1 O1 C1 -176.8(6) . . . . ?
O10 Cd1 O1 C1 -34.2(9) 2_645 . . . ?
O4 Cd1 O1 Cd2 149.1(3) 3_665 . . 1_455 ?
O11 Cd1 O1 Cd2 -100.1(3) . . . 1_455 ?
N5 Cd1 O1 Cd2 -15.0(4) . . . 1_455 ?
N3 Cd1 O1 Cd2 61.9(3) . . . 1_455 ?
O10 Cd1 O1 Cd2 -155.4(4) 2_645 . . 1_455 ?
O1 C1 O2 Cd2 -15.1(8) . . . 1_455 ?
C2 C1 O2 Cd2 161.8(7) . . . 1_455 ?
O4 C15 O3 Cd2 -36.2(13) . . . 3_665 ?
C4 C15 O3 Cd2 143.7(6) . . . 3_665 ?
O3 C15 O4 Cd1 16.0(16) . . . 3_665 ?
C4 C15 O4 Cd1 -163.8(7) . . . 3_665 ?
O10 C16 O9 Cd2 -5.5(9) . . . 2_655 ?
C11 C16 O9 Cd2 173.2(7) . . . 2_655 ?
O9 C16 O10 Cd2 5.5(9) . . . 2_655 ?
C11 C16 O10 Cd2 -173.2(7) . . . 2_655 ?
O9 C16 O10 Cd1 -102.8(10) . . . 2_655 ?
C11 C16 O10 Cd1 78.4(10) . . . 2_655 ?
Cd2 C16 O10 Cd1 -108.4(7) 2_655 . . 2_655 ?
O12 C14 O11 Cd1 -40.9(16) . . . . ?
C13 C14 O11 Cd1 136.7(8) . . . . ?
O4 Cd1 O11 C14 -15.2(11) 3_665 . . . ?
N5 Cd1 O11 C14 140.2(10) . . . . ?
N3 Cd1 O11 C14 -144.6(10) . . . . ?
O1 Cd1 O11 C14 -101.7(10) . . . . ?
O10 Cd1 O11 C14 57.9(10) 2_645 . . . ?
O11 C14 O12 Cd2 12.8(15) . . . . ?
C13 C14 O12 Cd2 -164.7(6) . . . . ?
O3 Cd2 O12 C14 67.8(9) 3_665 . . . ?
O1 Cd2 O12 C14 169.0(7) 1_655 . . . ?
O10 Cd2 O12 C14 -23.5(9) 2_645 . . . ?
O9 Cd2 O12 C14 -81.8(9) 2_645 . . . ?
O2 Cd2 O12 C14 167.4(9) 1_655 . . . ?
C16 Cd2 O12 C14 -53.2(9) 2_645 . . . ?
C1 Cd2 O12 C14 164.2(8) 1_655 . . . ?
C10 C9 N2 O7 -157.2(16) . . . . ?
C8 C9 N2 O7 24(2) . . . . ?
C10 C9 N2 O8 34(3) . . . . ?
C8 C9 N2 O8 -145(2) . . . . ?
C10 C9 N2 O8' 1(2) . . . . ?
C8 C9 N2 O8' -178.2(17) . . . . ?


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.453 0.216 0.150 44 5 ' '
2 0.453 0.284 0.650 44 5 ' '
3 0.547 0.784 0.850 44 5 ' '
4 0.547 0.716 0.350 44 5 ' '
_platon_squeeze_details          
;
;


_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.007
_refine_diff_density_min         -2.085
_refine_diff_density_rms         0.193
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1444254'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H20 Ag2 N4 O12'
_chemical_formula_weight         832.23

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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   9.8097(14)
_cell_length_b                   11.9458(17)
_cell_length_c                   13.1508(19)
_cell_angle_alpha                99.002(2)
_cell_angle_beta                 93.161(2)
_cell_angle_gamma                110.610(2)
_cell_volume                     1414.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5997
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      28.27

_exptl_crystal_description       columnar
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7393
_exptl_absorpt_correction_T_max  0.7587
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6944
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4922
_reflns_number_gt                4483
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1300P)²+3.0130P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4922
_refine_ls_number_parameters     426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1727
_refine_ls_wR_factor_gt          0.1522
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.44050(4) 0.83078(4) 0.59942(3) 0.04118(19) Uani 1 1 d . . .
Ag2 Ag 0.73764(5) 0.96647(4) 0.53407(3) 0.04052(19) Uani 1 1 d . . .
C1 C 0.5649(4) 0.7499(4) 0.3747(3) 0.0204(8) Uani 1 1 d . . .
C2 C 0.5077(4) 0.6503(4) 0.2802(3) 0.0201(8) Uani 1 1 d . . .
C3 C 0.3646(5) 0.6225(4) 0.2338(3) 0.0248(9) Uani 1 1 d . . .
H3 H 0.3081 0.6657 0.2609 0.030 Uiso 1 1 calc R . .
C4 C 0.3078(5) 0.5302(4) 0.1472(3) 0.0265(9) Uani 1 1 d . . .
C5 C 0.3895(5) 0.4621(4) 0.1092(3) 0.0272(9) Uani 1 1 d . . .
H5 H 0.3496 0.3968 0.0541 0.033 Uiso 1 1 calc R . .
C6 C 0.5318(5) 0.4934(4) 0.1553(3) 0.0221(8) Uani 1 1 d . . .
C7 C 0.5942(4) 0.5893(4) 0.2394(3) 0.0206(8) Uani 1 1 d . . .
C8 C 0.1626(5) 0.5082(5) 0.0891(4) 0.0343(11) Uani 1 1 d . . .
C9 C 0.7485(4) 0.6269(4) 0.2907(3) 0.0204(8) Uani 1 1 d . . .
C10 C 0.8684(5) 0.7185(4) 0.2629(3) 0.0219(8) Uani 1 1 d . . .
C11 C 1.0075(5) 0.7588(4) 0.3164(4) 0.0257(9) Uani 1 1 d . . .
H11 H 1.0847 0.8186 0.2954 0.031 Uiso 1 1 calc R . .
C12 C 1.0318(5) 0.7098(4) 0.4016(3) 0.0245(9) Uani 1 1 d . . .
C13 C 0.9152(4) 0.6204(4) 0.4307(3) 0.0229(9) Uani 1 1 d . . .
H13 H 0.9303 0.5877 0.4881 0.027 Uiso 1 1 calc R . .
C14 C 0.7765(5) 0.5786(4) 0.3764(3) 0.0221(8) Uani 1 1 d . . .
C15 C 0.6560(5) 0.4755(4) 0.4079(4) 0.0256(9) Uani 1 1 d . . .
C16 C 1.1819(5) 0.7566(4) 0.4643(4) 0.0281(10) Uani 1 1 d . . .
C17 C 0.6013(7) 1.0469(5) 0.7815(4) 0.0427(13) Uani 1 1 d . . .
H17 H 0.5639 1.0886 0.7404 0.051 Uiso 1 1 calc R . .
C18 C 0.6821(9) 1.1103(6) 0.8748(5) 0.0586(18) Uani 1 1 d . . .
H18 H 0.6969 1.1921 0.8965 0.070 Uiso 1 1 calc R . .
C19 C 0.7418(7) 1.0497(6) 0.9367(5) 0.0492(14) Uani 1 1 d . . .
C20 C 0.7048(7) 0.9282(6) 0.9031(4) 0.0502(15) Uani 1 1 d . . .
H20 H 0.7337 0.8825 0.9449 0.060 Uiso 1 1 calc R . .
C21 C 0.6254(6) 0.8722(5) 0.8081(4) 0.0404(12) Uani 1 1 d . . .
H21 H 0.6071 0.7899 0.7858 0.048 Uiso 1 1 calc R . .
C22 C 0.8366(8) 1.1191(7) 1.0377(5) 0.0586(17) Uani 1 1 d . . .
H22A H 0.8837 1.0685 1.0638 0.070 Uiso 1 1 calc R . .
H22B H 0.9130 1.1912 1.0244 0.070 Uiso 1 1 calc R . .
C23 C 0.7523(8) 1.1567(7) 1.1189(5) 0.0586(17) Uani 1 1 d . . .
H23A H 0.6897 1.0848 1.1422 0.070 Uiso 1 1 calc R . .
H23B H 0.6893 1.1926 1.0882 0.070 Uiso 1 1 calc R . .
C24 C 0.8502(7) 1.2488(6) 1.2138(4) 0.0444(13) Uani 1 1 d . . .
H24A H 0.9131 1.3203 1.1900 0.053 Uiso 1 1 calc R . .
H24B H 0.7878 1.2742 1.2594 0.053 Uiso 1 1 calc R . .
C25 C 0.9440(6) 1.2024(5) 1.2747(4) 0.0335(11) Uani 1 1 d . . .
C26 C 1.0910(6) 1.2672(5) 1.3051(4) 0.0408(12) Uani 1 1 d . . .
H26 H 1.1344 1.3435 1.2878 0.049 Uiso 1 1 calc R . .
C27 C 1.1754(6) 1.2207(5) 1.3611(4) 0.0386(11) Uani 1 1 d . . .
H27 H 1.2748 1.2663 1.3794 0.046 Uiso 1 1 calc R . .
C28 C 0.9747(6) 1.0501(5) 1.3624(4) 0.0347(11) Uani 1 1 d . . .
H28 H 0.9326 0.9756 1.3829 0.042 Uiso 1 1 calc R . .
C29 C 0.8880(6) 1.0907(5) 1.3065(4) 0.0364(11) Uani 1 1 d . . .
H29 H 0.7890 1.0431 1.2890 0.044 Uiso 1 1 calc R . .
N1 N 0.5732(5) 0.9295(4) 0.7463(3) 0.0334(9) Uani 1 1 d . . .
N2 N 1.1194(5) 1.1131(4) 1.3896(3) 0.0333(9) Uani 1 1 d . . .
N3 N 0.6132(5) 0.4208(4) 0.1103(4) 0.0361(10) Uani 1 1 d . . .
N4 N 0.8498(5) 0.7753(4) 0.1729(3) 0.0335(9) Uani 1 1 d . . .
O1 O 0.5296(4) 0.7189(3) 0.4601(2) 0.0323(7) Uani 1 1 d . . .
O2 O 0.6392(4) 0.8540(3) 0.3644(3) 0.0410(9) Uani 1 1 d . . .
O3 O 0.1018(5) 0.5823(4) 0.1193(4) 0.0593(13) Uani 1 1 d . . .
H3A H 0.0287 0.5687 0.0788 0.089 Uiso 1 1 calc R . .
O4 O 0.1093(5) 0.4222(4) 0.0166(4) 0.0551(12) Uani 1 1 d . . .
O5 O 0.5487(6) 0.3298(5) 0.0451(4) 0.0707(15) Uani 1 1 d . . .
O6 O 0.7444(5) 0.4547(5) 0.1376(4) 0.0620(13) Uani 1 1 d . . .
O7 O 0.7314(5) 0.7435(5) 0.1237(4) 0.0589(12) Uani 1 1 d . . .
O8 O 0.9585(5) 0.8556(5) 0.1529(4) 0.0720(16) Uani 1 1 d . . .
O9 O 1.2814(4) 0.8497(3) 0.4453(3) 0.0389(8) Uani 1 1 d . . .
O10 O 1.2002(4) 0.6995(3) 0.5300(3) 0.0352(8) Uani 1 1 d . . .
O11 O 0.6569(4) 0.4870(3) 0.5084(2) 0.0304(7) Uani 1 1 d . . .
H11A H 0.5926 0.4275 0.5221 0.046 Uiso 1 1 calc R . .
O12 O 0.5701(4) 0.3922(3) 0.3453(3) 0.0378(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N1 2.178(4) . ?
Ag1 O10 2.358(3) 1_455 ?
Ag1 O1 2.477(3) . ?
Ag1 O9 2.577(4) 1_455 ?
Ag1 Ag2 3.0411(7) . ?
Ag2 N2 2.228(4) 2_777 ?
Ag2 O9 2.244(4) 2_776 ?
Ag2 O2 2.373(4) . ?
C1 O2 1.234(6) . ?
C1 O1 1.266(5) . ?
C1 C2 1.505(6) . ?
C2 C7 1.380(6) . ?
C2 C3 1.403(6) . ?
C3 C4 1.389(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(7) . ?
C4 C8 1.494(6) . ?
C5 C6 1.387(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.394(6) . ?
C6 N3 1.456(6) . ?
C7 C9 1.504(6) . ?
C8 O4 1.224(7) . ?
C8 O3 1.260(7) . ?
C9 C14 1.400(6) . ?
C9 C10 1.407(6) . ?
C10 C11 1.384(6) . ?
C10 N4 1.487(6) . ?
C11 C12 1.388(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.383(6) . ?
C12 C16 1.518(6) . ?
C13 C14 1.383(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.508(6) . ?
C15 O12 1.207(6) . ?
C15 O11 1.306(6) . ?
C16 O10 1.223(6) . ?
C16 O9 1.266(6) . ?
C17 N1 1.330(7) . ?
C17 C18 1.374(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.400(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.358(9) . ?
C19 C22 1.514(9) . ?
C20 C21 1.371(8) . ?
C20 H20 0.9300 . ?
C21 N1 1.328(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.496(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.544(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.488(8) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.375(8) . ?
C25 C29 1.393(8) . ?
C26 C27 1.387(8) . ?
C26 H26 0.9300 . ?
C27 N2 1.330(7) . ?
C27 H27 0.9300 . ?
C28 N2 1.348(7) . ?
C28 C29 1.353(8) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
N2 Ag2 2.228(4) 2_777 ?
N3 O5 1.216(7) . ?
N3 O6 1.219(7) . ?
N4 O7 1.201(6) . ?
N4 O8 1.231(6) . ?
O3 H3A 0.8200 . ?
O9 Ag2 2.244(4) 2_776 ?
O9 Ag1 2.577(4) 1_655 ?
O10 Ag1 2.358(3) 1_655 ?
O11 H11A 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ag1 O10 141.57(14) . 1_455 ?
N1 Ag1 O1 123.08(14) . . ?
O10 Ag1 O1 87.59(12) 1_455 . ?
N1 Ag1 O9 143.62(15) . 1_455 ?
O10 Ag1 O9 52.57(11) 1_455 1_455 ?
O1 Ag1 O9 82.60(12) . 1_455 ?
N1 Ag1 Ag2 76.80(11) . . ?
O10 Ag1 Ag2 141.59(9) 1_455 . ?
O1 Ag1 Ag2 62.76(8) . . ?
O9 Ag1 Ag2 97.23(8) 1_455 . ?
N2 Ag2 O9 135.05(14) 2_777 2_776 ?
N2 Ag2 O2 110.76(15) 2_777 . ?
O9 Ag2 O2 110.93(14) 2_776 . ?
N2 Ag2 Ag1 101.77(11) 2_777 . ?
O9 Ag2 Ag1 96.81(9) 2_776 . ?
O2 Ag2 Ag1 86.45(9) . . ?
O2 C1 O1 124.9(4) . . ?
O2 C1 C2 119.2(4) . . ?
O1 C1 C2 115.9(4) . . ?
C7 C2 C3 120.9(4) . . ?
C7 C2 C1 121.0(4) . . ?
C3 C2 C1 118.0(4) . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 C8 118.9(4) . . ?
C3 C4 C8 120.6(4) . . ?
C6 C5 C4 118.7(4) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
C5 C6 C7 122.2(4) . . ?
C5 C6 N3 116.1(4) . . ?
C7 C6 N3 121.7(4) . . ?
C2 C7 C6 118.1(4) . . ?
C2 C7 C9 118.1(4) . . ?
C6 C7 C9 123.8(4) . . ?
O4 C8 O3 123.6(5) . . ?
O4 C8 C4 120.2(5) . . ?
O3 C8 C4 116.2(4) . . ?
C14 C9 C10 116.6(4) . . ?
C14 C9 C7 120.2(4) . . ?
C10 C9 C7 123.0(4) . . ?
C11 C10 C9 122.2(4) . . ?
C11 C10 N4 117.2(4) . . ?
C9 C10 N4 120.6(4) . . ?
C10 C11 C12 120.0(4) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 118.8(4) . . ?
C13 C12 C16 120.3(4) . . ?
C11 C12 C16 120.9(4) . . ?
C12 C13 C14 121.4(4) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C9 121.1(4) . . ?
C13 C14 C15 118.9(4) . . ?
C9 C14 C15 119.9(4) . . ?
O12 C15 O11 125.0(4) . . ?
O12 C15 C14 122.3(4) . . ?
O11 C15 C14 112.7(4) . . ?
O10 C16 O9 123.6(4) . . ?
O10 C16 C12 117.2(4) . . ?
O9 C16 C12 119.2(4) . . ?
N1 C17 C18 123.9(6) . . ?
N1 C17 H17 118.0 . . ?
C18 C17 H17 118.0 . . ?
C17 C18 C19 118.8(6) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C20 C19 C18 116.6(6) . . ?
C20 C19 C22 123.6(6) . . ?
C18 C19 C22 119.7(6) . . ?
C19 C20 C21 120.6(6) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
N1 C21 C20 123.4(5) . . ?
N1 C21 H21 118.3 . . ?
C20 C21 H21 118.3 . . ?
C23 C22 C19 113.2(6) . . ?
C23 C22 H22A 108.9 . . ?
C19 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
C19 C22 H22B 108.9 . . ?
H22A C22 H22B 107.8 . . ?
C22 C23 C24 113.7(6) . . ?
C22 C23 H23A 108.8 . . ?
C24 C23 H23A 108.8 . . ?
C22 C23 H23B 108.8 . . ?
C24 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C25 C24 C23 115.0(5) . . ?
C25 C24 H24A 108.5 . . ?
C23 C24 H24A 108.5 . . ?
C25 C24 H24B 108.5 . . ?
C23 C24 H24B 108.5 . . ?
H24A C24 H24B 107.5 . . ?
C26 C25 C29 115.4(5) . . ?
C26 C25 C24 122.6(5) . . ?
C29 C25 C24 122.1(5) . . ?
C25 C26 C27 121.0(5) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
N2 C27 C26 122.4(5) . . ?
N2 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
N2 C28 C29 122.8(5) . . ?
N2 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C28 C29 C25 121.3(5) . . ?
C28 C29 H29 119.3 . . ?
C25 C29 H29 119.3 . . ?
C17 N1 C21 116.3(4) . . ?
C17 N1 Ag1 123.0(4) . . ?
C21 N1 Ag1 120.6(3) . . ?
C27 N2 C28 117.1(5) . . ?
C27 N2 Ag2 121.2(4) . 2_777 ?
C28 N2 Ag2 121.5(3) . 2_777 ?
O5 N3 O6 122.3(5) . . ?
O5 N3 C6 119.0(5) . . ?
O6 N3 C6 118.7(4) . . ?
O7 N4 O8 122.6(5) . . ?
O7 N4 C10 119.9(4) . . ?
O8 N4 C10 117.5(4) . . ?
C1 O1 Ag1 126.7(3) . . ?
C1 O2 Ag2 106.2(3) . . ?
C8 O3 H3A 109.5 . . ?
C16 O9 Ag2 122.7(3) . 2_776 ?
C16 O9 Ag1 86.1(3) . 1_655 ?
Ag2 O9 Ag1 111.81(15) 2_776 1_655 ?
C16 O10 Ag1 97.4(3) . 1_655 ?
C15 O11 H11A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ag1 Ag2 N2 62.26(17) . . . 2_777 ?
O10 Ag1 Ag2 N2 -119.95(18) 1_455 . . 2_777 ?
O1 Ag1 Ag2 N2 -76.45(14) . . . 2_777 ?
O9 Ag1 Ag2 N2 -154.25(14) 1_455 . . 2_777 ?
N1 Ag1 Ag2 O9 -76.59(16) . . . 2_776 ?
O10 Ag1 Ag2 O9 101.21(18) 1_455 . . 2_776 ?
O1 Ag1 Ag2 O9 144.70(14) . . . 2_776 ?
O9 Ag1 Ag2 O9 66.90(16) 1_455 . . 2_776 ?
N1 Ag1 Ag2 O2 172.73(15) . . . . ?
O10 Ag1 Ag2 O2 -9.47(18) 1_455 . . . ?
O1 Ag1 Ag2 O2 34.03(13) . . . . ?
O9 Ag1 Ag2 O2 -43.77(13) 1_455 . . . ?
O2 C1 C2 C7 83.4(5) . . . . ?
O1 C1 C2 C7 -97.6(5) . . . . ?
O2 C1 C2 C3 -95.6(5) . . . . ?
O1 C1 C2 C3 83.4(5) . . . . ?
C7 C2 C3 C4 1.7(6) . . . . ?
C1 C2 C3 C4 -179.3(4) . . . . ?
C2 C3 C4 C5 2.8(7) . . . . ?
C2 C3 C4 C8 -173.0(4) . . . . ?
C3 C4 C5 C6 -4.2(7) . . . . ?
C8 C4 C5 C6 171.6(4) . . . . ?
C4 C5 C6 C7 1.2(6) . . . . ?
C4 C5 C6 N3 -178.4(4) . . . . ?
C3 C2 C7 C6 -4.5(6) . . . . ?
C1 C2 C7 C6 176.5(4) . . . . ?
C3 C2 C7 C9 177.8(4) . . . . ?
C1 C2 C7 C9 -1.2(6) . . . . ?
C5 C6 C7 C2 3.1(6) . . . . ?
N3 C6 C7 C2 -177.3(4) . . . . ?
C5 C6 C7 C9 -179.3(4) . . . . ?
N3 C6 C7 C9 0.3(6) . . . . ?
C5 C4 C8 O4 8.5(8) . . . . ?
C3 C4 C8 O4 -175.7(5) . . . . ?
C5 C4 C8 O3 -171.4(5) . . . . ?
C3 C4 C8 O3 4.5(7) . . . . ?
C2 C7 C9 C14 84.9(5) . . . . ?
C6 C7 C9 C14 -92.6(5) . . . . ?
C2 C7 C9 C10 -89.0(5) . . . . ?
C6 C7 C9 C10 93.4(5) . . . . ?
C14 C9 C10 C11 0.5(6) . . . . ?
C7 C9 C10 C11 174.7(4) . . . . ?
C14 C9 C10 N4 179.9(4) . . . . ?
C7 C9 C10 N4 -5.9(6) . . . . ?
C9 C10 C11 C12 -1.0(7) . . . . ?
N4 C10 C11 C12 179.6(4) . . . . ?
C10 C11 C12 C13 0.4(6) . . . . ?
C10 C11 C12 C16 -177.2(4) . . . . ?
C11 C12 C13 C14 0.7(6) . . . . ?
C16 C12 C13 C14 178.3(4) . . . . ?
C12 C13 C14 C9 -1.2(6) . . . . ?
C12 C13 C14 C15 176.2(4) . . . . ?
C10 C9 C14 C13 0.5(6) . . . . ?
C7 C9 C14 C13 -173.8(4) . . . . ?
C10 C9 C14 C15 -176.8(4) . . . . ?
C7 C9 C14 C15 8.8(6) . . . . ?
C13 C14 C15 O12 -137.1(5) . . . . ?
C9 C14 C15 O12 40.2(6) . . . . ?
C13 C14 C15 O11 42.4(5) . . . . ?
C9 C14 C15 O11 -140.2(4) . . . . ?
C13 C12 C16 O10 11.3(6) . . . . ?
C11 C12 C16 O10 -171.2(4) . . . . ?
C13 C12 C16 O9 -170.0(4) . . . . ?
C11 C12 C16 O9 7.5(6) . . . . ?
N1 C17 C18 C19 1.3(11) . . . . ?
C17 C18 C19 C20 -5.2(11) . . . . ?
C17 C18 C19 C22 177.4(7) . . . . ?
C18 C19 C20 C21 6.4(11) . . . . ?
C22 C19 C20 C21 -176.3(6) . . . . ?
C19 C20 C21 N1 -3.8(11) . . . . ?
C20 C19 C22 C23 -107.7(9) . . . . ?
C18 C19 C22 C23 69.5(9) . . . . ?
C19 C22 C23 C24 -168.4(6) . . . . ?
C22 C23 C24 C25 -63.6(8) . . . . ?
C23 C24 C25 C26 132.3(6) . . . . ?
C23 C24 C25 C29 -48.8(7) . . . . ?
C29 C25 C26 C27 1.6(8) . . . . ?
C24 C25 C26 C27 -179.4(5) . . . . ?
C25 C26 C27 N2 -1.1(9) . . . . ?
N2 C28 C29 C25 -0.9(8) . . . . ?
C26 C25 C29 C28 -0.7(7) . . . . ?
C24 C25 C29 C28 -179.7(5) . . . . ?
C18 C17 N1 C21 1.5(9) . . . . ?
C18 C17 N1 Ag1 178.6(6) . . . . ?
C20 C21 N1 C17 -0.3(9) . . . . ?
C20 C21 N1 Ag1 -177.5(5) . . . . ?
O10 Ag1 N1 C17 -98.1(5) 1_455 . . . ?
O1 Ag1 N1 C17 124.2(4) . . . . ?
O9 Ag1 N1 C17 -4.5(6) 1_455 . . . ?
Ag2 Ag1 N1 C17 79.7(4) . . . . ?
O10 Ag1 N1 C21 78.9(5) 1_455 . . . ?
O1 Ag1 N1 C21 -58.9(4) . . . . ?
O9 Ag1 N1 C21 172.4(4) 1_455 . . . ?
Ag2 Ag1 N1 C21 -103.3(4) . . . . ?
C26 C27 N2 C28 -0.6(8) . . . . ?
C26 C27 N2 Ag2 174.0(4) . . . 2_777 ?
C29 C28 N2 C27 1.5(8) . . . . ?
C29 C28 N2 Ag2 -173.0(4) . . . 2_777 ?
C5 C6 N3 O5 -8.7(7) . . . . ?
C7 C6 N3 O5 171.6(5) . . . . ?
C5 C6 N3 O6 169.6(5) . . . . ?
C7 C6 N3 O6 -10.0(7) . . . . ?
C11 C10 N4 O7 179.8(5) . . . . ?
C9 C10 N4 O7 0.5(7) . . . . ?
C11 C10 N4 O8 -1.2(7) . . . . ?
C9 C10 N4 O8 179.5(5) . . . . ?
O2 C1 O1 Ag1 43.7(6) . . . . ?
C2 C1 O1 Ag1 -135.2(3) . . . . ?
N1 Ag1 O1 C1 -107.5(4) . . . . ?
O10 Ag1 O1 C1 97.2(4) 1_455 . . . ?
O9 Ag1 O1 C1 44.6(3) 1_455 . . . ?
Ag2 Ag1 O1 C1 -57.5(3) . . . . ?
O1 C1 O2 Ag2 11.3(6) . . . . ?
C2 C1 O2 Ag2 -169.9(3) . . . . ?
N2 Ag2 O2 C1 61.3(4) 2_777 . . . ?
O9 Ag2 O2 C1 -135.9(3) 2_776 . . . ?
Ag1 Ag2 O2 C1 -39.9(3) . . . . ?
O10 C16 O9 Ag2 -118.5(4) . . . 2_776 ?
C12 C16 O9 Ag2 62.9(5) . . . 2_776 ?
O10 C16 O9 Ag1 -5.0(5) . . . 1_655 ?
C12 C16 O9 Ag1 176.4(4) . . . 1_655 ?
O9 C16 O10 Ag1 5.5(5) . . . 1_655 ?
C12 C16 O10 Ag1 -175.8(3) . . . 1_655 ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.629
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.179
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1444255'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H24 Co2 N6 O14'
_chemical_formula_weight         930.51

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   9.782(5)
_cell_length_b                   13.006(7)
_cell_length_c                   16.517(9)
_cell_angle_alpha                105.994(9)
_cell_angle_beta                 93.197(8)
_cell_angle_gamma                109.106(9)
_cell_volume                     1883.9(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3748
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      28.05

_exptl_crystal_description       block
_exptl_crystal_colour            rose-red
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8019
_exptl_absorpt_correction_T_max  0.8308
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9385
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         25.10
_reflns_number_total             6553
_reflns_number_gt                5067
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0950P)²+25.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6553
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.2470
_refine_ls_wR_factor_gt          0.1731
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3604(7) 0.9438(6) 0.1537(4) 0.0206(14) Uani 1 1 d . . .
C2 C 0.4234(7) 1.0160(6) 0.2460(4) 0.0181(14) Uani 1 1 d . . .
C3 C 0.5504(7) 1.0090(6) 0.2814(4) 0.0201(14) Uani 1 1 d . . .
H3 H 0.5887 0.9568 0.2501 0.024 Uiso 1 1 calc R . .
C4 C 0.6216(7) 1.0784(6) 0.3627(4) 0.0210(14) Uani 1 1 d . . .
C5 C 0.5655(7) 1.1572(6) 0.4089(4) 0.0199(14) Uani 1 1 d . . .
H5 H 0.6131 1.2053 0.4632 0.024 Uiso 1 1 calc R . .
C6 C 0.4387(7) 1.1637(6) 0.3740(4) 0.0203(14) Uani 1 1 d . . .
C7 C 0.3634(7) 1.0946(5) 0.2921(4) 0.0163(13) Uani 1 1 d . . .
C8 C 0.7545(8) 1.0675(6) 0.4026(4) 0.0220(15) Uani 1 1 d . . .
C9 C 0.2204(7) 1.0934(6) 0.2564(4) 0.0191(14) Uani 1 1 d . . .
C10 C 0.2079(7) 1.1627(6) 0.2066(4) 0.0204(14) Uani 1 1 d . . .
C11 C 0.0756(8) 1.1550(7) 0.1672(5) 0.0272(16) Uani 1 1 d . . .
H11 H 0.0718 1.2031 0.1352 0.033 Uiso 1 1 calc R . .
C12 C -0.0511(7) 1.0748(6) 0.1758(4) 0.0213(15) Uani 1 1 d . . .
C13 C -0.0462(7) 1.0038(6) 0.2245(4) 0.0212(15) Uani 1 1 d . . .
H13 H -0.1325 0.9498 0.2296 0.025 Uiso 1 1 calc R . .
C14 C 0.0895(7) 1.0134(5) 0.2663(4) 0.0173(13) Uani 1 1 d . . .
C15 C 0.0857(7) 0.9403(6) 0.3216(4) 0.0198(14) Uani 1 1 d . . .
C16 C -0.1965(7) 1.0589(7) 0.1271(5) 0.0256(16) Uani 1 1 d . . .
C17 C 0.3221(12) 0.6086(8) -0.1135(6) 0.046(2) Uani 1 1 d . . .
H17 H 0.4197 0.6553 -0.1070 0.055 Uiso 1 1 calc R . .
C18 C 0.2744(15) 0.4944(9) -0.1669(7) 0.064(3) Uani 1 1 d . . .
H18 H 0.3402 0.4661 -0.1954 0.077 Uiso 1 1 calc R . .
C19 C 0.1306(15) 0.4251(8) -0.1768(6) 0.063(3) Uani 1 1 d . . .
H19 H 0.0995 0.3488 -0.2103 0.075 Uiso 1 1 calc R . .
C20 C 0.0324(15) 0.4685(8) -0.1370(6) 0.059(3) Uani 1 1 d . . .
C21 C -0.1198(15) 0.4057(10) -0.1428(7) 0.068(4) Uani 1 1 d . . .
H21 H -0.1587 0.3291 -0.1761 0.082 Uiso 1 1 calc R . .
C22 C -0.2068(13) 0.4535(10) -0.1020(7) 0.063(3) Uani 1 1 d . . .
H22 H -0.3054 0.4093 -0.1084 0.076 Uiso 1 1 calc R . .
C23 C -0.1563(10) 0.5707(9) -0.0481(6) 0.048(2) Uani 1 1 d . . .
C24 C -0.0061(9) 0.6359(7) -0.0402(5) 0.0359(19) Uani 1 1 d . . .
C25 C 0.0886(10) 0.5838(7) -0.0849(5) 0.039(2) Uani 1 1 d . . .
C26 C -0.2440(11) 0.6260(12) -0.0030(8) 0.067(3) Uani 1 1 d . . .
H26 H -0.3432 0.5859 -0.0057 0.080 Uiso 1 1 calc R . .
C27 C -0.1836(12) 0.7370(13) 0.0442(8) 0.068(3) Uani 1 1 d . . .
H27 H -0.2414 0.7757 0.0716 0.081 Uiso 1 1 calc R . .
C28 C -0.0323(11) 0.7935(9) 0.0515(6) 0.048(2) Uani 1 1 d . . .
H28 H 0.0097 0.8685 0.0875 0.057 Uiso 1 1 calc R . .
C29 C 0.3461(10) 0.7963(8) 0.3561(6) 0.043(2) Uani 1 1 d . . .
H29 H 0.3748 0.8735 0.3605 0.052 Uiso 1 1 calc R . .
C30 C 0.4430(11) 0.7408(11) 0.3344(7) 0.054(3) Uani 1 1 d . . .
H30 H 0.5359 0.7801 0.3250 0.065 Uiso 1 1 calc R . .
C31 C 0.4012(12) 0.6283(11) 0.3269(7) 0.058(3) Uani 1 1 d . . .
H31 H 0.4650 0.5895 0.3110 0.070 Uiso 1 1 calc R . .
C32 C 0.2639(11) 0.5698(8) 0.3428(6) 0.045(2) Uani 1 1 d . . .
C33 C 0.2139(17) 0.4553(10) 0.3361(10) 0.086(5) Uani 1 1 d . . .
H33 H 0.2714 0.4125 0.3155 0.104 Uiso 1 1 calc R . .
C34 C 0.083(2) 0.4022(11) 0.3587(12) 0.105(6) Uani 1 1 d . . .
H34 H 0.0588 0.3281 0.3618 0.126 Uiso 1 1 calc R . .
C35 C -0.0167(13) 0.4630(8) 0.3777(9) 0.065(3) Uani 1 1 d . . .
C36 C 0.0287(10) 0.5781(7) 0.3820(6) 0.038(2) Uani 1 1 d . . .
C37 C 0.1700(9) 0.6323(7) 0.3645(5) 0.0301(17) Uani 1 1 d . . .
C38 C -0.1593(17) 0.4145(10) 0.3958(12) 0.103(6) Uani 1 1 d . . .
H38 H -0.1946 0.3385 0.3950 0.124 Uiso 1 1 calc R . .
C39 C -0.2446(15) 0.4803(11) 0.4145(10) 0.084(4) Uani 1 1 d . . .
H39 H -0.3399 0.4487 0.4241 0.101 Uiso 1 1 calc R . .
C40 C -0.1868(11) 0.5954(9) 0.4191(7) 0.052(3) Uani 1 1 d . . .
H40 H -0.2440 0.6402 0.4343 0.062 Uiso 1 1 calc R . .
Co1 Co 0.27673(10) 0.82480(8) 0.00036(6) 0.0225(3) Uani 1 1 d . . .
Co2 Co 0.05807(10) 0.81969(8) 0.41922(6) 0.0195(3) Uani 1 1 d . . .
N1 N 0.3840(7) 1.2483(5) 0.4253(4) 0.0298(14) Uani 1 1 d . . .
N2 N 0.3391(7) 1.2510(6) 0.1976(5) 0.0372(17) Uani 1 1 d . . .
N3 N 0.2302(8) 0.6507(5) -0.0723(4) 0.0326(15) Uani 1 1 d . . .
N4 N 0.0528(7) 0.7459(6) 0.0102(4) 0.0334(15) Uani 1 1 d . . .
N5 N 0.2133(7) 0.7440(5) 0.3710(4) 0.0270(14) Uani 1 1 d . . .
N6 N -0.0541(7) 0.6438(5) 0.4026(4) 0.0293(14) Uani 1 1 d . . .
O1 O 0.3232(6) 0.9873(4) 0.1036(3) 0.0307(12) Uani 1 1 d . . .
O2 O 0.3502(6) 0.8404(4) 0.1333(3) 0.0320(12) Uani 1 1 d . . .
O3 O 0.7726(7) 0.9733(5) 0.3756(4) 0.0426(15) Uani 1 1 d . . .
O4 O 0.8357(6) 1.1532(5) 0.4633(3) 0.0345(13) Uani 1 1 d . . .
O5 O 0.4642(8) 1.3202(7) 0.4892(5) 0.074(3) Uani 1 1 d . . .
O6 O 0.2644(7) 1.2473(6) 0.4044(4) 0.0536(19) Uani 1 1 d . . .
O7 O 0.1634(6) 0.9832(4) 0.3931(3) 0.0268(11) Uani 1 1 d . . .
O8 O -0.0008(6) 0.8383(4) 0.2962(3) 0.0285(12) Uani 1 1 d . . .
O9 O -0.2990(6) 0.9676(6) 0.1164(4) 0.0427(15) Uani 1 1 d . . .
O10 O -0.1976(6) 1.1408(5) 0.1008(4) 0.0383(14) Uani 1 1 d . . .
O11 O 0.3267(8) 1.2968(10) 0.1467(8) 0.109(4) Uani 1 1 d . . .
O12 O 0.4501(8) 1.2800(8) 0.2422(7) 0.092(4) Uani 1 1 d . . .
O1W O 0.4942(6) 0.8696(4) -0.0180(4) 0.0317(12) Uani 1 1 d . . .
O2W O -0.1185(6) 0.8647(4) 0.4579(3) 0.0307(12) Uani 1 1 d . . .
H1WA H 0.5483 0.9109 -0.0430 0.046 Uiso 1 1 d R . .
H1WB H 0.5618 0.9006 0.0260 0.046 Uiso 1 1 d R . .
H2WA H -0.1540 0.8997 0.4310 0.046 Uiso 1 1 d R . .
H2WB H -0.1317 0.9100 0.5022 0.046 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.223(9) . ?
C1 O2 1.262(9) . ?
C1 C2 1.521(9) . ?
C1 Co1 2.502(7) . ?
C2 C3 1.384(9) . ?
C2 C7 1.409(10) . ?
C3 C4 1.385(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(10) . ?
C4 C8 1.491(9) . ?
C5 C6 1.377(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.402(9) . ?
C6 N1 1.462(9) . ?
C7 C9 1.481(9) . ?
C8 O3 1.257(9) . ?
C8 O4 1.263(9) . ?
C9 C10 1.404(10) . ?
C9 C14 1.412(10) . ?
C10 C11 1.376(10) . ?
C10 N2 1.463(10) . ?
C11 C12 1.378(11) . ?
C11 H11 0.9300 . ?
C12 C13 1.393(10) . ?
C12 C16 1.516(9) . ?
C13 C14 1.412(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.483(10) . ?
C15 O7 1.242(8) . ?
C15 O8 1.253(9) . ?
C15 Co2 2.510(7) . ?
C16 O9 1.237(10) . ?
C16 O10 1.260(10) . ?
C17 N3 1.325(12) . ?
C17 C18 1.407(14) . ?
C17 H17 0.9300 . ?
C18 C19 1.372(18) . ?
C18 H18 0.9300 . ?
C19 C20 1.377(18) . ?
C19 H19 0.9300 . ?
C20 C25 1.410(12) . ?
C20 C21 1.428(18) . ?
C21 C22 1.320(19) . ?
C21 H21 0.9300 . ?
C22 C23 1.439(16) . ?
C22 H22 0.9300 . ?
C23 C26 1.411(17) . ?
C23 C24 1.413(12) . ?
C24 N4 1.349(11) . ?
C24 C25 1.440(13) . ?
C25 N3 1.341(11) . ?
C26 C27 1.346(18) . ?
C26 H26 0.9300 . ?
C27 C28 1.402(15) . ?
C27 H27 0.9300 . ?
C28 N4 1.307(12) . ?
C28 H28 0.9300 . ?
C29 N5 1.326(11) . ?
C29 C30 1.375(14) . ?
C29 H29 0.9300 . ?
C30 C31 1.352(16) . ?
C30 H30 0.9300 . ?
C31 C32 1.390(15) . ?
C31 H31 0.9300 . ?
C32 C33 1.377(16) . ?
C32 C37 1.412(11) . ?
C33 C34 1.37(2) . ?
C33 H33 0.9300 . ?
C34 C35 1.442(17) . ?
C34 H34 0.9300 . ?
C35 C36 1.395(12) . ?
C35 C38 1.417(17) . ?
C36 N6 1.351(11) . ?
C36 C37 1.418(12) . ?
C37 N5 1.345(10) . ?
C38 C39 1.370(19) . ?
C38 H38 0.9300 . ?
C39 C40 1.395(16) . ?
C39 H39 0.9300 . ?
C40 N6 1.324(11) . ?
C40 H40 0.9300 . ?
Co1 O10 2.021(5) 2_575 ?
Co1 O1W 2.077(6) . ?
Co1 N4 2.130(7) . ?
Co1 N3 2.131(6) . ?
Co1 O2 2.205(5) . ?
Co1 O1 2.209(5) . ?
Co2 O4 2.031(5) 2_676 ?
Co2 O2W 2.076(5) . ?
Co2 N6 2.119(6) . ?
Co2 N5 2.143(6) . ?
Co2 O8 2.179(5) . ?
Co2 O7 2.212(5) . ?
N1 O6 1.196(9) . ?
N1 O5 1.220(9) . ?
N2 O12 1.163(9) . ?
N2 O11 1.179(10) . ?
O4 Co2 2.031(5) 2_676 ?
O10 Co1 2.021(5) 2_575 ?
O1W H1WA 0.8364 . ?
O1W H1WB 0.8589 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 123.6(6) . . ?
O1 C1 C2 119.7(6) . . ?
O2 C1 C2 116.7(6) . . ?
O1 C1 Co1 62.0(4) . . ?
O2 C1 Co1 61.8(4) . . ?
C2 C1 Co1 175.4(5) . . ?
C3 C2 C7 120.5(6) . . ?
C3 C2 C1 117.5(6) . . ?
C7 C2 C1 121.8(6) . . ?
C4 C3 C2 121.3(6) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.3(6) . . ?
C5 C4 C8 119.2(6) . . ?
C3 C4 C8 121.4(6) . . ?
C4 C5 C6 119.5(6) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C7 122.8(6) . . ?
C5 C6 N1 117.4(6) . . ?
C7 C6 N1 119.8(6) . . ?
C6 C7 C2 116.6(6) . . ?
C6 C7 C9 123.5(6) . . ?
C2 C7 C9 119.6(6) . . ?
O3 C8 O4 126.0(6) . . ?
O3 C8 C4 117.7(6) . . ?
O4 C8 C4 116.2(6) . . ?
C10 C9 C14 117.4(6) . . ?
C10 C9 C7 122.9(6) . . ?
C14 C9 C7 119.5(6) . . ?
C11 C10 C9 123.2(6) . . ?
C11 C10 N2 116.9(6) . . ?
C9 C10 N2 119.8(6) . . ?
C10 C11 C12 118.8(7) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C11 C12 C13 120.8(6) . . ?
C11 C12 C16 119.5(6) . . ?
C13 C12 C16 119.6(6) . . ?
C12 C13 C14 120.2(6) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C9 119.5(6) . . ?
C13 C14 C15 117.3(6) . . ?
C9 C14 C15 123.2(6) . . ?
O7 C15 O8 121.9(7) . . ?
O7 C15 C14 119.1(6) . . ?
O8 C15 C14 118.9(6) . . ?
O7 C15 Co2 61.8(4) . . ?
O8 C15 Co2 60.2(4) . . ?
C14 C15 Co2 174.7(5) . . ?
O9 C16 O10 127.3(7) . . ?
O9 C16 C12 117.4(7) . . ?
O10 C16 C12 115.3(7) . . ?
N3 C17 C18 121.1(10) . . ?
N3 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 119.8(11) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 120.0(9) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C25 116.8(11) . . ?
C19 C20 C21 125.3(10) . . ?
C25 C20 C21 117.9(12) . . ?
C22 C21 C20 121.6(10) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C21 C22 C23 123.2(10) . . ?
C21 C22 H22 118.4 . . ?
C23 C22 H22 118.4 . . ?
C26 C23 C24 117.3(10) . . ?
C26 C23 C22 125.6(10) . . ?
C24 C23 C22 117.1(10) . . ?
N4 C24 C23 121.8(9) . . ?
N4 C24 C25 118.5(7) . . ?
C23 C24 C25 119.7(8) . . ?
N3 C25 C20 123.5(10) . . ?
N3 C25 C24 116.0(7) . . ?
C20 C25 C24 120.5(9) . . ?
C27 C26 C23 119.7(10) . . ?
C27 C26 H26 120.1 . . ?
C23 C26 H26 120.1 . . ?
C26 C27 C28 118.9(12) . . ?
C26 C27 H27 120.5 . . ?
C28 C27 H27 120.5 . . ?
N4 C28 C27 123.3(10) . . ?
N4 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
N5 C29 C30 122.6(9) . . ?
N5 C29 H29 118.7 . . ?
C30 C29 H29 118.7 . . ?
C31 C30 C29 118.9(10) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C30 C31 C32 120.8(9) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 H31 119.6 . . ?
C33 C32 C31 123.9(10) . . ?
C33 C32 C37 119.0(10) . . ?
C31 C32 C37 117.1(9) . . ?
C34 C33 C32 122.6(11) . . ?
C34 C33 H33 118.7 . . ?
C32 C33 H33 118.7 . . ?
C33 C34 C35 118.8(11) . . ?
C33 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C36 C35 C38 116.5(10) . . ?
C36 C35 C34 119.4(11) . . ?
C38 C35 C34 124.1(11) . . ?
N6 C36 C35 124.0(9) . . ?
N6 C36 C37 116.5(7) . . ?
C35 C36 C37 119.5(8) . . ?
N5 C37 C32 121.2(8) . . ?
N5 C37 C36 118.7(7) . . ?
C32 C37 C36 120.1(8) . . ?
C39 C38 C35 119.5(10) . . ?
C39 C38 H38 120.3 . . ?
C35 C38 H38 120.3 . . ?
C38 C39 C40 119.2(11) . . ?
C38 C39 H39 120.4 . . ?
C40 C39 H39 120.4 . . ?
N6 C40 C39 123.0(10) . . ?
N6 C40 H40 118.5 . . ?
C39 C40 H40 118.5 . . ?
O10 Co1 O1W 97.6(2) 2_575 . ?
O10 Co1 N4 85.5(3) 2_575 . ?
O1W Co1 N4 169.0(2) . . ?
O10 Co1 N3 92.0(3) 2_575 . ?
O1W Co1 N3 91.6(2) . . ?
N4 Co1 N3 77.7(3) . . ?
O10 Co1 O2 160.6(2) 2_575 . ?
O1W Co1 O2 88.5(2) . . ?
N4 Co1 O2 92.0(2) . . ?
N3 Co1 O2 106.3(2) . . ?
O10 Co1 O1 101.7(2) 2_575 . ?
O1W Co1 O1 92.1(2) . . ?
N4 Co1 O1 97.7(2) . . ?
N3 Co1 O1 165.2(2) . . ?
O2 Co1 O1 59.5(2) . . ?
O10 Co1 C1 130.9(2) 2_575 . ?
O1W Co1 C1 89.1(2) . . ?
N4 Co1 C1 96.9(2) . . ?
N3 Co1 C1 136.5(2) . . ?
O2 Co1 C1 30.3(2) . . ?
O1 Co1 C1 29.3(2) . . ?
O4 Co2 O2W 97.8(2) 2_676 . ?
O4 Co2 N6 92.5(3) 2_676 . ?
O2W Co2 N6 93.2(2) . . ?
O4 Co2 N5 85.6(2) 2_676 . ?
O2W Co2 N5 170.2(2) . . ?
N6 Co2 N5 77.5(2) . . ?
O4 Co2 O8 162.5(2) 2_676 . ?
O2W Co2 O8 87.5(2) . . ?
N6 Co2 O8 103.9(2) . . ?
N5 Co2 O8 91.9(2) . . ?
O4 Co2 O7 103.4(2) 2_676 . ?
O2W Co2 O7 92.3(2) . . ?
N6 Co2 O7 162.3(2) . . ?
N5 Co2 O7 95.8(2) . . ?
O8 Co2 O7 59.58(19) . . ?
O4 Co2 C15 133.0(2) 2_676 . ?
O2W Co2 C15 89.2(2) . . ?
N6 Co2 C15 133.6(2) . . ?
N5 Co2 C15 95.2(2) . . ?
O8 Co2 C15 30.0(2) . . ?
O7 Co2 C15 29.6(2) . . ?
O6 N1 O5 121.2(7) . . ?
O6 N1 C6 120.7(6) . . ?
O5 N1 C6 118.1(6) . . ?
O12 N2 O11 120.7(8) . . ?
O12 N2 C10 121.6(7) . . ?
O11 N2 C10 117.6(7) . . ?
C17 N3 C25 118.8(7) . . ?
C17 N3 Co1 126.2(6) . . ?
C25 N3 Co1 114.3(6) . . ?
C28 N4 C24 118.8(8) . . ?
C28 N4 Co1 128.1(7) . . ?
C24 N4 Co1 112.7(6) . . ?
C29 N5 C37 119.4(7) . . ?
C29 N5 Co2 127.8(6) . . ?
C37 N5 Co2 112.5(5) . . ?
C40 N6 C36 117.8(7) . . ?
C40 N6 Co2 127.6(6) . . ?
C36 N6 Co2 114.2(5) . . ?
C1 O1 Co1 88.7(4) . . ?
C1 O2 Co1 88.0(4) . . ?
C8 O4 Co2 136.3(5) . 2_676 ?
C15 O7 Co2 88.6(4) . . ?
C15 O8 Co2 89.8(4) . . ?
C16 O10 Co1 142.1(5) . 2_575 ?
Co1 O1W H1WA 136.4 . . ?
Co1 O1W H1WB 118.7 . . ?
H1WA O1W H1WB 89.0 . . ?
Co2 O2W H2WA 119.5 . . ?
Co2 O2W H2WB 134.9 . . ?
H2WA O2W H2WB 84.7 . . ?

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
O1 C1 C2 C3 -132.7(7) . . . . ?
O2 C1 C2 C3 47.1(9) . . . . ?
O1 C1 C2 C7 41.9(10) . . . . ?
O2 C1 C2 C7 -138.3(7) . . . . ?
C7 C2 C3 C4 0.1(10) . . . . ?
C1 C2 C3 C4 174.8(6) . . . . ?
C2 C3 C4 C5 -0.7(11) . . . . ?
C2 C3 C4 C8 177.2(7) . . . . ?
C3 C4 C5 C6 1.1(11) . . . . ?
C8 C4 C5 C6 -176.8(6) . . . . ?
C4 C5 C6 C7 -1.0(11) . . . . ?
C4 C5 C6 N1 -179.9(6) . . . . ?
C5 C6 C7 C2 0.3(10) . . . . ?
N1 C6 C7 C2 179.2(6) . . . . ?
C5 C6 C7 C9 174.6(6) . . . . ?
N1 C6 C7 C9 -6.5(10) . . . . ?
C3 C2 C7 C6 0.1(9) . . . . ?
C1 C2 C7 C6 -174.4(6) . . . . ?
C3 C2 C7 C9 -174.4(6) . . . . ?
C1 C2 C7 C9 11.1(9) . . . . ?
C5 C4 C8 O3 154.5(7) . . . . ?
C3 C4 C8 O3 -23.3(11) . . . . ?
C5 C4 C8 O4 -22.6(10) . . . . ?
C3 C4 C8 O4 159.5(7) . . . . ?
C6 C7 C9 C10 93.1(8) . . . . ?
C2 C7 C9 C10 -92.8(8) . . . . ?
C6 C7 C9 C14 -92.2(8) . . . . ?
C2 C7 C9 C14 81.9(8) . . . . ?
C14 C9 C10 C11 -0.6(10) . . . . ?
C7 C9 C10 C11 174.2(7) . . . . ?
C14 C9 C10 N2 176.9(6) . . . . ?
C7 C9 C10 N2 -8.2(10) . . . . ?
C9 C10 C11 C12 -0.7(11) . . . . ?
N2 C10 C11 C12 -178.4(7) . . . . ?
C10 C11 C12 C13 0.9(11) . . . . ?
C10 C11 C12 C16 -175.2(7) . . . . ?
C11 C12 C13 C14 0.3(10) . . . . ?
C16 C12 C13 C14 176.4(6) . . . . ?
C12 C13 C14 C9 -1.7(10) . . . . ?
C12 C13 C14 C15 176.1(6) . . . . ?
C10 C9 C14 C13 1.8(9) . . . . ?
C7 C9 C14 C13 -173.2(6) . . . . ?
C10 C9 C14 C15 -175.8(6) . . . . ?
C7 C9 C14 C15 9.1(10) . . . . ?
C13 C14 C15 O7 -135.1(7) . . . . ?
C9 C14 C15 O7 42.6(9) . . . . ?
C13 C14 C15 O8 41.8(9) . . . . ?
C9 C14 C15 O8 -140.5(7) . . . . ?
C11 C12 C16 O9 159.7(7) . . . . ?
C13 C12 C16 O9 -16.4(10) . . . . ?
C11 C12 C16 O10 -19.1(10) . . . . ?
C13 C12 C16 O10 164.8(7) . . . . ?
N3 C17 C18 C19 0.0(17) . . . . ?
C17 C18 C19 C20 2.4(17) . . . . ?
C18 C19 C20 C25 -2.1(15) . . . . ?
C18 C19 C20 C21 179.5(10) . . . . ?
C19 C20 C21 C22 179.4(10) . . . . ?
C25 C20 C21 C22 1.1(15) . . . . ?
C20 C21 C22 C23 -0.9(17) . . . . ?
C21 C22 C23 C26 -179.8(11) . . . . ?
C21 C22 C23 C24 0.5(15) . . . . ?
C26 C23 C24 N4 1.6(13) . . . . ?
C22 C23 C24 N4 -178.6(8) . . . . ?
C26 C23 C24 C25 180.0(8) . . . . ?
C22 C23 C24 C25 -0.3(13) . . . . ?
C19 C20 C25 N3 -0.5(13) . . . . ?
C21 C20 C25 N3 178.0(8) . . . . ?
C19 C20 C25 C24 -179.4(8) . . . . ?
C21 C20 C25 C24 -0.9(13) . . . . ?
N4 C24 C25 N3 0.0(11) . . . . ?
C23 C24 C25 N3 -178.4(8) . . . . ?
N4 C24 C25 C20 178.9(8) . . . . ?
C23 C24 C25 C20 0.5(12) . . . . ?
C24 C23 C26 C27 0.9(16) . . . . ?
C22 C23 C26 C27 -178.8(11) . . . . ?
C23 C26 C27 C28 -3.8(18) . . . . ?
C26 C27 C28 N4 4.6(17) . . . . ?
N5 C29 C30 C31 0.8(15) . . . . ?
C29 C30 C31 C32 -1.5(16) . . . . ?
C30 C31 C32 C33 179.8(12) . . . . ?
C30 C31 C32 C37 1.7(15) . . . . ?
C31 C32 C33 C34 174.6(15) . . . . ?
C37 C32 C33 C34 -7(2) . . . . ?
C32 C33 C34 C35 10(3) . . . . ?
C33 C34 C35 C36 -7(2) . . . . ?
C33 C34 C35 C38 175.3(17) . . . . ?
C38 C35 C36 N6 0.4(19) . . . . ?
C34 C35 C36 N6 -177.2(12) . . . . ?
C38 C35 C36 C37 -179.9(12) . . . . ?
C34 C35 C36 C37 2.4(19) . . . . ?
C33 C32 C37 N5 -179.4(11) . . . . ?
C31 C32 C37 N5 -1.2(13) . . . . ?
C33 C32 C37 C36 2.2(15) . . . . ?
C31 C32 C37 C36 -179.6(9) . . . . ?
N6 C36 C37 N5 1.3(12) . . . . ?
C35 C36 C37 N5 -178.4(9) . . . . ?
N6 C36 C37 C32 179.7(8) . . . . ?
C35 C36 C37 C32 0.0(14) . . . . ?
C36 C35 C38 C39 1(2) . . . . ?
C34 C35 C38 C39 178.8(17) . . . . ?
C35 C38 C39 C40 -3(3) . . . . ?
C38 C39 C40 N6 3(2) . . . . ?
O1 C1 Co1 O10 -3.4(6) . . . 2_575 ?
O2 C1 Co1 O10 172.2(4) . . . 2_575 ?
O1 C1 Co1 O1W 95.9(4) . . . . ?
O2 C1 Co1 O1W -88.5(4) . . . . ?
O1 C1 Co1 N4 -93.4(4) . . . . ?
O2 C1 Co1 N4 82.2(4) . . . . ?
O1 C1 Co1 N3 -172.7(4) . . . . ?
O2 C1 Co1 N3 2.9(6) . . . . ?
O1 C1 Co1 O2 -175.6(7) . . . . ?
O2 C1 Co1 O1 175.6(7) . . . . ?
O7 C15 Co2 O4 -3.7(5) . . . 2_676 ?
O8 C15 Co2 O4 173.6(4) . . . 2_676 ?
O7 C15 Co2 O2W 96.2(4) . . . . ?
O8 C15 Co2 O2W -86.5(4) . . . . ?
O7 C15 Co2 N6 -170.2(4) . . . . ?
O8 C15 Co2 N6 7.1(5) . . . . ?
O7 C15 Co2 N5 -92.6(4) . . . . ?
O8 C15 Co2 N5 84.7(4) . . . . ?
O7 C15 Co2 O8 -177.3(7) . . . . ?
O8 C15 Co2 O7 177.3(7) . . . . ?
C5 C6 N1 O6 -169.0(8) . . . . ?
C7 C6 N1 O6 12.1(11) . . . . ?
C5 C6 N1 O5 11.6(11) . . . . ?
C7 C6 N1 O5 -167.3(8) . . . . ?
C11 C10 N2 O12 163.6(10) . . . . ?
C9 C10 N2 O12 -14.1(13) . . . . ?
C11 C10 N2 O11 -12.0(13) . . . . ?
C9 C10 N2 O11 170.2(10) . . . . ?
C18 C17 N3 C25 -2.6(14) . . . . ?
C18 C17 N3 Co1 -173.1(8) . . . . ?
C20 C25 N3 C17 2.9(13) . . . . ?
C24 C25 N3 C17 -178.2(8) . . . . ?
C20 C25 N3 Co1 174.5(7) . . . . ?
C24 C25 N3 Co1 -6.6(9) . . . . ?
O10 Co1 N3 C17 93.5(8) 2_575 . . . ?
O1W Co1 N3 C17 -4.1(7) . . . . ?
N4 Co1 N3 C17 178.5(8) . . . . ?
O2 Co1 N3 C17 -93.0(8) . . . . ?
O1 Co1 N3 C17 -108.5(11) . . . . ?
C1 Co1 N3 C17 -94.5(8) . . . . ?
O10 Co1 N3 C25 -77.4(6) 2_575 . . . ?
O1W Co1 N3 C25 -175.0(6) . . . . ?
N4 Co1 N3 C25 7.6(6) . . . . ?
O2 Co1 N3 C25 96.1(6) . . . . ?
O1 Co1 N3 C25 80.6(11) . . . . ?
C1 Co1 N3 C25 94.6(6) . . . . ?
C27 C28 N4 C24 -2.1(14) . . . . ?
C27 C28 N4 Co1 170.9(8) . . . . ?
C23 C24 N4 C28 -1.0(12) . . . . ?
C25 C24 N4 C28 -179.4(8) . . . . ?
C23 C24 N4 Co1 -175.1(6) . . . . ?
C25 C24 N4 Co1 6.5(9) . . . . ?
O10 Co1 N4 C28 -87.7(8) 2_575 . . . ?
O1W Co1 N4 C28 165.7(11) . . . . ?
N3 Co1 N4 C28 179.3(8) . . . . ?
O2 Co1 N4 C28 73.0(8) . . . . ?
O1 Co1 N4 C28 13.6(8) . . . . ?
C1 Co1 N4 C28 43.1(8) . . . . ?
O10 Co1 N4 C24 85.7(6) 2_575 . . . ?
O1W Co1 N4 C24 -21.0(16) . . . . ?
N3 Co1 N4 C24 -7.4(5) . . . . ?
O2 Co1 N4 C24 -113.6(6) . . . . ?
O1 Co1 N4 C24 -173.1(5) . . . . ?
C1 Co1 N4 C24 -143.6(6) . . . . ?
C30 C29 N5 C37 -0.3(13) . . . . ?
C30 C29 N5 Co2 172.2(7) . . . . ?
C32 C37 N5 C29 0.5(12) . . . . ?
C36 C37 N5 C29 178.9(8) . . . . ?
C32 C37 N5 Co2 -173.1(6) . . . . ?
C36 C37 N5 Co2 5.3(9) . . . . ?
O4 Co2 N5 C29 -86.2(7) 2_676 . . . ?
N6 Co2 N5 C29 -179.7(7) . . . . ?
O8 Co2 N5 C29 76.5(7) . . . . ?
O7 Co2 N5 C29 16.9(7) . . . . ?
C15 Co2 N5 C29 46.6(7) . . . . ?
O4 Co2 N5 C37 86.7(5) 2_676 . . . ?
N6 Co2 N5 C37 -6.8(5) . . . . ?
O8 Co2 N5 C37 -110.6(5) . . . . ?
O7 Co2 N5 C37 -170.2(5) . . . . ?
C15 Co2 N5 C37 -140.4(5) . . . . ?
C39 C40 N6 C36 -1.1(16) . . . . ?
C39 C40 N6 Co2 -172.9(10) . . . . ?
C35 C36 N6 C40 -0.5(15) . . . . ?
C37 C36 N6 C40 179.8(8) . . . . ?
C35 C36 N6 Co2 172.3(9) . . . . ?
C37 C36 N6 Co2 -7.3(10) . . . . ?
O4 Co2 N6 C40 94.7(8) 2_676 . . . ?
O2W Co2 N6 C40 -3.3(8) . . . . ?
N5 Co2 N6 C40 179.7(9) . . . . ?
O8 Co2 N6 C40 -91.5(8) . . . . ?
O7 Co2 N6 C40 -111.2(10) . . . . ?
C15 Co2 N6 C40 -95.2(8) . . . . ?
O4 Co2 N6 C36 -77.4(6) 2_676 . . . ?
O2W Co2 N6 C36 -175.4(6) . . . . ?
N5 Co2 N6 C36 7.6(6) . . . . ?
O8 Co2 N6 C36 96.4(6) . . . . ?
O7 Co2 N6 C36 76.7(10) . . . . ?
C15 Co2 N6 C36 92.8(6) . . . . ?
O2 C1 O1 Co1 -4.6(7) . . . . ?
C2 C1 O1 Co1 175.1(6) . . . . ?
O10 Co1 O1 C1 177.4(4) 2_575 . . . ?
O1W Co1 O1 C1 -84.5(4) . . . . ?
N4 Co1 O1 C1 90.4(4) . . . . ?
N3 Co1 O1 C1 19.8(11) . . . . ?
O2 Co1 O1 C1 2.6(4) . . . . ?
O1 C1 O2 Co1 4.6(7) . . . . ?
C2 C1 O2 Co1 -175.1(5) . . . . ?
O10 Co1 O2 C1 -18.0(9) 2_575 . . . ?
O1W Co1 O2 C1 90.8(4) . . . . ?
N4 Co1 O2 C1 -100.2(4) . . . . ?
N3 Co1 O2 C1 -177.9(4) . . . . ?
O1 Co1 O2 C1 -2.5(4) . . . . ?
O3 C8 O4 Co2 -41.2(12) . . . 2_676 ?
C4 C8 O4 Co2 135.8(6) . . . 2_676 ?
O8 C15 O7 Co2 -2.8(7) . . . . ?
C14 C15 O7 Co2 174.0(5) . . . . ?
O4 Co2 O7 C15 177.2(4) 2_676 . . . ?
O2W Co2 O7 C15 -84.2(4) . . . . ?
N6 Co2 O7 C15 23.8(9) . . . . ?
N5 Co2 O7 C15 90.3(4) . . . . ?
O8 Co2 O7 C15 1.6(4) . . . . ?
O7 C15 O8 Co2 2.8(7) . . . . ?
C14 C15 O8 Co2 -174.0(5) . . . . ?
O4 Co2 O8 C15 -15.8(9) 2_676 . . . ?
O2W Co2 O8 C15 92.6(4) . . . . ?
N6 Co2 O8 C15 -174.7(4) . . . . ?
N5 Co2 O8 C15 -97.2(4) . . . . ?
O7 Co2 O8 C15 -1.5(4) . . . . ?
O9 C16 O10 Co1 -38.4(14) . . . 2_575 ?
C12 C16 O10 Co1 140.3(7) . . . 2_575 ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.623
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.236
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1444256'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H24 N6 Ni2 O14'
_chemical_formula_weight         930.07

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   9.7979(14)
_cell_length_b                   12.9930(18)
_cell_length_c                   16.450(2)
_cell_angle_alpha                106.174(2)
_cell_angle_beta                 93.467(2)
_cell_angle_gamma                108.962(2)
_cell_volume                     1875.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3733
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      28.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8120
_exptl_absorpt_correction_T_max  0.8369
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9439
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         25.10
_reflns_number_total             6537
_reflns_number_gt                5128
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0100P)²+45.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6537
_refine_ls_number_parameters     559
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0622
_refine_ls_wR_factor_ref         0.2270
_refine_ls_wR_factor_gt          0.1482
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8603(8) 0.9385(7) 0.6538(5) 0.0201(16) Uani 1 1 d . . .
C2 C 0.9246(8) 1.0139(6) 0.7445(5) 0.0182(16) Uani 1 1 d . . .
C3 C 1.0536(8) 1.0064(7) 0.7824(5) 0.0194(16) Uani 1 1 d . . .
H3 H 1.0911 0.9525 0.7525 0.023 Uiso 1 1 calc R . .
C4 C 1.1236(8) 1.0792(7) 0.8637(5) 0.0205(16) Uani 1 1 d . . .
C5 C 1.0675(8) 1.1581(7) 0.9101(5) 0.0206(16) Uani 1 1 d . . .
H5 H 1.1155 1.2073 0.9644 0.025 Uiso 1 1 calc R . .
C6 C 0.9392(8) 1.1627(6) 0.8745(5) 0.0188(16) Uani 1 1 d . . .
C7 C 0.8614(8) 1.0907(6) 0.7915(5) 0.0171(15) Uani 1 1 d . . .
C8 C 0.7195(8) 1.0894(6) 0.7548(5) 0.0175(15) Uani 1 1 d . . .
C9 C 0.7070(8) 1.1621(7) 0.7068(5) 0.0221(17) Uani 1 1 d . . .
C10 C 0.5744(9) 1.1548(7) 0.6680(5) 0.0256(18) Uani 1 1 d . . .
H10 H 0.5707 1.2033 0.6364 0.031 Uiso 1 1 calc R . .
C11 C 0.4459(9) 1.0748(7) 0.6762(5) 0.0232(17) Uani 1 1 d . . .
C12 C 0.4536(8) 1.0046(7) 0.7225(5) 0.0219(17) Uani 1 1 d . . .
H12 H 0.3674 0.9497 0.7263 0.026 Uiso 1 1 calc R . .
C13 C 0.5852(9) 1.0117(6) 0.7644(5) 0.0191(16) Uani 1 1 d . . .
C14 C 0.5816(9) 0.9375(7) 0.8194(5) 0.0201(16) Uani 1 1 d . . .
C15 C 0.7422(8) 0.9302(7) 1.0954(5) 0.0206(17) Uani 1 1 d . . .
C16 C 0.7001(9) 0.9376(8) 0.3733(5) 0.0284(19) Uani 1 1 d . . .
C17 C 0.8265(13) 0.6103(9) 0.3901(7) 0.045(3) Uani 1 1 d . . .
H17 H 0.9250 0.6557 0.3993 0.054 Uiso 1 1 calc R . .
C18 C 0.7809(16) 0.4956(10) 0.3346(8) 0.060(3) Uani 1 1 d . . .
H18 H 0.8477 0.4674 0.3073 0.072 Uiso 1 1 calc R . .
C19 C 0.6391(17) 0.4283(9) 0.3224(8) 0.065(4) Uani 1 1 d U . .
H19 H 0.6074 0.3530 0.2862 0.078 Uiso 1 1 calc R . .
C20 C 0.5400(15) 0.4708(10) 0.3635(7) 0.055(3) Uani 1 1 d . . .
C21 C 0.5948(12) 0.5868(8) 0.4167(6) 0.043(3) Uani 1 1 d . . .
C22 C 0.4990(10) 0.6394(8) 0.4596(6) 0.033(2) Uani 1 1 d . . .
C23 C 0.3485(12) 0.5757(11) 0.4515(7) 0.051(3) Uani 1 1 d . . .
C24 C 0.2943(15) 0.4579(12) 0.3985(9) 0.066(4) Uani 1 1 d . . .
H24 H 0.1961 0.4140 0.3937 0.080 Uiso 1 1 calc R . .
C25 C 0.3779(16) 0.4110(10) 0.3572(8) 0.066(4) Uani 1 1 d U . .
H25 H 0.3355 0.3355 0.3213 0.079 Uiso 1 1 calc R . .
C26 C 0.2613(13) 0.6307(14) 0.4948(9) 0.064(4) Uani 1 1 d . . .
H26 H 0.1620 0.5912 0.4910 0.077 Uiso 1 1 calc R . .
C27 C 0.3233(14) 0.7426(15) 0.5426(9) 0.069(4) Uani 1 1 d . . .
H27 H 0.2662 0.7809 0.5712 0.082 Uiso 1 1 calc R . .
C28 C 0.4703(13) 0.7996(12) 0.5489(7) 0.054(3) Uani 1 1 d . . .
H28 H 0.5104 0.8764 0.5822 0.065 Uiso 1 1 calc R . .
C29 C 0.8448(11) 0.8024(9) 0.8580(7) 0.043(2) Uani 1 1 d . . .
H29 H 0.8737 0.8802 0.8642 0.051 Uiso 1 1 calc R . .
C30 C 0.9427(12) 0.7463(11) 0.8355(8) 0.051(3) Uani 1 1 d . . .
H30 H 1.0342 0.7858 0.8252 0.061 Uiso 1 1 calc R . .
C31 C 0.9029(14) 0.6313(12) 0.8285(8) 0.060(3) Uani 1 1 d . . .
H31 H 0.9673 0.5928 0.8133 0.072 Uiso 1 1 calc R . .
C32 C 0.7672(13) 0.5746(9) 0.8444(7) 0.048(3) Uani 1 1 d . . .
C33 C 0.6704(10) 0.6360(8) 0.8659(6) 0.031(2) Uani 1 1 d . . .
C34 C 0.5304(12) 0.5817(7) 0.8801(6) 0.036(2) Uani 1 1 d . . .
C35 C 0.4821(15) 0.4640(10) 0.8717(10) 0.064(4) Uani 1 1 d . . .
C36 C 0.5782(19) 0.4047(11) 0.8543(12) 0.086(5) Uani 1 1 d . . .
H36 H 0.5498 0.3287 0.8534 0.104 Uiso 1 1 calc R . .
C37 C 0.7085(19) 0.4561(11) 0.8393(10) 0.077(4) Uani 1 1 d . . .
H37 H 0.7673 0.4126 0.8243 0.092 Uiso 1 1 calc R . .
C38 C 0.3405(19) 0.4172(12) 0.8894(13) 0.099(6) Uani 1 1 d U . .
H38 H 0.3048 0.3412 0.8885 0.119 Uiso 1 1 calc R . .
C39 C 0.2553(18) 0.4823(11) 0.9080(11) 0.089(5) Uani 1 1 d . . .
H39 H 0.1588 0.4488 0.9144 0.107 Uiso 1 1 calc R . .
C40 C 0.3134(12) 0.6013(9) 0.9177(7) 0.047(3) Uani 1 1 d . . .
H40 H 0.2583 0.6474 0.9350 0.056 Uiso 1 1 calc R . .
N1 N 0.8828(8) 1.2489(7) 0.9243(5) 0.0313(17) Uani 1 1 d . . .
N2 N 0.8386(9) 1.2496(7) 0.6980(5) 0.039(2) Uani 1 1 d . . .
N3 N 0.7372(8) 0.6556(6) 0.4290(5) 0.0305(17) Uani 1 1 d . . .
N4 N 0.5579(8) 0.7504(7) 0.5097(5) 0.0333(17) Uani 1 1 d . . .
N5 N 0.7110(8) 0.7482(6) 0.8709(5) 0.0281(16) Uani 1 1 d . . .
N6 N 0.4461(8) 0.6450(6) 0.9018(4) 0.0258(15) Uani 1 1 d . . .
Ni1 Ni 0.77690(11) 0.82316(9) 0.50030(7) 0.0232(3) Uani 1 1 d . . .
Ni2 Ni 0.55796(11) 0.81849(8) 0.91627(6) 0.0199(3) Uani 1 1 d . . .
O1 O 0.8207(6) 0.9822(5) 0.6010(3) 0.0262(13) Uani 1 1 d . . .
O2 O 0.8555(7) 0.8368(5) 0.6312(4) 0.0285(13) Uani 1 1 d . . .
O3 O 0.6622(6) 0.8433(5) 1.0360(4) 0.0316(14) Uani 1 1 d . . .
O4 O 0.7240(7) 1.0247(6) 1.1222(4) 0.0370(16) Uani 1 1 d . . .
O5 O 0.9665(10) 1.3234(8) 0.9863(5) 0.078(3) Uani 1 1 d . . .
O6 O 0.7636(8) 1.2447(7) 0.9044(5) 0.056(2) Uani 1 1 d . . .
O7 O 0.9516(9) 1.2727(10) 0.7375(8) 0.100(4) Uani 1 1 d . . .
O8 O 0.8272(10) 1.2979(12) 0.6476(9) 0.127(6) Uani 1 1 d . . .
O9 O 0.6991(7) 0.8545(6) 0.3959(4) 0.0325(15) Uani 1 1 d U . .
O10 O 0.8011(7) 1.0300(6) 0.3859(5) 0.0443(18) Uani 1 1 d . . .
O11 O 0.6614(6) 0.9778(5) 0.8930(3) 0.0245(12) Uani 1 1 d . . .
O12 O 0.4936(6) 0.8355(5) 0.7941(4) 0.0269(13) Uani 1 1 d . . .
O1W O 0.9885(6) 0.8687(5) 0.4789(4) 0.0310(14) Uani 1 1 d . . .
O2W O 0.3898(6) 0.8641(5) 0.9584(4) 0.0303(14) Uani 1 1 d . . .
H1WA H 1.0468 0.9124 0.4553 0.046 Uiso 1 1 d R . .
H1WB H 1.0583 0.9010 0.5226 0.046 Uiso 1 1 d R . .
H2WA H 0.3534 0.8996 0.9324 0.046 Uiso 1 1 d R . .
H2WB H 0.3750 0.9101 1.0020 0.046 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.252(10) . ?
C1 O1 1.267(10) . ?
C1 C2 1.500(11) . ?
C1 Ni1 2.477(8) . ?
C2 C3 1.418(10) . ?
C2 C7 1.418(11) . ?
C3 C4 1.385(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(11) . ?
C4 C15 1.497(10) 2_777 ?
C5 C6 1.380(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.421(10) . ?
C6 N1 1.475(10) . ?
C7 C8 1.475(10) . ?
C8 C9 1.416(11) . ?
C8 C13 1.423(11) . ?
C9 C10 1.375(11) . ?
C9 N2 1.463(11) . ?
C10 C11 1.390(12) . ?
C10 H10 0.9300 . ?
C11 C12 1.357(11) . ?
C11 C16 1.540(11) 2_676 ?
C12 C13 1.388(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.489(10) . ?
C14 O12 1.257(10) . ?
C14 O11 1.271(9) . ?
C14 Ni2 2.483(8) . ?
C15 O3 1.250(10) . ?
C15 O4 1.258(10) . ?
C15 C4 1.497(10) 2_777 ?
C16 O9 1.234(11) . ?
C16 O10 1.236(11) . ?
C16 C11 1.540(11) 2_676 ?
C17 N3 1.309(13) . ?
C17 C18 1.419(14) . ?
C17 H17 0.9300 . ?
C18 C19 1.347(19) . ?
C18 H18 0.9300 . ?
C19 C20 1.39(2) . ?
C19 H19 0.9300 . ?
C20 C21 1.418(15) . ?
C20 C25 1.507(19) . ?
C21 N3 1.357(12) . ?
C21 C22 1.439(15) . ?
C22 N4 1.354(12) . ?
C22 C23 1.414(14) . ?
C23 C26 1.391(19) . ?
C23 C24 1.435(19) . ?
C24 C25 1.29(2) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.35(2) . ?
C26 H26 0.9300 . ?
C27 C28 1.370(17) . ?
C27 H27 0.9300 . ?
C28 N4 1.324(14) . ?
C28 H28 0.9300 . ?
C29 N5 1.333(12) . ?
C29 C30 1.390(15) . ?
C29 H29 0.9300 . ?
C30 C31 1.386(17) . ?
C30 H30 0.9300 . ?
C31 C32 1.375(17) . ?
C31 H31 0.9300 . ?
C32 C33 1.427(13) . ?
C32 C37 1.434(17) . ?
C33 N5 1.357(11) . ?
C33 C34 1.391(14) . ?
C34 N6 1.342(12) . ?
C34 C35 1.409(14) . ?
C35 C36 1.395(18) . ?
C35 C38 1.41(2) . ?
C36 C37 1.31(2) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 C39 1.36(2) . ?
C38 H38 0.9300 . ?
C39 C40 1.421(16) . ?
C39 H39 0.9300 . ?
C40 N6 1.313(13) . ?
C40 H40 0.9300 . ?
N1 O6 1.173(10) . ?
N1 O5 1.217(10) . ?
N2 O7 1.151(11) . ?
N2 O8 1.191(11) . ?
N3 Ni1 2.059(7) . ?
N4 Ni1 2.080(8) . ?
N5 Ni2 2.071(7) . ?
N6 Ni2 2.099(7) . ?
Ni1 O9 2.032(5) . ?
Ni1 O1W 2.044(6) . ?
Ni1 O1 2.151(6) . ?
Ni1 O2 2.182(6) . ?
Ni2 O2W 2.022(6) . ?
Ni2 O3 2.054(6) . ?
Ni2 O11 2.141(6) . ?
Ni2 O12 2.161(6) . ?
O1W H1WA 0.8591 . ?
O1W H1WB 0.8634 . ?
O2W H2WA 0.8498 . ?
O2W H2WB 0.8501 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 121.9(7) . . ?
O2 C1 C2 119.4(7) . . ?
O1 C1 C2 118.5(7) . . ?
O2 C1 Ni1 61.7(4) . . ?
O1 C1 Ni1 60.2(4) . . ?
C2 C1 Ni1 174.5(6) . . ?
C3 C2 C7 120.3(7) . . ?
C3 C2 C1 117.5(7) . . ?
C7 C2 C1 122.2(7) . . ?
C4 C3 C2 120.2(7) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 120.8(7) . . ?
C5 C4 C15 118.9(7) . 2_777 ?
C3 C4 C15 120.2(7) . 2_777 ?
C6 C5 C4 119.1(7) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 123.2(7) . . ?
C5 C6 N1 118.2(7) . . ?
C7 C6 N1 118.6(7) . . ?
C2 C7 C6 116.3(7) . . ?
C2 C7 C8 119.8(6) . . ?
C6 C7 C8 123.8(7) . . ?
C9 C8 C13 115.8(7) . . ?
C9 C8 C7 123.1(7) . . ?
C13 C8 C7 121.1(7) . . ?
C10 C9 C8 122.6(7) . . ?
C10 C9 N2 117.7(7) . . ?
C8 C9 N2 119.8(7) . . ?
C9 C10 C11 119.8(8) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 119.2(7) . . ?
C12 C11 C16 121.9(8) . 2_676 ?
C10 C11 C16 118.8(7) . 2_676 ?
C11 C12 C13 122.4(7) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
C12 C13 C8 120.0(7) . . ?
C12 C13 C14 118.5(7) . . ?
C8 C13 C14 121.5(7) . . ?
O12 C14 O11 120.0(7) . . ?
O12 C14 C13 119.3(7) . . ?
O11 C14 C13 120.7(7) . . ?
O12 C14 Ni2 60.5(4) . . ?
O11 C14 Ni2 59.6(4) . . ?
C13 C14 Ni2 175.0(6) . . ?
O3 C15 O4 127.0(7) . . ?
O3 C15 C4 115.6(7) . 2_777 ?
O4 C15 C4 117.3(7) . 2_777 ?
O9 C16 O10 129.1(8) . . ?
O9 C16 C11 115.4(8) . 2_676 ?
O10 C16 C11 115.5(8) . 2_676 ?
N3 C17 C18 123.5(11) . . ?
N3 C17 H17 118.3 . . ?
C18 C17 H17 118.3 . . ?
C19 C18 C17 118.7(12) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C20 120.4(10) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C21 117.0(11) . . ?
C19 C20 C25 128.6(11) . . ?
C21 C20 C25 114.4(12) . . ?
N3 C21 C20 123.1(11) . . ?
N3 C21 C22 116.0(8) . . ?
C20 C21 C22 120.9(10) . . ?
N4 C22 C23 121.0(10) . . ?
N4 C22 C21 118.1(8) . . ?
C23 C22 C21 120.9(9) . . ?
C26 C23 C22 118.3(11) . . ?
C26 C23 C24 123.7(12) . . ?
C22 C23 C24 117.9(12) . . ?
C25 C24 C23 121.8(12) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C24 C25 C20 124.1(11) . . ?
C24 C25 H25 118.0 . . ?
C20 C25 H25 118.0 . . ?
C27 C26 C23 119.0(11) . . ?
C27 C26 H26 120.5 . . ?
C23 C26 H26 120.5 . . ?
C26 C27 C28 120.1(13) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
N4 C28 C27 123.1(13) . . ?
N4 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
N5 C29 C30 122.1(10) . . ?
N5 C29 H29 119.0 . . ?
C30 C29 H29 119.0 . . ?
C31 C30 C29 119.6(10) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C32 C31 C30 119.3(10) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C31 C32 C33 118.7(10) . . ?
C31 C32 C37 126.4(11) . . ?
C33 C32 C37 114.9(11) . . ?
N5 C33 C34 118.2(8) . . ?
N5 C33 C32 120.9(9) . . ?
C34 C33 C32 120.9(9) . . ?
N6 C34 C33 117.8(8) . . ?
N6 C34 C35 122.4(10) . . ?
C33 C34 C35 119.8(10) . . ?
C36 C35 C38 124.4(12) . . ?
C36 C35 C34 119.6(12) . . ?
C38 C35 C34 115.8(12) . . ?
C37 C36 C35 119.9(12) . . ?
C37 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C36 C37 C32 124.8(12) . . ?
C36 C37 H37 117.6 . . ?
C32 C37 H37 117.6 . . ?
C39 C38 C35 120.6(12) . . ?
C39 C38 H38 119.7 . . ?
C35 C38 H38 119.7 . . ?
C38 C39 C40 120.2(13) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
N6 C40 C39 118.9(12) . . ?
N6 C40 H40 120.6 . . ?
C39 C40 H40 120.6 . . ?
O6 N1 O5 122.6(8) . . ?
O6 N1 C6 121.1(7) . . ?
O5 N1 C6 116.3(7) . . ?
O7 N2 O8 119.4(9) . . ?
O7 N2 C9 122.5(8) . . ?
O8 N2 C9 118.1(8) . . ?
C17 N3 C21 117.3(8) . . ?
C17 N3 Ni1 129.2(7) . . ?
C21 N3 Ni1 113.4(7) . . ?
C28 N4 C22 118.5(9) . . ?
C28 N4 Ni1 129.6(8) . . ?
C22 N4 Ni1 111.5(6) . . ?
C29 N5 C33 119.4(8) . . ?
C29 N5 Ni2 127.9(7) . . ?
C33 N5 Ni2 112.0(6) . . ?
C40 N6 C34 122.0(8) . . ?
C40 N6 Ni2 125.8(7) . . ?
C34 N6 Ni2 112.0(6) . . ?
O9 Ni1 O1W 94.7(3) . . ?
O9 Ni1 N3 90.9(3) . . ?
O1W Ni1 N3 90.3(3) . . ?
O9 Ni1 N4 85.2(3) . . ?
O1W Ni1 N4 170.8(3) . . ?
N3 Ni1 N4 80.5(3) . . ?
O9 Ni1 O1 102.6(2) . . ?
O1W Ni1 O1 92.8(2) . . ?
N3 Ni1 O1 165.9(3) . . ?
N4 Ni1 O1 96.3(3) . . ?
O9 Ni1 O2 163.5(2) . . ?
O1W Ni1 O2 88.9(2) . . ?
N3 Ni1 O2 105.2(3) . . ?
N4 Ni1 O2 93.8(3) . . ?
O1 Ni1 O2 61.1(2) . . ?
O9 Ni1 C1 133.3(3) . . ?
O1W Ni1 C1 90.5(2) . . ?
N3 Ni1 C1 135.5(3) . . ?
N4 Ni1 C1 96.3(3) . . ?
O1 Ni1 C1 30.8(2) . . ?
O2 Ni1 C1 30.3(2) . . ?
O2W Ni2 O3 95.3(3) . . ?
O2W Ni2 N5 171.9(3) . . ?
O3 Ni2 N5 85.3(3) . . ?
O2W Ni2 N6 92.6(3) . . ?
O3 Ni2 N6 90.6(3) . . ?
N5 Ni2 N6 79.3(3) . . ?
O2W Ni2 O11 92.9(2) . . ?
O3 Ni2 O11 103.7(2) . . ?
N5 Ni2 O11 94.9(3) . . ?
N6 Ni2 O11 164.1(2) . . ?
O2W Ni2 O12 88.3(2) . . ?
O3 Ni2 O12 164.7(2) . . ?
N5 Ni2 O12 93.3(3) . . ?
N6 Ni2 O12 104.1(2) . . ?
O11 Ni2 O12 61.2(2) . . ?
O2W Ni2 C14 89.9(3) . . ?
O3 Ni2 C14 134.5(3) . . ?
N5 Ni2 C14 95.5(3) . . ?
N6 Ni2 C14 134.3(3) . . ?
O11 Ni2 C14 30.8(2) . . ?
O12 Ni2 C14 30.4(2) . . ?
C1 O1 Ni1 89.0(5) . . ?
C1 O2 Ni1 88.0(5) . . ?
C15 O3 Ni2 133.6(5) . . ?
C16 O9 Ni1 138.6(6) . . ?
C14 O11 Ni2 89.6(5) . . ?
C14 O12 Ni2 89.2(4) . . ?
Ni1 O1W H1WA 139.9 . . ?
Ni1 O1W H1WB 118.6 . . ?
H1WA O1W H1WB 84.7 . . ?
Ni2 O2W H2WA 119.0 . . ?
Ni2 O2W H2WB 138.2 . . ?
H2WA O2W H2WB 81.8 . . ?

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
O2 C1 C2 C3 41.4(11) . . . . ?
O1 C1 C2 C3 -134.2(8) . . . . ?
O2 C1 C2 C7 -139.0(8) . . . . ?
O1 C1 C2 C7 45.4(11) . . . . ?
C7 C2 C3 C4 -4.0(11) . . . . ?
C1 C2 C3 C4 175.7(7) . . . . ?
C2 C3 C4 C5 1.6(12) . . . . ?
C2 C3 C4 C15 178.6(7) . . . 2_777 ?
C3 C4 C5 C6 0.6(12) . . . . ?
C15 C4 C5 C6 -176.4(7) 2_777 . . . ?
C4 C5 C6 C7 -0.6(12) . . . . ?
C4 C5 C6 N1 -178.8(7) . . . . ?
C3 C2 C7 C6 3.9(11) . . . . ?
C1 C2 C7 C6 -175.8(7) . . . . ?
C3 C2 C7 C8 -173.8(7) . . . . ?
C1 C2 C7 C8 6.5(11) . . . . ?
C5 C6 C7 C2 -1.7(11) . . . . ?
N1 C6 C7 C2 176.5(7) . . . . ?
C5 C6 C7 C8 175.9(7) . . . . ?
N1 C6 C7 C8 -5.9(11) . . . . ?
C2 C7 C8 C9 -93.4(9) . . . . ?
C6 C7 C8 C9 89.1(10) . . . . ?
C2 C7 C8 C13 85.3(9) . . . . ?
C6 C7 C8 C13 -92.2(9) . . . . ?
C13 C8 C9 C10 -3.2(12) . . . . ?
C7 C8 C9 C10 175.5(8) . . . . ?
C13 C8 C9 N2 176.2(7) . . . . ?
C7 C8 C9 N2 -5.0(12) . . . . ?
C8 C9 C10 C11 0.9(13) . . . . ?
N2 C9 C10 C11 -178.5(8) . . . . ?
C9 C10 C11 C12 -0.1(12) . . . . ?
C9 C10 C11 C16 -175.6(8) . . . 2_676 ?
C10 C11 C12 C13 1.9(12) . . . . ?
C16 C11 C12 C13 177.2(7) 2_676 . . . ?
C11 C12 C13 C8 -4.3(12) . . . . ?
C11 C12 C13 C14 175.1(7) . . . . ?
C9 C8 C13 C12 4.8(11) . . . . ?
C7 C8 C13 C12 -174.0(7) . . . . ?
C9 C8 C13 C14 -174.6(7) . . . . ?
C7 C8 C13 C14 6.6(11) . . . . ?
C12 C13 C14 O12 40.7(11) . . . . ?
C8 C13 C14 O12 -139.8(8) . . . . ?
C12 C13 C14 O11 -136.0(8) . . . . ?
C8 C13 C14 O11 43.4(11) . . . . ?
N3 C17 C18 C19 -1.5(18) . . . . ?
C17 C18 C19 C20 0.0(19) . . . . ?
C18 C19 C20 C21 0.9(17) . . . . ?
C18 C19 C20 C25 178.7(11) . . . . ?
C19 C20 C21 N3 -0.4(16) . . . . ?
C25 C20 C21 N3 -178.5(9) . . . . ?
C19 C20 C21 C22 177.9(10) . . . . ?
C25 C20 C21 C22 -0.2(14) . . . . ?
N3 C21 C22 N4 -1.7(13) . . . . ?
C20 C21 C22 N4 179.9(9) . . . . ?
N3 C21 C22 C23 -179.9(8) . . . . ?
C20 C21 C22 C23 1.7(14) . . . . ?
N4 C22 C23 C26 1.4(14) . . . . ?
C21 C22 C23 C26 179.6(9) . . . . ?
N4 C22 C23 C24 -178.9(9) . . . . ?
C21 C22 C23 C24 -0.7(14) . . . . ?
C26 C23 C24 C25 177.8(12) . . . . ?
C22 C23 C24 C25 -1.9(17) . . . . ?
C23 C24 C25 C20 4(2) . . . . ?
C19 C20 C25 C24 179.7(13) . . . . ?
C21 C20 C25 C24 -2.4(17) . . . . ?
C22 C23 C26 C27 0.3(17) . . . . ?
C24 C23 C26 C27 -179.4(12) . . . . ?
C23 C26 C27 C28 -1.0(19) . . . . ?
C26 C27 C28 N4 0(2) . . . . ?
N5 C29 C30 C31 -2.0(17) . . . . ?
C29 C30 C31 C32 -0.3(18) . . . . ?
C30 C31 C32 C33 1.2(18) . . . . ?
C30 C31 C32 C37 179.4(13) . . . . ?
C31 C32 C33 N5 -0.1(16) . . . . ?
C37 C32 C33 N5 -178.5(10) . . . . ?
C31 C32 C33 C34 178.1(11) . . . . ?
C37 C32 C33 C34 -0.3(15) . . . . ?
N5 C33 C34 N6 -3.1(13) . . . . ?
C32 C33 C34 N6 178.7(9) . . . . ?
N5 C33 C34 C35 177.2(10) . . . . ?
C32 C33 C34 C35 -1.0(15) . . . . ?
N6 C34 C35 C36 -175.9(13) . . . . ?
C33 C34 C35 C36 4(2) . . . . ?
N6 C34 C35 C38 -1(2) . . . . ?
C33 C34 C35 C38 178.4(14) . . . . ?
C38 C35 C36 C37 -179.4(19) . . . . ?
C34 C35 C36 C37 -5(3) . . . . ?
C35 C36 C37 C32 4(3) . . . . ?
C31 C32 C37 C36 -179.5(17) . . . . ?
C33 C32 C37 C36 -1(2) . . . . ?
C36 C35 C38 C39 178.2(18) . . . . ?
C34 C35 C38 C39 4(3) . . . . ?
C35 C38 C39 C40 -6(3) . . . . ?
C38 C39 C40 N6 5(2) . . . . ?
C5 C6 N1 O6 -167.1(9) . . . . ?
C7 C6 N1 O6 14.6(12) . . . . ?
C5 C6 N1 O5 12.8(12) . . . . ?
C7 C6 N1 O5 -165.5(9) . . . . ?
C10 C9 N2 O7 169.1(12) . . . . ?
C8 C9 N2 O7 -10.4(16) . . . . ?
C10 C9 N2 O8 -11.2(16) . . . . ?
C8 C9 N2 O8 169.4(12) . . . . ?
C18 C17 N3 C21 2.0(15) . . . . ?
C18 C17 N3 Ni1 -172.6(8) . . . . ?
C20 C21 N3 C17 -1.0(14) . . . . ?
C22 C21 N3 C17 -179.4(9) . . . . ?
C20 C21 N3 Ni1 174.4(8) . . . . ?
C22 C21 N3 Ni1 -4.0(10) . . . . ?
C27 C28 N4 C22 1.4(16) . . . . ?
C27 C28 N4 Ni1 173.3(9) . . . . ?
C23 C22 N4 C28 -2.2(13) . . . . ?
C21 C22 N4 C28 179.6(9) . . . . ?
C23 C22 N4 Ni1 -175.5(7) . . . . ?
C21 C22 N4 Ni1 6.3(10) . . . . ?
C30 C29 N5 C33 3.1(15) . . . . ?
C30 C29 N5 Ni2 173.3(8) . . . . ?
C34 C33 N5 C29 179.7(9) . . . . ?
C32 C33 N5 C29 -2.0(14) . . . . ?
C34 C33 N5 Ni2 8.1(10) . . . . ?
C32 C33 N5 Ni2 -173.7(8) . . . . ?
C39 C40 N6 C34 -2.7(17) . . . . ?
C39 C40 N6 Ni2 -177.4(10) . . . . ?
C33 C34 N6 C40 -178.9(9) . . . . ?
C35 C34 N6 C40 0.8(15) . . . . ?
C33 C34 N6 Ni2 -3.5(10) . . . . ?
C35 C34 N6 Ni2 176.2(9) . . . . ?
C17 N3 Ni1 O9 95.3(9) . . . . ?
C21 N3 Ni1 O9 -79.4(6) . . . . ?
C17 N3 Ni1 O1W 0.6(9) . . . . ?
C21 N3 Ni1 O1W -174.1(6) . . . . ?
C17 N3 Ni1 N4 -179.7(9) . . . . ?
C21 N3 Ni1 N4 5.6(6) . . . . ?
C17 N3 Ni1 O1 -102.0(14) . . . . ?
C21 N3 Ni1 O1 83.3(13) . . . . ?
C17 N3 Ni1 O2 -88.3(9) . . . . ?
C21 N3 Ni1 O2 97.0(6) . . . . ?
C17 N3 Ni1 C1 -90.4(9) . . . . ?
C21 N3 Ni1 C1 94.9(7) . . . . ?
C28 N4 Ni1 O9 -87.0(9) . . . . ?
C22 N4 Ni1 O9 85.4(6) . . . . ?
C28 N4 Ni1 N3 -178.7(9) . . . . ?
C22 N4 Ni1 N3 -6.4(6) . . . . ?
C28 N4 Ni1 O1 15.2(9) . . . . ?
C22 N4 Ni1 O1 -172.5(6) . . . . ?
C28 N4 Ni1 O2 76.5(9) . . . . ?
C22 N4 Ni1 O2 -111.1(6) . . . . ?
C28 N4 Ni1 C1 46.2(9) . . . . ?
C22 N4 Ni1 C1 -141.5(6) . . . . ?
O2 C1 Ni1 O9 176.1(4) . . . . ?
O1 C1 Ni1 O9 -2.3(6) . . . . ?
O2 C1 Ni1 O1W -87.0(5) . . . . ?
O1 C1 Ni1 O1W 94.6(5) . . . . ?
O2 C1 Ni1 N3 3.9(7) . . . . ?
O1 C1 Ni1 N3 -174.5(5) . . . . ?
O2 C1 Ni1 N4 86.7(5) . . . . ?
O1 C1 Ni1 N4 -91.7(5) . . . . ?
O2 C1 Ni1 O1 178.4(8) . . . . ?
O1 C1 Ni1 O2 -178.4(8) . . . . ?
C29 N5 Ni2 O3 -86.6(8) . . . . ?
C33 N5 Ni2 O3 84.2(6) . . . . ?
C29 N5 Ni2 N6 -178.1(9) . . . . ?
C33 N5 Ni2 N6 -7.4(6) . . . . ?
C29 N5 Ni2 O11 16.8(8) . . . . ?
C33 N5 Ni2 O11 -172.4(6) . . . . ?
C29 N5 Ni2 O12 78.1(8) . . . . ?
C33 N5 Ni2 O12 -111.1(6) . . . . ?
C29 N5 Ni2 C14 47.7(9) . . . . ?
C33 N5 Ni2 C14 -141.5(6) . . . . ?
C40 N6 Ni2 O2W 0.6(8) . . . . ?
C34 N6 Ni2 O2W -174.5(6) . . . . ?
C40 N6 Ni2 O3 96.0(8) . . . . ?
C34 N6 Ni2 O3 -79.2(6) . . . . ?
C40 N6 Ni2 N5 -178.9(9) . . . . ?
C34 N6 Ni2 N5 5.9(6) . . . . ?
C40 N6 Ni2 O11 -109.3(11) . . . . ?
C34 N6 Ni2 O11 75.6(11) . . . . ?
C40 N6 Ni2 O12 -88.2(8) . . . . ?
C34 N6 Ni2 O12 96.6(6) . . . . ?
C40 N6 Ni2 C14 -91.8(9) . . . . ?
C34 N6 Ni2 C14 93.0(7) . . . . ?
O12 C14 Ni2 O2W -86.7(5) . . . . ?
O11 C14 Ni2 O2W 95.7(5) . . . . ?
O12 C14 Ni2 O3 175.9(4) . . . . ?
O11 C14 Ni2 O3 -1.6(6) . . . . ?
O12 C14 Ni2 N5 87.1(5) . . . . ?
O11 C14 Ni2 N5 -90.4(5) . . . . ?
O12 C14 Ni2 N6 6.8(6) . . . . ?
O11 C14 Ni2 N6 -170.7(4) . . . . ?
O12 C14 Ni2 O11 177.5(7) . . . . ?
O11 C14 Ni2 O12 -177.5(7) . . . . ?
O2 C1 O1 Ni1 -1.7(8) . . . . ?
C2 C1 O1 Ni1 173.8(6) . . . . ?
O9 Ni1 O1 C1 178.3(5) . . . . ?
O1W Ni1 O1 C1 -86.3(5) . . . . ?
N3 Ni1 O1 C1 16.1(13) . . . . ?
N4 Ni1 O1 C1 91.8(5) . . . . ?
O2 Ni1 O1 C1 0.9(4) . . . . ?
O1 C1 O2 Ni1 1.6(8) . . . . ?
C2 C1 O2 Ni1 -173.8(6) . . . . ?
O9 Ni1 O2 C1 -10.1(11) . . . . ?
O1W Ni1 O2 C1 92.8(5) . . . . ?
N3 Ni1 O2 C1 -177.1(5) . . . . ?
N4 Ni1 O2 C1 -96.0(5) . . . . ?
O1 Ni1 O2 C1 -0.9(4) . . . . ?
O4 C15 O3 Ni2 42.6(13) . . . . ?
C4 C15 O3 Ni2 -135.2(6) 2_777 . . . ?
O2W Ni2 O3 C15 -78.8(8) . . . . ?
N5 Ni2 O3 C15 109.4(8) . . . . ?
N6 Ni2 O3 C15 -171.5(8) . . . . ?
O11 Ni2 O3 C15 15.4(8) . . . . ?
O12 Ni2 O3 C15 24.2(14) . . . . ?
C14 Ni2 O3 C15 16.3(9) . . . . ?
O10 C16 O9 Ni1 40.4(15) . . . . ?
C11 C16 O9 Ni1 -138.3(7) 2_676 . . . ?
O1W Ni1 O9 C16 -75.0(9) . . . . ?
N3 Ni1 O9 C16 -165.3(9) . . . . ?
N4 Ni1 O9 C16 114.3(9) . . . . ?
O1 Ni1 O9 C16 18.9(9) . . . . ?
O2 Ni1 O9 C16 27.2(15) . . . . ?
C1 Ni1 O9 C16 20.2(11) . . . . ?
O12 C14 O11 Ni2 -2.5(8) . . . . ?
C13 C14 O11 Ni2 174.2(6) . . . . ?
O2W Ni2 O11 C14 -85.0(5) . . . . ?
O3 Ni2 O11 C14 178.8(4) . . . . ?
N5 Ni2 O11 C14 92.5(5) . . . . ?
N6 Ni2 O11 C14 24.8(11) . . . . ?
O12 Ni2 O11 C14 1.4(4) . . . . ?
O11 C14 O12 Ni2 2.5(7) . . . . ?
C13 C14 O12 Ni2 -174.3(6) . . . . ?
O2W Ni2 O12 C14 92.8(5) . . . . ?
O3 Ni2 O12 C14 -11.1(12) . . . . ?
N5 Ni2 O12 C14 -95.2(5) . . . . ?
N6 Ni2 O12 C14 -175.0(5) . . . . ?
O11 Ni2 O12 C14 -1.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         1.356
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.261
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1444257'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H22 Co N6 O14'
_chemical_formula_weight         869.57

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   10.059(2)
_cell_length_b                   11.605(3)
_cell_length_c                   16.860(4)
_cell_angle_alpha                77.458(4)
_cell_angle_beta                 79.847(4)
_cell_angle_gamma                79.381(4)
_cell_volume                     1869.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2656
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      23.92

_exptl_crystal_description       columnar
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             886
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9479
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9712
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6807
_reflns_number_gt                4920
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+10.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6807
_refine_ls_number_parameters     552
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0786
_refine_ls_wR_factor_ref         0.3123
_refine_ls_wR_factor_gt          0.2095
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.971
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.71465(8) 0.54886(7) 0.72914(5) 0.0284(3) Uani 1 1 d . . .
O9 O 0.8912(4) 0.4232(4) 0.7108(3) 0.0332(10) Uani 1 1 d . . .
O3 O 0.5713(5) 0.4356(4) 0.7432(3) 0.0351(10) Uani 1 1 d . . .
O4 O 0.8188(5) 0.3600(5) 0.3585(3) 0.0502(14) Uani 1 1 d . . .
H4 H 0.7954 0.3871 0.3131 0.075 Uiso 1 1 calc R . .
N4 N 0.7052(6) 0.5007(5) 0.8614(3) 0.0348(12) Uani 1 1 d . . .
C34 C 0.6514(6) 0.3621(5) 0.5657(4) 0.0288(13) Uani 1 1 d . . .
H34 H 0.5721 0.4147 0.5551 0.035 Uiso 1 1 calc R . .
N3 N 0.8314(5) 0.6700(5) 0.7564(3) 0.0343(12) Uani 1 1 d . . .
C30 C 0.7905(6) 0.2365(5) 0.6642(4) 0.0277(13) Uani 1 1 d . . .
C52 C 0.9486(6) 0.3395(5) 0.7592(4) 0.0303(13) Uani 1 1 d . . .
C33 C 0.7477(6) 0.3332(5) 0.5006(4) 0.0266(12) Uani 1 1 d . . .
C19 C 0.8444(7) 0.6543(6) 0.8371(4) 0.0391(15) Uani 1 1 d . . .
N1 N 0.7296(5) 0.6154(4) 0.5988(3) 0.0282(11) Uani 1 1 d . . .
N6 N 1.0147(6) 0.1269(5) 0.6078(4) 0.0428(14) Uani 1 1 d . . .
C48 C 0.8752(6) 0.2332(5) 0.7981(4) 0.0271(12) Uani 1 1 d . . .
O10 O 1.0627(6) 0.3349(5) 0.7786(4) 0.0596(16) Uani 1 1 d . . .
O2W O 0.2356(6) 0.4953(5) 0.7788(3) 0.0515(13) Uani 1 1 d . . .
N2 N 0.5493(5) 0.6964(5) 0.7190(4) 0.0354(12) Uani 1 1 d . . .
C5 C 0.6259(6) 0.7034(5) 0.5771(4) 0.0302(13) Uani 1 1 d . . .
C13 C 0.5296(6) 0.7470(6) 0.6427(4) 0.0354(15) Uani 1 1 d . . .
C1 C 0.8223(7) 0.5791(6) 0.5389(4) 0.0364(14) Uani 1 1 d . . .
H1 H 0.8951 0.5205 0.5533 0.044 Uiso 1 1 calc R . .
C4 C 0.6110(8) 0.7542(6) 0.4950(4) 0.0412(16) Uani 1 1 d . . .
C2 C 0.8159(8) 0.6242(7) 0.4556(4) 0.0462(18) Uani 1 1 d . . .
H2 H 0.8826 0.5956 0.4159 0.055 Uiso 1 1 calc R . .
C8 C 0.4218(7) 0.8405(6) 0.6237(6) 0.0469(19) Uani 1 1 d . . .
C3 C 0.7100(9) 0.7112(7) 0.4331(4) 0.0483(19) Uani 1 1 d . . .
H3 H 0.7032 0.7417 0.3780 0.058 Uiso 1 1 calc R . .
C11 C 0.4626(8) 0.7338(8) 0.7817(6) 0.054(2) Uani 1 1 d . . .
H11 H 0.4727 0.6959 0.8353 0.064 Uiso 1 1 calc R . .
C9 C 0.3356(8) 0.8804(7) 0.6903(8) 0.064(3) Uani 1 1 d . . .
H9 H 0.2635 0.9423 0.6811 0.077 Uiso 1 1 calc R . .
C6 C 0.4974(10) 0.8475(7) 0.4773(6) 0.056(2) Uani 1 1 d . . .
H6 H 0.4862 0.8813 0.4231 0.067 Uiso 1 1 calc R . .
C7 C 0.4093(10) 0.8849(7) 0.5381(7) 0.065(3) Uani 1 1 d . . .
H7 H 0.3353 0.9428 0.5249 0.078 Uiso 1 1 calc R . .
C10 C 0.3569(8) 0.8294(9) 0.7669(7) 0.067(3) Uani 1 1 d . . .
H10 H 0.3010 0.8577 0.8109 0.080 Uiso 1 1 calc R . .
C23 C 0.7792(7) 0.5654(7) 0.8923(4) 0.0405(16) Uani 1 1 d . . .
C16 C 0.9666(8) 0.8260(7) 0.7264(6) 0.0499(19) Uani 1 1 d . . .
H16 H 1.0083 0.8831 0.6873 0.060 Uiso 1 1 calc R . .
C25 C 0.6458(8) 0.4172(7) 0.9123(4) 0.0455(17) Uani 1 1 d . . .
H25 H 0.5955 0.3739 0.8915 0.055 Uiso 1 1 calc R . .
C18 C 0.9158(8) 0.7258(8) 0.8661(5) 0.051(2) Uani 1 1 d . . .
C15 C 0.8918(8) 0.7543(7) 0.7036(5) 0.0452(17) Uani 1 1 d . . .
H15 H 0.8828 0.7653 0.6484 0.054 Uiso 1 1 calc R . .
C26 C 0.6536(9) 0.3896(8) 0.9963(5) 0.057(2) Uani 1 1 d . . .
H26 H 0.6102 0.3287 1.0301 0.068 Uiso 1 1 calc R . .
C17 C 0.9788(9) 0.8122(8) 0.8063(6) 0.059(2) Uani 1 1 d . . .
H17 H 1.0294 0.8604 0.8224 0.071 Uiso 1 1 calc R . .
C22 C 0.7866(9) 0.5440(8) 0.9764(5) 0.054(2) Uani 1 1 d . . .
C27 C 0.7267(10) 0.4537(9) 1.0288(5) 0.065(2) Uani 1 1 d . . .
H27 H 0.7350 0.4362 1.0844 0.078 Uiso 1 1 calc R . .
C21 C 0.8648(11) 0.6197(12) 1.0024(7) 0.080(3) Uani 1 1 d . . .
H21 H 0.8728 0.6080 1.0578 0.096 Uiso 1 1 calc R . .
C20 C 0.9250(10) 0.7046(10) 0.9505(6) 0.066(2) Uani 1 1 d . . .
H20 H 0.9739 0.7505 0.9701 0.079 Uiso 1 1 calc R . .
O1 O 0.4708(6) 0.2855(6) 0.7383(4) 0.0598(16) Uani 1 1 d . . .
O2 O 0.6110(5) 0.4509(5) 0.4014(3) 0.0494(13) Uani 1 1 d . . .
C29 C 0.6710(6) 0.3143(5) 0.6459(4) 0.0261(12) Uani 1 1 d . . .
C37 C 0.5626(6) 0.3466(6) 0.7149(3) 0.0280(13) Uani 1 1 d . . .
C32 C 0.8667(6) 0.2571(6) 0.5162(4) 0.0311(13) Uani 1 1 d . . .
H32 H 0.9322 0.2373 0.4730 0.037 Uiso 1 1 calc R . .
C31 C 0.8879(6) 0.2105(5) 0.5962(4) 0.0309(13) Uani 1 1 d . . .
C35 C 0.7177(6) 0.3887(6) 0.4157(4) 0.0311(13) Uani 1 1 d . . .
O12 O 1.0549(6) 0.1055(6) 0.6738(3) 0.0617(17) Uani 1 1 d . . .
O11 O 1.0776(8) 0.0841(7) 0.5498(5) 0.095(3) Uani 1 1 d . . .
C40 C 0.8048(6) 0.1835(5) 0.7517(4) 0.0289(13) Uani 1 1 d . . .
C47 C 0.8787(7) 0.1836(6) 0.8814(4) 0.0331(14) Uani 1 1 d . . .
H47 H 0.9286 0.2150 0.9109 0.040 Uiso 1 1 calc R . .
O8 O 0.8661(7) 0.0914(6) 1.0524(3) 0.0609(16) Uani 1 1 d . . .
C41 C 0.7384(7) 0.0852(6) 0.7938(4) 0.0355(14) Uani 1 1 d . . .
C42 C 0.7400(7) 0.0418(6) 0.8768(4) 0.0410(16) Uani 1 1 d . . .
H42 H 0.6928 -0.0209 0.9034 0.049 Uiso 1 1 calc R . .
O7 O 0.7453(8) -0.0435(6) 1.0409(3) 0.0680(19) Uani 1 1 d . . .
H7A H 0.7371 -0.0570 1.0911 0.102 Uiso 1 1 calc R . .
C46 C 0.8118(7) 0.0915(6) 0.9202(4) 0.0357(15) Uani 1 1 d . . .
C49 C 0.8117(8) 0.0469(6) 1.0114(4) 0.0410(16) Uani 1 1 d . . .
O5 O 0.7079(8) 0.0255(6) 0.6766(4) 0.075(2) Uani 1 1 d . . .
O1W O 0.7352(6) 0.8607(5) 0.1941(4) 0.0596(15) Uani 1 1 d . . .
N5 N 0.6715(8) 0.0243(7) 0.7496(5) 0.063(2) Uani 1 1 d . . .
O17 O 0.5775(11) -0.0259(10) 0.7894(7) 0.117(3) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O3 2.076(5) . ?
Co1 O9 2.104(4) . ?
Co1 N1 2.154(5) . ?
Co1 N3 2.155(5) . ?
Co1 N2 2.156(5) . ?
Co1 N4 2.168(5) . ?
O9 C52 1.248(7) . ?
O3 C37 1.250(8) . ?
O4 C35 1.321(8) . ?
O4 H4 0.8200 . ?
N4 C25 1.305(9) . ?
N4 C23 1.379(9) . ?
C34 C29 1.379(8) . ?
C34 C33 1.385(9) . ?
C34 H34 0.9300 . ?
N3 C15 1.331(9) . ?
N3 C19 1.360(9) . ?
C30 C29 1.402(8) . ?
C30 C31 1.419(9) . ?
C30 C40 1.491(8) . ?
C52 O10 1.237(8) . ?
C52 C48 1.520(8) . ?
C33 C32 1.379(8) . ?
C33 C35 1.495(8) . ?
C19 C18 1.401(10) . ?
C19 C23 1.406(10) . ?
N1 C1 1.332(9) . ?
N1 C5 1.359(8) . ?
N6 O12 1.211(8) . ?
N6 O11 1.217(9) . ?
N6 C31 1.469(8) . ?
C48 C47 1.401(9) . ?
C48 C40 1.410(9) . ?
N2 C13 1.325(9) . ?
N2 C11 1.343(9) . ?
C5 C4 1.404(9) . ?
C5 C13 1.451(9) . ?
C13 C8 1.411(9) . ?
C1 C2 1.397(10) . ?
C1 H1 0.9300 . ?
C4 C3 1.416(12) . ?
C4 C6 1.445(11) . ?
C2 C3 1.371(12) . ?
C2 H2 0.9300 . ?
C8 C9 1.400(13) . ?
C8 C7 1.443(14) . ?
C3 H3 0.9300 . ?
C11 C10 1.401(12) . ?
C11 H11 0.9300 . ?
C9 C10 1.336(15) . ?
C9 H9 0.9300 . ?
C6 C7 1.326(14) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C10 H10 0.9300 . ?
C23 C22 1.399(10) . ?
C16 C17 1.347(13) . ?
C16 C15 1.370(11) . ?
C16 H16 0.9300 . ?
C25 C26 1.395(11) . ?
C25 H25 0.9300 . ?
C18 C20 1.406(13) . ?
C18 C17 1.412(13) . ?
C15 H15 0.9300 . ?
C26 C27 1.384(14) . ?
C26 H26 0.9300 . ?
C17 H17 0.9300 . ?
C22 C27 1.373(13) . ?
C22 C21 1.458(14) . ?
C27 H27 0.9300 . ?
C21 C20 1.327(15) . ?
C21 H21 0.9300 . ?
C20 H20 0.9300 . ?
O1 C37 1.225(8) . ?
O2 C35 1.208(8) . ?
C29 C37 1.508(8) . ?
C32 C31 1.377(9) . ?
C32 H32 0.9300 . ?
C40 C41 1.418(9) . ?
C47 C46 1.353(9) . ?
C47 H47 0.9300 . ?
O8 C49 1.199(9) . ?
C41 C42 1.382(10) . ?
C41 N5 1.445(10) . ?
C42 C46 1.384(10) . ?
C42 H42 0.9300 . ?
O7 C49 1.307(9) . ?
O7 H7A 0.8200 . ?
C46 C49 1.512(9) . ?
O5 N5 1.219(10) . ?
N5 O17 1.222(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O9 97.81(18) . . ?
O3 Co1 N1 99.82(19) . . ?
O9 Co1 N1 90.25(18) . . ?
O3 Co1 N3 160.5(2) . . ?
O9 Co1 N3 91.54(19) . . ?
N1 Co1 N3 97.2(2) . . ?
O3 Co1 N2 87.9(2) . . ?
O9 Co1 N2 166.7(2) . . ?
N1 Co1 N2 76.9(2) . . ?
N3 Co1 N2 86.8(2) . . ?
O3 Co1 N4 85.7(2) . . ?
O9 Co1 N4 92.07(19) . . ?
N1 Co1 N4 173.6(2) . . ?
N3 Co1 N4 76.9(2) . . ?
N2 Co1 N4 100.4(2) . . ?
C52 O9 Co1 131.7(4) . . ?
C37 O3 Co1 136.0(4) . . ?
C35 O4 H4 109.5 . . ?
C25 N4 C23 118.3(6) . . ?
C25 N4 Co1 128.7(5) . . ?
C23 N4 Co1 112.9(4) . . ?
C29 C34 C33 121.3(5) . . ?
C29 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C15 N3 C19 118.3(6) . . ?
C15 N3 Co1 127.4(5) . . ?
C19 N3 Co1 114.3(4) . . ?
C29 C30 C31 116.2(5) . . ?
C29 C30 C40 119.1(5) . . ?
C31 C30 C40 124.6(5) . . ?
O10 C52 O9 125.2(6) . . ?
O10 C52 C48 116.1(5) . . ?
O9 C52 C48 118.7(5) . . ?
C32 C33 C34 119.5(6) . . ?
C32 C33 C35 122.9(6) . . ?
C34 C33 C35 117.6(5) . . ?
N3 C19 C18 122.2(7) . . ?
N3 C19 C23 117.6(6) . . ?
C18 C19 C23 120.2(7) . . ?
C1 N1 C5 117.7(5) . . ?
C1 N1 Co1 128.8(4) . . ?
C5 N1 Co1 113.4(4) . . ?
O12 N6 O11 122.4(6) . . ?
O12 N6 C31 119.0(6) . . ?
O11 N6 C31 118.6(6) . . ?
C47 C48 C40 119.7(6) . . ?
C47 C48 C52 119.2(5) . . ?
C40 C48 C52 121.1(5) . . ?
C13 N2 C11 119.2(6) . . ?
C13 N2 Co1 114.8(4) . . ?
C11 N2 Co1 125.9(5) . . ?
N1 C5 C4 122.8(6) . . ?
N1 C5 C13 117.4(5) . . ?
C4 C5 C13 119.8(6) . . ?
N2 C13 C8 123.1(7) . . ?
N2 C13 C5 117.1(6) . . ?
C8 C13 C5 119.8(7) . . ?
N1 C1 C2 123.5(6) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C5 C4 C3 117.7(6) . . ?
C5 C4 C6 119.3(8) . . ?
C3 C4 C6 123.1(7) . . ?
C3 C2 C1 119.2(7) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C9 C8 C13 116.6(8) . . ?
C9 C8 C7 126.0(8) . . ?
C13 C8 C7 117.4(8) . . ?
C2 C3 C4 119.1(6) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
N2 C11 C10 120.5(9) . . ?
N2 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C10 C9 C8 119.9(7) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C7 C6 C4 120.1(8) . . ?
C7 C6 H6 120.0 . . ?
C4 C6 H6 120.0 . . ?
C6 C7 C8 123.6(7) . . ?
C6 C7 H7 118.2 . . ?
C8 C7 H7 118.2 . . ?
C9 C10 C11 120.7(8) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
N4 C23 C22 120.5(7) . . ?
N4 C23 C19 118.2(6) . . ?
C22 C23 C19 121.3(7) . . ?
C17 C16 C15 118.9(8) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
N4 C25 C26 123.5(8) . . ?
N4 C25 H25 118.3 . . ?
C26 C25 H25 118.3 . . ?
C19 C18 C20 119.0(8) . . ?
C19 C18 C17 116.3(8) . . ?
C20 C18 C17 124.6(8) . . ?
N3 C15 C16 123.4(8) . . ?
N3 C15 H15 118.3 . . ?
C16 C15 H15 118.3 . . ?
C27 C26 C25 119.3(8) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C16 C17 C18 121.0(7) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C27 C22 C23 120.4(8) . . ?
C27 C22 C21 123.8(8) . . ?
C23 C22 C21 115.8(9) . . ?
C22 C27 C26 117.9(7) . . ?
C22 C27 H27 121.1 . . ?
C26 C27 H27 121.1 . . ?
C20 C21 C22 122.9(9) . . ?
C20 C21 H21 118.5 . . ?
C22 C21 H21 118.5 . . ?
C21 C20 C18 120.7(8) . . ?
C21 C20 H20 119.6 . . ?
C18 C20 H20 119.6 . . ?
C34 C29 C30 121.0(6) . . ?
C34 C29 C37 119.6(5) . . ?
C30 C29 C37 119.5(5) . . ?
O1 C37 O3 124.5(6) . . ?
O1 C37 C29 118.0(6) . . ?
O3 C37 C29 117.5(5) . . ?
C31 C32 C33 119.6(6) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C32 C31 C30 122.5(5) . . ?
C32 C31 N6 116.4(6) . . ?
C30 C31 N6 121.1(5) . . ?
O2 C35 O4 124.0(6) . . ?
O2 C35 C33 123.3(6) . . ?
O4 C35 C33 112.7(5) . . ?
C48 C40 C41 116.9(6) . . ?
C48 C40 C30 122.2(5) . . ?
C41 C40 C30 120.7(5) . . ?
C46 C47 C48 121.9(6) . . ?
C46 C47 H47 119.0 . . ?
C48 C47 H47 119.0 . . ?
C42 C41 C40 121.7(6) . . ?
C42 C41 N5 118.0(6) . . ?
C40 C41 N5 120.3(6) . . ?
C41 C42 C46 119.9(6) . . ?
C41 C42 H42 120.0 . . ?
C46 C42 H42 120.0 . . ?
C49 O7 H7A 109.5 . . ?
C47 C46 C42 119.8(6) . . ?
C47 C46 C49 119.6(6) . . ?
C42 C46 C49 120.5(6) . . ?
O8 C49 O7 123.7(7) . . ?
O8 C49 C46 122.9(6) . . ?
O7 C49 C46 113.4(6) . . ?
O5 N5 O17 123.2(9) . . ?
O5 N5 C41 120.6(7) . . ?
O17 N5 C41 116.2(9) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.252
_refine_diff_density_min         -1.590
_refine_diff_density_rms         0.260
####################################################################### 
# 
# 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 1457021'
_audit_update_record             
;
2016-03-02 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H14 N4 O12 Zn2'
_chemical_formula_weight         729.17

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   13.230(2)
_cell_length_b                   14.587(3)
_cell_length_c                   15.124(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.618(3)
_cell_angle_gamma                90.00
_cell_volume                     2885.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4981
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.68

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    1.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7229
_exptl_absorpt_correction_T_max  0.7808
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13942
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5010
_reflns_number_gt                4148
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1280P)²+27.4891P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5010
_refine_ls_number_parameters     453
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0826
_refine_ls_wR_factor_ref         0.2311
_refine_ls_wR_factor_gt          0.2185
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.01619(6) 0.78224(5) 0.07679(5) 0.0223(3) Uani 1 1 d . . .
Zn2 Zn 0.15611(6) -0.18496(5) 0.39044(5) 0.0224(3) Uani 1 1 d . . .
N1 N 0.2976(5) 0.3097(4) 0.0768(5) 0.0320(15) Uani 1 1 d . . .
N2 N 0.3629(5) 0.2767(4) 0.3259(4) 0.0291(14) Uani 1 1 d . . .
N3 N 0.2686(5) -0.2769(4) 0.3877(5) 0.0302(14) Uani 1 1 d . . .
N4 N 0.8549(5) -0.6412(4) 0.4196(4) 0.0261(13) Uani 1 1 d . . .
O1 O 0.0598(5) 0.6568(4) 0.1075(4) 0.0448(16) Uani 1 1 d . . .
O2 O 0.1659(5) 0.6337(4) 0.0104(4) 0.0465(16) Uani 1 1 d . . .
O3 O 0.0661(5) 0.3034(3) 0.3313(4) 0.0334(13) Uani 1 1 d . . .
O4 O 0.0621(4) 0.4522(4) 0.3598(3) 0.0327(12) Uani 1 1 d . A .
O5 O 0.0665(5) 0.2034(5) 0.0408(4) 0.0436(15) Uani 1 1 d . . .
O6 O -0.0392(4) 0.2305(4) 0.1394(4) 0.0401(14) Uani 1 1 d . . .
O7 O 0.1365(4) -0.0812(4) 0.3090(4) 0.0373(13) Uani 1 1 d . B .
O8 O 0.2927(5) -0.0578(4) 0.3771(4) 0.0465(16) Uani 1 1 d . B .
O9 O 0.3658(10) 0.2719(8) 0.1307(8) 0.032(3) Uani 0.598(19) 1 d P A 1
O10 O 0.2806(8) 0.2973(6) -0.0033(6) 0.032(3) Uani 0.598(19) 1 d P A 1
O9' O 0.3194(14) 0.2351(12) 0.0969(11) 0.032(4) Uani 0.402(19) 1 d P A 2
O10' O 0.3522(11) 0.3406(9) 0.0244(9) 0.032(5) Uani 0.402(19) 1 d P A 2
O11 O 0.3338(19) 0.3561(8) 0.348(3) 0.029(6) Uani 0.57(8) 1 d P B 3
O12 O 0.4549(14) 0.2417(11) 0.335(3) 0.029(6) Uani 0.57(8) 1 d P B 3
O11' O 0.361(3) 0.3555(11) 0.309(3) 0.029(8) Uani 0.43(8) 1 d P B 4
O12' O 0.4390(18) 0.2541(15) 0.378(4) 0.029(8) Uani 0.43(8) 1 d P B 4
C1 C 0.1211(6) 0.6090(5) 0.0727(5) 0.0247(15) Uani 1 1 d . . .
C2 C 0.1456(6) 0.5159(4) 0.1133(4) 0.0217(14) Uani 1 1 d . A .
C3 C 0.2091(6) 0.4554(5) 0.0760(5) 0.0311(17) Uani 1 1 d . . .
H3 H 0.2382 0.4715 0.0260 0.037 Uiso 1 1 calc R A .
C4 C 0.2271(6) 0.3711(5) 0.1159(5) 0.0303(17) Uani 1 1 d . A .
C5 C 0.1880(5) 0.3420(4) 0.1910(4) 0.0201(14) Uani 1 1 d . . .
C6 C 0.1274(5) 0.4055(4) 0.2294(4) 0.0166(13) Uani 1 1 d . A .
C7 C 0.1060(5) 0.4910(4) 0.1895(4) 0.0197(14) Uani 1 1 d . . .
H7 H 0.0643 0.5319 0.2145 0.024 Uiso 1 1 calc R A .
C8 C 0.2011(5) 0.2449(4) 0.2248(4) 0.0192(13) Uani 1 1 d . A .
C9 C 0.2815(6) 0.2139(5) 0.2876(5) 0.0293(17) Uani 1 1 d . A .
C10 C 0.2897(6) 0.1236(5) 0.3179(5) 0.0336(18) Uani 1 1 d . . .
H10 H 0.3460 0.1048 0.3582 0.040 Uiso 1 1 calc R B .
C11 C 0.2129(6) 0.0630(5) 0.2870(5) 0.0249(15) Uani 1 1 d . B .
C12 C 0.1329(5) 0.0902(4) 0.2231(4) 0.0193(13) Uani 1 1 d . . .
H12 H 0.0816 0.0488 0.2015 0.023 Uiso 1 1 calc R B .
C13 C 0.1291(5) 0.1803(4) 0.1911(4) 0.0171(13) Uani 1 1 d . A .
C14 C 0.0436(5) 0.2075(4) 0.1173(5) 0.0212(14) Uani 1 1 d . . .
C15 C 0.0815(5) 0.3874(5) 0.3146(4) 0.0223(14) Uani 1 1 d . . .
C16 C 0.2164(6) -0.0328(5) 0.3271(5) 0.0283(16) Uani 1 1 d . . .
C17 C 0.2542(7) -0.3560(6) 0.3436(7) 0.045(2) Uani 1 1 d . . .
H17 H 0.1885 -0.3706 0.3162 0.054 Uiso 1 1 calc R . .
C18 C 0.3317(7) -0.4170(6) 0.3367(8) 0.053(3) Uani 1 1 d . . .
H18 H 0.3188 -0.4702 0.3030 0.064 Uiso 1 1 calc R . .
C19 C 0.4282(7) -0.3988(6) 0.3799(7) 0.041(2) Uani 1 1 d . . .
C20 C 0.4421(7) -0.3187(7) 0.4301(8) 0.056(3) Uani 1 1 d . . .
H20 H 0.5056 -0.3058 0.4633 0.068 Uiso 1 1 calc R . .
C21 C 0.3619(7) -0.2582(6) 0.4308(7) 0.048(2) Uani 1 1 d . . .
H21 H 0.3732 -0.2033 0.4619 0.057 Uiso 1 1 calc R . .
C22 C 0.5113(7) -0.4657(7) 0.3736(8) 0.053(2) Uani 1 1 d . . .
H22 H 0.4958 -0.5160 0.3362 0.064 Uiso 1 1 calc R . .
C23 C 0.6026(7) -0.4598(7) 0.4157(7) 0.050(2) Uani 1 1 d . . .
H23 H 0.6175 -0.4080 0.4511 0.060 Uiso 1 1 calc R . .
C24 C 0.6869(7) -0.5259(6) 0.4143(6) 0.040(2) Uani 1 1 d . . .
C25 C 0.7790(7) -0.5060(6) 0.4657(6) 0.041(2) Uani 1 1 d . . .
H25 H 0.7863 -0.4526 0.4997 0.049 Uiso 1 1 calc R . .
C26 C 0.8601(6) -0.5646(6) 0.4671(6) 0.0368(19) Uani 1 1 d . . .
H26 H 0.9215 -0.5499 0.5028 0.044 Uiso 1 1 calc R . .
C27 C 0.7664(7) -0.6617(6) 0.3689(6) 0.0396(19) Uani 1 1 d . . .
H27 H 0.7623 -0.7149 0.3346 0.048 Uiso 1 1 calc R . .
C28 C 0.6806(7) -0.6070(7) 0.3654(7) 0.048(2) Uani 1 1 d . . .
H28 H 0.6194 -0.6242 0.3308 0.058 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 1.914(5) 2 ?
Zn1 O1 1.953(5) . ?
Zn1 O5 1.954(6) 3_565 ?
Zn1 N4 2.033(6) 2_665 ?
Zn2 O7 1.944(5) . ?
Zn2 O2 1.948(6) 4_566 ?
Zn2 O6 1.976(6) 2_545 ?
Zn2 N3 2.008(6) . ?
N1 O9' 1.153(16) . ?
N1 O10 1.212(12) . ?
N1 O10' 1.234(15) . ?
N1 O9 1.249(13) . ?
N1 C4 1.479(9) . ?
N2 O11' 1.18(2) . ?
N2 O12' 1.22(2) . ?
N2 O11 1.28(2) . ?
N2 O12 1.31(2) . ?
N2 C9 1.466(9) . ?
N3 C17 1.332(11) . ?
N3 C21 1.335(11) . ?
N4 C26 1.325(10) . ?
N4 C27 1.333(11) . ?
N4 Zn1 2.033(6) 2_635 ?
O1 C1 1.245(9) . ?
O2 C1 1.239(9) . ?
O2 Zn2 1.948(6) 4_565 ?
O3 C15 1.274(9) . ?
O3 Zn1 1.914(5) 2_545 ?
O4 C15 1.217(9) . ?
O5 C14 1.240(9) . ?
O5 Zn1 1.954(6) 3_565 ?
O6 C14 1.240(9) . ?
O6 Zn2 1.976(6) 2 ?
O7 C16 1.266(10) . ?
O8 C16 1.223(10) . ?
C1 C2 1.506(9) . ?
C2 C7 1.384(9) . ?
C2 C3 1.394(10) . ?
C3 C4 1.375(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(10) . ?
C5 C6 1.406(9) . ?
C5 C8 1.507(9) . ?
C6 C7 1.397(9) . ?
C6 C15 1.526(9) . ?
C7 H7 0.9300 . ?
C8 C13 1.381(9) . ?
C8 C9 1.391(10) . ?
C9 C10 1.393(10) . ?
C10 C11 1.375(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(10) . ?
C11 C16 1.521(9) . ?
C12 C13 1.400(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.518(9) . ?
C17 C18 1.374(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.370(14) . ?
C18 H18 0.9300 . ?
C19 C20 1.391(14) . ?
C19 C22 1.484(12) . ?
C20 C21 1.381(13) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.281(14) . ?
C22 H22 0.9300 . ?
C23 C24 1.477(12) . ?
C23 H23 0.9300 . ?
C24 C25 1.375(13) . ?
C24 C28 1.390(14) . ?
C25 C26 1.369(12) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.383(13) . ?
C27 H27 0.9300 . ?
C28 H28 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 Zn1 O1 99.1(2) 2 . ?
O3 Zn1 O5 110.0(3) 2 3_565 ?
O1 Zn1 O5 114.9(3) . 3_565 ?
O3 Zn1 N4 117.3(2) 2 2_665 ?
O1 Zn1 N4 106.9(3) . 2_665 ?
O5 Zn1 N4 108.6(3) 3_565 2_665 ?
O7 Zn2 O2 106.0(3) . 4_566 ?
O7 Zn2 O6 108.4(3) . 2_545 ?
O2 Zn2 O6 113.1(3) 4_566 2_545 ?
O7 Zn2 N3 122.4(3) . . ?
O2 Zn2 N3 109.2(3) 4_566 . ?
O6 Zn2 N3 97.8(3) 2_545 . ?
O9' N1 O10 97.1(11) . . ?
O9' N1 O10' 111.5(11) . . ?
O10 N1 O10' 56.7(8) . . ?
O10 N1 O9 126.4(9) . . ?
O10' N1 O9 98.4(9) . . ?
O9' N1 C4 127.8(9) . . ?
O10 N1 C4 117.1(7) . . ?
O10' N1 C4 120.0(8) . . ?
O9 N1 C4 116.3(8) . . ?
O11' N2 O12' 113.1(12) . . ?
O12' N2 O11 109.0(19) . . ?
O11' N2 O12 113.5(19) . . ?
O11 N2 O12 129.4(17) . . ?
O11' N2 C9 122.2(9) . . ?
O12' N2 C9 124.7(10) . . ?
O11 N2 C9 115.9(10) . . ?
O12 N2 C9 114.6(11) . . ?
C17 N3 C21 118.2(7) . . ?
C17 N3 Zn2 122.6(6) . . ?
C21 N3 Zn2 119.2(5) . . ?
C26 N4 C27 118.1(7) . . ?
C26 N4 Zn1 118.2(5) . 2_635 ?
C27 N4 Zn1 123.6(5) . 2_635 ?
C1 O1 Zn1 127.8(5) . . ?
C1 O2 Zn2 147.9(6) . 4_565 ?
C15 O3 Zn1 115.2(5) . 2_545 ?
C14 O5 Zn1 131.5(5) . 3_565 ?
C14 O6 Zn2 143.2(5) . 2 ?
C16 O7 Zn2 105.6(5) . . ?
O2 C1 O1 125.1(7) . . ?
O2 C1 C2 118.3(6) . . ?
O1 C1 C2 116.6(6) . . ?
C7 C2 C3 119.8(6) . . ?
C7 C2 C1 119.3(6) . . ?
C3 C2 C1 120.8(6) . . ?
C4 C3 C2 117.7(7) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
C3 C4 C5 125.0(7) . . ?
C3 C4 N1 116.4(7) . . ?
C5 C4 N1 118.6(6) . . ?
C4 C5 C6 116.3(6) . . ?
C4 C5 C8 121.9(6) . . ?
C6 C5 C8 121.5(6) . . ?
C7 C6 C5 120.1(6) . . ?
C7 C6 C15 116.0(6) . . ?
C5 C6 C15 123.9(6) . . ?
C2 C7 C6 121.1(6) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C13 C8 C9 116.4(6) . . ?
C13 C8 C5 118.5(6) . . ?
C9 C8 C5 125.1(6) . . ?
C8 C9 C10 123.1(7) . . ?
C8 C9 N2 120.5(6) . . ?
C10 C9 N2 116.3(6) . . ?
C11 C10 C9 118.6(7) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 120.2(6) . . ?
C10 C11 C16 118.6(7) . . ?
C12 C11 C16 121.1(6) . . ?
C11 C12 C13 119.7(6) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C8 C13 C12 121.7(6) . . ?
C8 C13 C14 119.3(6) . . ?
C12 C13 C14 118.9(6) . . ?
O5 C14 O6 127.9(7) . . ?
O5 C14 C13 114.5(6) . . ?
O6 C14 C13 117.6(6) . . ?
O4 C15 O3 125.6(6) . . ?
O4 C15 C6 119.0(6) . . ?
O3 C15 C6 115.4(6) . . ?
O8 C16 O7 123.5(7) . . ?
O8 C16 C11 119.5(7) . . ?
O7 C16 C11 116.9(7) . . ?
N3 C17 C18 123.2(8) . . ?
N3 C17 H17 118.4 . . ?
C18 C17 H17 118.4 . . ?
C19 C18 C17 119.4(8) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 117.5(8) . . ?
C18 C19 C22 119.2(8) . . ?
C20 C19 C22 123.3(9) . . ?
C21 C20 C19 120.1(9) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
N3 C21 C20 121.5(9) . . ?
N3 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C23 C22 C19 125.2(10) . . ?
C23 C22 H22 117.4 . . ?
C19 C22 H22 117.4 . . ?
C22 C23 C24 127.4(10) . . ?
C22 C23 H23 116.3 . . ?
C24 C23 H23 116.3 . . ?
C25 C24 C28 117.3(8) . . ?
C25 C24 C23 117.5(8) . . ?
C28 C24 C23 125.3(9) . . ?
C26 C25 C24 120.2(8) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
N4 C26 C25 122.7(8) . . ?
N4 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
N4 C27 C28 122.5(8) . . ?
N4 C27 H27 118.7 . . ?
C28 C27 H27 118.7 . . ?
C27 C28 C24 119.2(8) . . ?
C27 C28 H28 120.4 . . ?
C24 C28 H28 120.4 . . ?
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.000 121 6 ' '
2 0.500 1.000 0.500 121 6 ' '
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.303
_refine_diff_density_min         -2.250
_refine_diff_density_rms         0.187
