# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_184_10zn
_database_code_depnum_ccdc_archive 'CCDC 1430225'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H36 N4 O13 Zn'
_chemical_formula_weight         1014.24

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                   11.8801(11)
_cell_length_b                   13.7323(17)
_cell_length_c                   13.9872(19)
_cell_angle_alpha                84.567(11)
_cell_angle_beta                 79.104(9)
_cell_angle_gamma                79.225(9)
_cell_volume                     2197.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            coloreless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8569
_exptl_absorpt_correction_T_max  0.8831
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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            16042
_diffrn_reflns_av_R_equivalents  0.1017
_diffrn_reflns_av_sigmaI/netI    0.1886
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.05
_reflns_number_total             7782
_reflns_number_gt                3592
_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)+(0.0362P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7782
_refine_ls_number_parameters     656
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.0770
_refine_ls_wR_factor_ref         0.1885
_refine_ls_wR_factor_gt          0.1251
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.74378(7) 0.07907(6) 0.23088(6) 0.0399(3) Uani 1 1 d . . .
O1 O 0.9119(4) -0.0182(3) 0.2163(3) 0.0406(12) Uani 1 1 d . . .
O2 O 0.7572(4) -0.0879(3) 0.2432(3) 0.0459(13) Uani 1 1 d . . .
O3 O 1.0919(4) -0.3441(3) 0.5552(3) 0.0460(13) Uani 1 1 d . . .
O4 O 0.9369(4) -0.2228(3) 0.5731(3) 0.0421(12) Uani 1 1 d . . .
H4 H 0.9472 -0.2287 0.6298 0.063 Uiso 1 1 calc R . .
O5 O 0.9166(4) -0.2309(3) -0.2386(3) 0.0445(13) Uani 1 1 d . . .
O6 O 0.8685(4) -0.3793(4) -0.1860(4) 0.0493(14) Uani 1 1 d . . .
H6 H 0.8301 -0.3707 -0.2299 0.074 Uiso 1 1 calc R . .
O7 O 0.6724(4) 0.3717(4) 0.4748(3) 0.0457(13) Uani 1 1 d . . .
H7 H 0.7407 0.3603 0.4819 0.069 Uiso 1 1 calc R . .
O8 O 0.6421(4) 0.3336(4) 0.6330(3) 0.0584(15) Uani 1 1 d . . .
O9 O 0.3921(4) 0.3843(4) 0.2709(3) 0.0517(14) Uani 1 1 d . . .
O10 O 0.2025(4) 0.4000(3) 0.3359(3) 0.0471(13) Uani 1 1 d . . .
O11 O 0.3798(5) 0.2358(4) 1.0849(4) 0.0622(16) Uani 1 1 d . . .
O12 O 0.4224(5) 0.3876(4) 1.0821(3) 0.0628(16) Uani 1 1 d . . .
H12 H 0.4118 0.3771 1.1416 0.094 Uiso 1 1 calc R . .
O13 O 0.1234(5) 0.0190(4) 0.2573(5) 0.0757(18) Uani 1 1 d G . .
H1W H 0.0685 0.0000 0.2368 0.114 Uiso 1 1 d G . .
H2W H 0.1187 0.0814 0.2460 0.114 Uiso 1 1 d G . .
N1 N 0.7198(5) 0.0940(5) 0.0840(4) 0.0505(17) Uani 1 1 d . . .
N2 N 0.7726(4) 0.2248(4) 0.1920(4) 0.0361(14) Uani 1 1 d . . .
N3 N 0.5672(5) 0.1070(4) 0.2954(4) 0.0399(15) Uani 1 1 d . . .
N4 N 0.7556(5) 0.0867(4) 0.3819(4) 0.0356(14) Uani 1 1 d . . .
C1 C 0.8632(6) -0.0939(5) 0.2397(4) 0.0292(15) Uani 1 1 d . . .
C2 C 0.9335(5) -0.1889(4) 0.2745(4) 0.0239(14) Uani 1 1 d . . .
C3 C 0.9461(5) -0.1939(5) 0.3725(4) 0.0284(15) Uani 1 1 d . . .
H3 H 0.9123 -0.1399 0.4098 0.034 Uiso 1 1 calc R . .
C4 C 1.0076(5) -0.2772(5) 0.4157(4) 0.0295(15) Uani 1 1 d . . .
C5 C 1.0582(5) -0.3569(5) 0.3590(5) 0.0328(16) Uani 1 1 d . . .
H5 H 1.1027 -0.4125 0.3852 0.039 Uiso 1 1 calc R . .
C6 C 1.0422(5) -0.3532(5) 0.2632(5) 0.0346(17) Uani 1 1 d . . .
H23 H 1.0747 -0.4081 0.2268 0.042 Uiso 1 1 calc R . .
C7 C 0.9799(5) -0.2716(5) 0.2191(5) 0.0298(16) Uani 1 1 d . . .
C8 C 1.0178(5) -0.2848(5) 0.5208(5) 0.0329(16) Uani 1 1 d . . .
C9 C 0.9612(5) -0.2750(4) 0.1168(5) 0.0291(16) Uani 1 1 d . . .
C10 C 0.9641(5) -0.1939(5) 0.0485(5) 0.0340(17) Uani 1 1 d . . .
H10 H 0.9787 -0.1345 0.0662 0.041 Uiso 1 1 calc R . .
C11 C 0.9454(5) -0.2011(5) -0.0458(5) 0.0345(16) Uani 1 1 d . . .
H11 H 0.9480 -0.1468 -0.0907 0.041 Uiso 1 1 calc R . .
C12 C 0.9229(5) -0.2896(5) -0.0728(5) 0.0299(16) Uani 1 1 d . . .
C13 C 0.9230(5) -0.3700(5) -0.0065(5) 0.0350(17) Uani 1 1 d . . .
H13 H 0.9103 -0.4299 -0.0248 0.042 Uiso 1 1 calc R . .
C14 C 0.9420(5) -0.3633(5) 0.0879(5) 0.0373(17) Uani 1 1 d . . .
H14 H 0.9417 -0.4185 0.1318 0.045 Uiso 1 1 calc R . .
C15 C 0.9003(6) -0.2982(5) -0.1743(5) 0.0379(18) Uani 1 1 d . . .
C16 C 0.6977(7) 0.0255(7) 0.0334(6) 0.071(3) Uani 1 1 d . . .
H16 H 0.6958 -0.0386 0.0609 0.085 Uiso 1 1 calc R . .
C17 C 0.6768(9) 0.0504(9) -0.0630(8) 0.097(4) Uani 1 1 d . . .
H17 H 0.6583 0.0025 -0.0972 0.116 Uiso 1 1 calc R . .
C18 C 0.6831(8) 0.1406(9) -0.1061(7) 0.087(4) Uani 1 1 d . . .
H18 H 0.6702 0.1551 -0.1698 0.105 Uiso 1 1 calc R . .
C19 C 0.7095(6) 0.2136(7) -0.0535(6) 0.053(2) Uani 1 1 d . . .
C20 C 0.7270(5) 0.1859(6) 0.0427(5) 0.046(2) Uani 1 1 d . . .
C21 C 0.7178(6) 0.3144(7) -0.0912(6) 0.067(3) Uani 1 1 d . . .
H21 H 0.7068 0.3338 -0.1548 0.080 Uiso 1 1 calc R . .
C22 C 0.7414(6) 0.3812(7) -0.0349(7) 0.071(3) Uani 1 1 d . . .
H22 H 0.7457 0.4456 -0.0608 0.085 Uiso 1 1 calc R . .
C23 C 0.7598(6) 0.3550(6) 0.0626(6) 0.048(2) Uani 1 1 d . . .
C24 C 0.7538(5) 0.2573(6) 0.0989(5) 0.0419(18) Uani 1 1 d . . .
C25 C 0.7861(6) 0.4177(6) 0.1239(7) 0.061(2) Uani 1 1 d . . .
H25 H 0.7917 0.4829 0.1017 0.073 Uiso 1 1 calc R . .
C26 C 0.8036(6) 0.3866(6) 0.2146(7) 0.058(2) Uani 1 1 d . . .
H26 H 0.8190 0.4298 0.2559 0.070 Uiso 1 1 calc R . .
C27 C 0.7983(6) 0.2883(5) 0.2452(6) 0.047(2) Uani 1 1 d . . .
H27 H 0.8138 0.2661 0.3070 0.056 Uiso 1 1 calc R . .
C28 C 0.4744(6) 0.1177(5) 0.2528(6) 0.047(2) Uani 1 1 d . . .
H28 H 0.4859 0.1130 0.1856 0.056 Uiso 1 1 calc R . .
C29 C 0.3607(6) 0.1357(5) 0.3039(6) 0.055(2) Uani 1 1 d . . .
H29 H 0.2978 0.1430 0.2715 0.066 Uiso 1 1 calc R . .
C30 C 0.3434(6) 0.1425(5) 0.4022(7) 0.054(2) Uani 1 1 d . . .
H30 H 0.2681 0.1558 0.4374 0.065 Uiso 1 1 calc R . .
C31 C 0.4396(6) 0.1291(5) 0.4509(5) 0.0380(17) Uani 1 1 d . . .
C32 C 0.5489(5) 0.1134(4) 0.3937(5) 0.0356(17) Uani 1 1 d . . .
C33 C 0.6503(6) 0.1026(5) 0.4413(5) 0.0364(17) Uani 1 1 d . . .
C34 C 0.4274(6) 0.1333(5) 0.5542(6) 0.047(2) Uani 1 1 d . . .
H34 H 0.3535 0.1438 0.5922 0.057 Uiso 1 1 calc R . .
C35 C 0.5216(7) 0.1222(5) 0.5973(5) 0.048(2) Uani 1 1 d . . .
H35 H 0.5117 0.1240 0.6647 0.057 Uiso 1 1 calc R . .
C36 C 0.6364(6) 0.1076(5) 0.5413(6) 0.0414(18) Uani 1 1 d . . .
C37 C 0.7384(7) 0.0942(5) 0.5812(6) 0.050(2) Uani 1 1 d . . .
H37 H 0.7336 0.0960 0.6482 0.060 Uiso 1 1 calc R . .
C38 C 0.8422(6) 0.0789(5) 0.5236(6) 0.048(2) Uani 1 1 d . . .
H38 H 0.9098 0.0693 0.5502 0.058 Uiso 1 1 calc R . .
C39 C 0.8491(6) 0.0774(5) 0.4241(5) 0.0441(19) Uani 1 1 d . . .
H39 H 0.9222 0.0696 0.3847 0.053 Uiso 1 1 calc R . .
C40 C 0.6046(6) 0.3572(5) 0.5600(5) 0.0372(17) Uani 1 1 d . . .
C41 C 0.4779(5) 0.3747(4) 0.5497(4) 0.0260(15) Uani 1 1 d . . .
C42 C 0.4516(5) 0.3826(4) 0.4563(5) 0.0314(16) Uani 1 1 d . . .
H42 H 0.5113 0.3808 0.4025 0.038 Uiso 1 1 calc R . .
C43 C 0.3369(5) 0.3929(5) 0.4421(5) 0.0331(16) Uani 1 1 d . . .
C44 C 0.2504(5) 0.3971(5) 0.5215(5) 0.0337(17) Uani 1 1 d . . .
H44 H 0.1734 0.4055 0.5128 0.040 Uiso 1 1 calc R . .
C45 C 0.2754(5) 0.3891(5) 0.6148(5) 0.0354(17) Uani 1 1 d . . .
H45 H 0.2146 0.3921 0.6678 0.043 Uiso 1 1 calc R . .
C46 C 0.3894(5) 0.3764(4) 0.6314(4) 0.0276(15) Uani 1 1 d . . .
C47 C 0.3111(7) 0.3922(5) 0.3407(5) 0.0402(18) Uani 1 1 d . . .
C48 C 0.4031(5) 0.3596(4) 0.7346(4) 0.0272(15) Uani 1 1 d . . .
C49 C 0.3597(6) 0.2814(5) 0.7883(5) 0.0408(18) Uani 1 1 d . . .
H49 H 0.3285 0.2385 0.7572 0.049 Uiso 1 1 calc R . .
C50 C 0.3611(5) 0.2648(5) 0.8869(5) 0.0376(17) Uani 1 1 d . . .
H50 H 0.3321 0.2110 0.9218 0.045 Uiso 1 1 calc R . .
C51 C 0.4069(5) 0.3303(5) 0.9334(5) 0.0358(17) Uani 1 1 d . . .
C52 C 0.4508(5) 0.4088(5) 0.8814(5) 0.0333(16) Uani 1 1 d . . .
H52 H 0.4814 0.4521 0.9126 0.040 Uiso 1 1 calc R . .
C53 C 0.4495(5) 0.4230(5) 0.7830(5) 0.0315(16) Uani 1 1 d . . .
H53 H 0.4800 0.4759 0.7479 0.038 Uiso 1 1 calc R . .
C54 C 0.4019(6) 0.3113(6) 1.0413(5) 0.0441(19) 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 N2 2.096(5) . ?
Zn1 N3 2.101(6) . ?
Zn1 N1 2.113(6) . ?
Zn1 N4 2.156(5) . ?
Zn1 O1 2.172(4) . ?
Zn1 O2 2.260(4) . ?
O1 C1 1.270(7) . ?
O2 C1 1.239(7) . ?
O3 C8 1.219(7) . ?
O4 C8 1.314(7) . ?
O4 H4 0.8200 . ?
O5 C15 1.243(8) . ?
O6 C15 1.275(7) . ?
O6 H6 0.8200 . ?
O7 C40 1.327(8) . ?
O7 H7 0.8200 . ?
O8 C40 1.184(7) . ?
O9 C47 1.232(8) . ?
O10 C47 1.288(7) . ?
O11 C54 1.199(8) . ?
O12 C54 1.321(8) . ?
O12 H12 0.8200 . ?
O13 H1W 0.8500 . ?
O13 H2W 0.8500 . ?
N1 C16 1.320(9) . ?
N1 C20 1.348(9) . ?
N2 C27 1.310(7) . ?
N2 C24 1.381(8) . ?
N3 C28 1.328(7) . ?
N3 C32 1.359(8) . ?
N4 C39 1.334(7) . ?
N4 C33 1.357(8) . ?
C1 C2 1.504(7) . ?
C2 C3 1.401(7) . ?
C2 C7 1.402(8) . ?
C3 C4 1.389(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(8) . ?
C4 C8 1.491(8) . ?
C5 C6 1.383(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.384(8) . ?
C6 H23 0.9300 . ?
C7 C9 1.495(8) . ?
C9 C14 1.384(8) . ?
C9 C10 1.398(8) . ?
C10 C11 1.393(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.392(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.373(8) . ?
C12 C15 1.512(8) . ?
C13 C14 1.395(8) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C16 C17 1.415(11) . ?
C16 H16 0.9300 . ?
C17 C18 1.334(13) . ?
C17 H17 0.9300 . ?
C18 C19 1.409(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.407(9) . ?
C19 C21 1.449(11) . ?
C20 C24 1.428(9) . ?
C21 C22 1.363(11) . ?
C21 H21 0.9300 . ?
C22 C23 1.424(10) . ?
C22 H22 0.9300 . ?
C23 C25 1.384(10) . ?
C23 C24 1.398(9) . ?
C25 C26 1.341(10) . ?
C25 H25 0.9300 . ?
C26 C27 1.386(9) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.394(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.361(10) . ?
C29 H29 0.9300 . ?
C30 C31 1.413(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.382(9) . ?
C31 C34 1.430(9) . ?
C32 C33 1.462(8) . ?
C33 C36 1.383(9) . ?
C34 C35 1.346(8) . ?
C34 H34 0.9300 . ?
C35 C36 1.427(9) . ?
C35 H35 0.9300 . ?
C36 C37 1.404(9) . ?
C37 C38 1.332(9) . ?
C37 H37 0.9300 . ?
C38 C39 1.380(9) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.510(8) . ?
C41 C42 1.390(7) . ?
C41 C46 1.398(8) . ?
C42 C43 1.393(8) . ?
C42 H42 0.9300 . ?
C43 C44 1.360(9) . ?
C43 C47 1.509(8) . ?
C44 C45 1.383(8) . ?
C44 H44 0.9300 . ?
C45 C46 1.393(7) . ?
C45 H45 0.9300 . ?
C46 C48 1.476(8) . ?
C48 C49 1.374(9) . ?
C48 C53 1.396(7) . ?
C49 C50 1.380(8) . ?
C49 H49 0.9300 . ?
C50 C51 1.398(8) . ?
C50 H50 0.9300 . ?
C51 C52 1.372(9) . ?
C51 C54 1.498(9) . ?
C52 C53 1.374(8) . ?
C52 H52 0.9300 . ?
C53 H53 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
N2 Zn1 N3 100.2(2) . . ?
N2 Zn1 N1 79.2(2) . . ?
N3 Zn1 N1 97.4(2) . . ?
N2 Zn1 N4 94.0(2) . . ?
N3 Zn1 N4 78.6(2) . . ?
N1 Zn1 N4 171.4(2) . . ?
N2 Zn1 O1 107.98(18) . . ?
N3 Zn1 O1 149.23(19) . . ?
N1 Zn1 O1 99.86(19) . . ?
N4 Zn1 O1 87.09(18) . . ?
N2 Zn1 O2 164.5(2) . . ?
N3 Zn1 O2 94.56(19) . . ?
N1 Zn1 O2 94.3(2) . . ?
N4 Zn1 O2 93.53(18) . . ?
O1 Zn1 O2 58.98(15) . . ?
C1 O1 Zn1 91.0(4) . . ?
C1 O2 Zn1 87.7(4) . . ?
C8 O4 H4 109.5 . . ?
C15 O6 H6 109.5 . . ?
C40 O7 H7 109.5 . . ?
C54 O12 H12 109.5 . . ?
H1W O13 H2W 109.5 . . ?
C16 N1 C20 120.2(7) . . ?
C16 N1 Zn1 127.2(6) . . ?
C20 N1 Zn1 112.6(5) . . ?
C27 N2 C24 117.7(6) . . ?
C27 N2 Zn1 129.0(5) . . ?
C24 N2 Zn1 113.2(5) . . ?
C28 N3 C32 117.7(6) . . ?
C28 N3 Zn1 128.4(5) . . ?
C32 N3 Zn1 113.9(4) . . ?
C39 N4 C33 116.7(6) . . ?
C39 N4 Zn1 130.0(5) . . ?
C33 N4 Zn1 113.3(4) . . ?
O2 C1 O1 121.0(6) . . ?
O2 C1 C2 119.8(6) . . ?
O1 C1 C2 118.8(6) . . ?
C3 C2 C7 119.3(5) . . ?
C3 C2 C1 115.1(5) . . ?
C7 C2 C1 125.5(5) . . ?
C4 C3 C2 121.9(6) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C5 C4 C3 118.4(6) . . ?
C5 C4 C8 119.3(6) . . ?
C3 C4 C8 122.3(6) . . ?
C6 C5 C4 119.6(6) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 122.9(6) . . ?
C5 C6 H23 118.5 . . ?
C7 C6 H23 118.5 . . ?
C6 C7 C2 117.7(5) . . ?
C6 C7 C9 119.9(6) . . ?
C2 C7 C9 122.4(5) . . ?
O3 C8 O4 123.5(6) . . ?
O3 C8 C4 123.4(6) . . ?
O4 C8 C4 113.1(5) . . ?
C14 C9 C10 118.4(6) . . ?
C14 C9 C7 118.4(6) . . ?
C10 C9 C7 123.2(5) . . ?
C11 C10 C9 120.8(6) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 120.1(6) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C11 119.2(6) . . ?
C13 C12 C15 120.0(6) . . ?
C11 C12 C15 120.8(6) . . ?
C12 C13 C14 120.9(6) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C9 C14 C13 120.6(6) . . ?
C9 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
O5 C15 O6 125.6(6) . . ?
O5 C15 C12 120.2(6) . . ?
O6 C15 C12 114.2(6) . . ?
N1 C16 C17 119.5(9) . . ?
N1 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 121.9(10) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 119.0(9) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C20 C19 C18 117.0(9) . . ?
C20 C19 C21 118.4(8) . . ?
C18 C19 C21 124.6(9) . . ?
N1 C20 C19 122.3(8) . . ?
N1 C20 C24 118.6(7) . . ?
C19 C20 C24 119.0(8) . . ?
C22 C21 C19 121.0(8) . . ?
C22 C21 H21 119.5 . . ?
C19 C21 H21 119.5 . . ?
C21 C22 C23 121.7(9) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C25 C23 C24 117.1(7) . . ?
C25 C23 C22 125.3(8) . . ?
C24 C23 C22 117.6(8) . . ?
N2 C24 C23 121.6(7) . . ?
N2 C24 C20 116.1(7) . . ?
C23 C24 C20 122.3(7) . . ?
C26 C25 C23 121.5(8) . . ?
C26 C25 H25 119.2 . . ?
C23 C25 H25 119.2 . . ?
C25 C26 C27 118.2(8) . . ?
C25 C26 H26 120.9 . . ?
C27 C26 H26 120.9 . . ?
N2 C27 C26 123.8(7) . . ?
N2 C27 H27 118.1 . . ?
C26 C27 H27 118.1 . . ?
N3 C28 C29 123.1(7) . . ?
N3 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C30 C29 C28 118.7(7) . . ?
C30 C29 H29 120.7 . . ?
C28 C29 H29 120.7 . . ?
C29 C30 C31 120.1(7) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C32 C31 C30 116.8(7) . . ?
C32 C31 C34 120.2(6) . . ?
C30 C31 C34 122.9(7) . . ?
N3 C32 C31 123.5(6) . . ?
N3 C32 C33 118.2(6) . . ?
C31 C32 C33 118.3(7) . . ?
N4 C33 C36 123.6(6) . . ?
N4 C33 C32 115.9(6) . . ?
C36 C33 C32 120.4(7) . . ?
C35 C34 C31 120.9(7) . . ?
C35 C34 H34 119.6 . . ?
C31 C34 H34 119.6 . . ?
C34 C35 C36 121.1(7) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C33 C36 C37 116.7(7) . . ?
C33 C36 C35 119.1(6) . . ?
C37 C36 C35 124.2(7) . . ?
C38 C37 C36 120.2(7) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C39 119.7(7) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
N4 C39 C38 123.0(7) . . ?
N4 C39 H39 118.5 . . ?
C38 C39 H39 118.5 . . ?
O8 C40 O7 122.5(6) . . ?
O8 C40 C41 126.3(6) . . ?
O7 C40 C41 111.2(6) . . ?
C42 C41 C46 120.4(5) . . ?
C42 C41 C40 118.1(6) . . ?
C46 C41 C40 121.4(5) . . ?
C41 C42 C43 120.9(6) . . ?
C41 C42 H42 119.6 . . ?
C43 C42 H42 119.6 . . ?
C44 C43 C42 118.8(6) . . ?
C44 C43 C47 121.0(6) . . ?
C42 C43 C47 120.0(6) . . ?
C43 C44 C45 120.9(6) . . ?
C43 C44 H44 119.6 . . ?
C45 C44 H44 119.6 . . ?
C44 C45 C46 121.6(6) . . ?
C44 C45 H45 119.2 . . ?
C46 C45 H45 119.2 . . ?
C45 C46 C41 117.4(6) . . ?
C45 C46 C48 115.4(5) . . ?
C41 C46 C48 127.1(5) . . ?
O9 C47 O10 125.7(6) . . ?
O9 C47 C43 119.3(6) . . ?
O10 C47 C43 115.0(6) . . ?
C49 C48 C53 117.9(6) . . ?
C49 C48 C46 118.1(5) . . ?
C53 C48 C46 123.7(6) . . ?
C48 C49 C50 121.9(6) . . ?
C48 C49 H49 119.1 . . ?
C50 C49 H49 119.1 . . ?
C49 C50 C51 118.8(7) . . ?
C49 C50 H50 120.6 . . ?
C51 C50 H50 120.6 . . ?
C52 C51 C50 120.4(6) . . ?
C52 C51 C54 122.9(6) . . ?
C50 C51 C54 116.6(7) . . ?
C51 C52 C53 119.6(6) . . ?
C51 C52 H52 120.2 . . ?
C53 C52 H52 120.2 . . ?
C52 C53 C48 121.4(6) . . ?
C52 C53 H53 119.3 . . ?
C48 C53 H53 119.3 . . ?
O11 C54 O12 124.5(7) . . ?
O11 C54 C51 123.3(7) . . ?
O12 C54 C51 112.3(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
N2 Zn1 O1 C1 -177.4(3) . . . . ?
N3 Zn1 O1 C1 27.4(5) . . . . ?
N1 Zn1 O1 C1 -95.7(4) . . . . ?
N4 Zn1 O1 C1 89.3(4) . . . . ?
O2 Zn1 O1 C1 -6.6(3) . . . . ?
N2 Zn1 O2 C1 41.3(8) . . . . ?
N3 Zn1 O2 C1 -156.6(4) . . . . ?
N1 Zn1 O2 C1 105.6(4) . . . . ?
N4 Zn1 O2 C1 -77.7(4) . . . . ?
O1 Zn1 O2 C1 6.7(3) . . . . ?
N2 Zn1 N1 C16 177.5(7) . . . . ?
N3 Zn1 N1 C16 -83.5(6) . . . . ?
N4 Zn1 N1 C16 -145.2(14) . . . . ?
O1 Zn1 N1 C16 70.9(6) . . . . ?
O2 Zn1 N1 C16 11.7(6) . . . . ?
N2 Zn1 N1 C20 -3.8(5) . . . . ?
N3 Zn1 N1 C20 95.2(5) . . . . ?
N4 Zn1 N1 C20 33.6(18) . . . . ?
O1 Zn1 N1 C20 -110.4(5) . . . . ?
O2 Zn1 N1 C20 -169.6(5) . . . . ?
N3 Zn1 N2 C27 84.3(6) . . . . ?
N1 Zn1 N2 C27 180.0(6) . . . . ?
N4 Zn1 N2 C27 5.2(6) . . . . ?
O1 Zn1 N2 C27 -83.1(6) . . . . ?
O2 Zn1 N2 C27 -113.8(8) . . . . ?
N3 Zn1 N2 C24 -91.3(4) . . . . ?
N1 Zn1 N2 C24 4.4(4) . . . . ?
N4 Zn1 N2 C24 -170.4(4) . . . . ?
O1 Zn1 N2 C24 101.4(4) . . . . ?
O2 Zn1 N2 C24 70.6(8) . . . . ?
N2 Zn1 N3 C28 87.4(6) . . . . ?
N1 Zn1 N3 C28 7.1(6) . . . . ?
N4 Zn1 N3 C28 179.4(6) . . . . ?
O1 Zn1 N3 C28 -116.6(6) . . . . ?
O2 Zn1 N3 C28 -87.9(6) . . . . ?
N2 Zn1 N3 C32 -93.3(5) . . . . ?
N1 Zn1 N3 C32 -173.6(5) . . . . ?
N4 Zn1 N3 C32 -1.3(4) . . . . ?
O1 Zn1 N3 C32 62.7(6) . . . . ?
O2 Zn1 N3 C32 91.4(4) . . . . ?
N2 Zn1 N4 C39 -79.8(6) . . . . ?
N3 Zn1 N4 C39 -179.4(6) . . . . ?
N1 Zn1 N4 C39 -116.4(15) . . . . ?
O1 Zn1 N4 C39 28.0(5) . . . . ?
O2 Zn1 N4 C39 86.7(6) . . . . ?
N2 Zn1 N4 C33 100.8(4) . . . . ?
N3 Zn1 N4 C33 1.2(4) . . . . ?
N1 Zn1 N4 C33 64.1(16) . . . . ?
O1 Zn1 N4 C33 -151.4(4) . . . . ?
O2 Zn1 N4 C33 -92.7(4) . . . . ?
Zn1 O2 C1 O1 -11.6(6) . . . . ?
Zn1 O2 C1 C2 161.4(5) . . . . ?
Zn1 O1 C1 O2 12.0(6) . . . . ?
Zn1 O1 C1 C2 -161.0(5) . . . . ?
O2 C1 C2 C3 -92.4(7) . . . . ?
O1 C1 C2 C3 80.6(7) . . . . ?
O2 C1 C2 C7 83.9(8) . . . . ?
O1 C1 C2 C7 -103.0(7) . . . . ?
C7 C2 C3 C4 2.7(9) . . . . ?
C1 C2 C3 C4 179.3(6) . . . . ?
C2 C3 C4 C5 0.5(9) . . . . ?
C2 C3 C4 C8 -177.7(5) . . . . ?
C3 C4 C5 C6 -2.7(9) . . . . ?
C8 C4 C5 C6 175.4(5) . . . . ?
C4 C5 C6 C7 1.9(9) . . . . ?
C5 C6 C7 C2 1.3(9) . . . . ?
C5 C6 C7 C9 -176.9(5) . . . . ?
C3 C2 C7 C6 -3.5(8) . . . . ?
C1 C2 C7 C6 -179.7(6) . . . . ?
C3 C2 C7 C9 174.6(5) . . . . ?
C1 C2 C7 C9 -1.6(9) . . . . ?
C5 C4 C8 O3 20.2(9) . . . . ?
C3 C4 C8 O3 -161.7(6) . . . . ?
C5 C4 C8 O4 -158.2(6) . . . . ?
C3 C4 C8 O4 19.9(9) . . . . ?
C6 C7 C9 C14 37.3(9) . . . . ?
C2 C7 C9 C14 -140.8(6) . . . . ?
C6 C7 C9 C10 -141.6(7) . . . . ?
C2 C7 C9 C10 40.3(9) . . . . ?
C14 C9 C10 C11 1.5(9) . . . . ?
C7 C9 C10 C11 -179.6(5) . . . . ?
C9 C10 C11 C12 0.4(9) . . . . ?
C10 C11 C12 C13 -2.0(9) . . . . ?
C10 C11 C12 C15 178.9(5) . . . . ?
C11 C12 C13 C14 1.9(9) . . . . ?
C15 C12 C13 C14 -179.1(5) . . . . ?
C10 C9 C14 C13 -1.7(9) . . . . ?
C7 C9 C14 C13 179.4(5) . . . . ?
C12 C13 C14 C9 0.0(9) . . . . ?
C13 C12 C15 O5 -169.6(6) . . . . ?
C11 C12 C15 O5 9.4(9) . . . . ?
C13 C12 C15 O6 8.2(9) . . . . ?
C11 C12 C15 O6 -172.8(6) . . . . ?
C20 N1 C16 C17 -2.6(12) . . . . ?
Zn1 N1 C16 C17 176.0(6) . . . . ?
N1 C16 C17 C18 2.5(15) . . . . ?
C16 C17 C18 C19 -1.0(16) . . . . ?
C17 C18 C19 C20 -0.4(13) . . . . ?
C17 C18 C19 C21 -179.3(9) . . . . ?
C16 N1 C20 C19 1.3(11) . . . . ?
Zn1 N1 C20 C19 -177.6(5) . . . . ?
C16 N1 C20 C24 -178.5(6) . . . . ?
Zn1 N1 C20 C24 2.6(8) . . . . ?
C18 C19 C20 N1 0.3(10) . . . . ?
C21 C19 C20 N1 179.3(7) . . . . ?
C18 C19 C20 C24 -179.9(7) . . . . ?
C21 C19 C20 C24 -0.9(10) . . . . ?
C20 C19 C21 C22 -0.3(11) . . . . ?
C18 C19 C21 C22 178.6(8) . . . . ?
C19 C21 C22 C23 0.5(12) . . . . ?
C21 C22 C23 C25 178.8(7) . . . . ?
C21 C22 C23 C24 0.6(11) . . . . ?
C27 N2 C24 C23 -1.2(9) . . . . ?
Zn1 N2 C24 C23 175.0(5) . . . . ?
C27 N2 C24 C20 179.5(6) . . . . ?
Zn1 N2 C24 C20 -4.4(7) . . . . ?
C25 C23 C24 N2 0.4(10) . . . . ?
C22 C23 C24 N2 178.8(6) . . . . ?
C25 C23 C24 C20 179.7(6) . . . . ?
C22 C23 C24 C20 -1.9(10) . . . . ?
N1 C20 C24 N2 1.2(9) . . . . ?
C19 C20 C24 N2 -178.6(5) . . . . ?
N1 C20 C24 C23 -178.2(6) . . . . ?
C19 C20 C24 C23 2.0(10) . . . . ?
C24 C23 C25 C26 -0.8(11) . . . . ?
C22 C23 C25 C26 -179.1(7) . . . . ?
C23 C25 C26 C27 1.9(12) . . . . ?
C24 N2 C27 C26 2.4(10) . . . . ?
Zn1 N2 C27 C26 -173.0(5) . . . . ?
C25 C26 C27 N2 -2.8(12) . . . . ?
C32 N3 C28 C29 0.4(10) . . . . ?
Zn1 N3 C28 C29 179.7(5) . . . . ?
N3 C28 C29 C30 -0.2(11) . . . . ?
C28 C29 C30 C31 -1.4(11) . . . . ?
C29 C30 C31 C32 2.5(10) . . . . ?
C29 C30 C31 C34 -178.7(7) . . . . ?
C28 N3 C32 C31 0.9(9) . . . . ?
Zn1 N3 C32 C31 -178.5(5) . . . . ?
C28 N3 C32 C33 -179.5(5) . . . . ?
Zn1 N3 C32 C33 1.2(7) . . . . ?
C30 C31 C32 N3 -2.4(10) . . . . ?
C34 C31 C32 N3 178.9(6) . . . . ?
C30 C31 C32 C33 178.0(6) . . . . ?
C34 C31 C32 C33 -0.7(9) . . . . ?
C39 N4 C33 C36 -1.3(9) . . . . ?
Zn1 N4 C33 C36 178.2(5) . . . . ?
C39 N4 C33 C32 179.5(5) . . . . ?
Zn1 N4 C33 C32 -1.0(7) . . . . ?
N3 C32 C33 N4 -0.1(9) . . . . ?
C31 C32 C33 N4 179.6(6) . . . . ?
N3 C32 C33 C36 -179.3(6) . . . . ?
C31 C32 C33 C36 0.3(9) . . . . ?
C32 C31 C34 C35 0.1(10) . . . . ?
C30 C31 C34 C35 -178.6(6) . . . . ?
C31 C34 C35 C36 1.0(10) . . . . ?
N4 C33 C36 C37 -0.6(10) . . . . ?
C32 C33 C36 C37 178.6(6) . . . . ?
N4 C33 C36 C35 -178.4(6) . . . . ?
C32 C33 C36 C35 0.8(10) . . . . ?
C34 C35 C36 C33 -1.5(10) . . . . ?
C34 C35 C36 C37 -179.1(6) . . . . ?
C33 C36 C37 C38 0.8(10) . . . . ?
C35 C36 C37 C38 178.6(7) . . . . ?
C36 C37 C38 C39 0.7(11) . . . . ?
C33 N4 C39 C38 3.0(9) . . . . ?
Zn1 N4 C39 C38 -176.4(5) . . . . ?
C37 C38 C39 N4 -2.8(11) . . . . ?
O8 C40 C41 C42 -167.4(7) . . . . ?
O7 C40 C41 C42 12.7(8) . . . . ?
O8 C40 C41 C46 8.2(11) . . . . ?
O7 C40 C41 C46 -171.6(6) . . . . ?
C46 C41 C42 C43 0.5(9) . . . . ?
C40 C41 C42 C43 176.2(6) . . . . ?
C41 C42 C43 C44 1.2(9) . . . . ?
C41 C42 C43 C47 -174.6(6) . . . . ?
C42 C43 C44 C45 -1.4(10) . . . . ?
C47 C43 C44 C45 174.3(6) . . . . ?
C43 C44 C45 C46 0.0(10) . . . . ?
C44 C45 C46 C41 1.6(9) . . . . ?
C44 C45 C46 C48 -174.5(6) . . . . ?
C42 C41 C46 C45 -1.8(9) . . . . ?
C40 C41 C46 C45 -177.4(5) . . . . ?
C42 C41 C46 C48 173.8(6) . . . . ?
C40 C41 C46 C48 -1.8(10) . . . . ?
C44 C43 C47 O9 -177.1(7) . . . . ?
C42 C43 C47 O9 -1.4(10) . . . . ?
C44 C43 C47 O10 2.8(9) . . . . ?
C42 C43 C47 O10 178.4(6) . . . . ?
C45 C46 C48 C49 56.3(8) . . . . ?
C41 C46 C48 C49 -119.3(7) . . . . ?
C45 C46 C48 C53 -118.5(7) . . . . ?
C41 C46 C48 C53 65.9(9) . . . . ?
C53 C48 C49 C50 0.0(9) . . . . ?
C46 C48 C49 C50 -175.1(6) . . . . ?
C48 C49 C50 C51 0.8(10) . . . . ?
C49 C50 C51 C52 -0.8(10) . . . . ?
C49 C50 C51 C54 177.6(6) . . . . ?
C50 C51 C52 C53 0.1(9) . . . . ?
C54 C51 C52 C53 -178.1(6) . . . . ?
C51 C52 C53 C48 0.6(9) . . . . ?
C49 C48 C53 C52 -0.7(9) . . . . ?
C46 C48 C53 C52 174.1(5) . . . . ?
C52 C51 C54 O11 -168.7(7) . . . . ?
C50 C51 C54 O11 13.0(10) . . . . ?
C52 C51 C54 O12 12.4(9) . . . . ?
C50 C51 C54 O12 -166.0(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H2W O5 0.85 2.01 2.855(7) 169.9 2_655
O13 H1W O1 0.85 2.00 2.824(6) 163.7 1_455
O12 H12 O9 0.82 1.79 2.593(7) 166.4 1_556
O7 H7 O3 0.82 1.93 2.711(6) 157.8 2_756
O6 H6 O10 0.82 1.70 2.463(6) 153.1 2_655
O4 H4 O5 0.82 1.81 2.593(6) 160.5 1_556

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.087
####################################################################### 
# 
# 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_241-12co1
_database_code_depnum_ccdc_archive 'CCDC 1430226'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H30 Co N8 O12'
_chemical_formula_weight         897.67

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                   8.0674(10)
_cell_length_b                   9.2640(15)
_cell_length_c                   13.4563(18)
_cell_angle_alpha                72.758(13)
_cell_angle_beta                 83.095(11)
_cell_angle_gamma                82.579(12)
_cell_volume                     948.9(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             461
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8783
_exptl_absorpt_correction_T_max  0.9009
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5859
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.1102
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         25.05
_reflns_number_total             3360
_reflns_number_gt                1978
_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)+(0.0908P)²+1.2155P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3360
_refine_ls_number_parameters     287
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.2333
_refine_ls_wR_factor_gt          0.1877
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.037
_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 0.5000 1.0000 0.0000 0.0426(4) Uani 1 2 d S . .
N1 N 0.5283(6) 1.0867(6) 0.1263(4) 0.0414(13) Uani 1 1 d . . .
N2 N 0.6951(6) 1.1952(6) 0.1937(4) 0.0465(14) Uani 1 1 d . . .
H4 H 0.7805 1.2367 0.2010 0.056 Uiso 1 1 calc R . .
N3 N 0.9297(6) 1.2067(6) -0.0131(4) 0.0433(13) Uani 1 1 d . . .
H5 H 0.9822 1.2515 0.0195 0.052 Uiso 1 1 calc R . .
N4 N 0.7351(6) 1.0904(6) -0.0499(4) 0.0387(12) Uani 1 1 d . . .
O1 O 0.6240(5) 0.7773(5) 0.0837(4) 0.0556(11) Uani 1 1 d U . .
O2 O 0.6757(9) 0.5513(8) 0.0625(6) 0.101(2) Uani 1 1 d . . .
H1 H 0.7355 0.5992 0.0133 0.151 Uiso 1 1 calc R . .
O3 O -0.0438(6) 0.3188(7) 0.2328(4) 0.0737(17) Uani 1 1 d . . .
O4 O 0.1186(5) 0.3422(6) 0.0856(4) 0.0545(13) Uani 1 1 d . . .
O5 O 0.7920(6) 0.9756(6) 0.5061(4) 0.0693(16) Uani 1 1 d . . .
O6 O 1.0147(6) 0.8650(7) 0.4327(5) 0.0778(18) Uani 1 1 d . . .
H2 H 1.0633 0.9179 0.4568 0.117 Uiso 1 1 calc R . .
C1 C 0.5868(8) 0.6471(8) 0.1117(6) 0.0538(11) Uani 1 1 d DU . .
C2 C 0.4497(7) 0.5702(7) 0.1944(5) 0.0461(12) Uani 1 1 d DU . .
C3 C 0.3418(7) 0.5005(7) 0.1555(5) 0.0432(16) Uani 1 1 d . . .
H3 H 0.3620 0.4966 0.0868 0.052 Uiso 1 1 calc R . .
C4 C 0.2034(7) 0.4360(7) 0.2165(5) 0.0375(14) Uani 1 1 d . . .
C5 C 0.0842(7) 0.3598(8) 0.1751(6) 0.0452(16) Uani 1 1 d . . .
C6 C 0.1771(8) 0.4430(8) 0.3190(5) 0.0475(17) Uani 1 1 d . . .
H6 H 0.0851 0.4016 0.3614 0.057 Uiso 1 1 calc R . .
C7 C 0.2867(7) 0.5112(7) 0.3587(5) 0.0448(16) Uani 1 1 d . . .
H7 H 0.2685 0.5140 0.4277 0.054 Uiso 1 1 calc R . .
C8 C 0.4227(7) 0.5748(7) 0.2965(5) 0.0386(15) Uani 1 1 d . . .
C9 C 0.5395(7) 0.6493(7) 0.3407(5) 0.0373(14) Uani 1 1 d . . .
C10 C 0.4715(7) 0.7442(7) 0.4014(5) 0.0431(16) Uani 1 1 d . . .
H10 H 0.3560 0.7577 0.4164 0.052 Uiso 1 1 calc R . .
C11 C 0.5756(7) 0.8180(7) 0.4391(5) 0.0453(16) Uani 1 1 d . . .
H11 H 0.5297 0.8816 0.4795 0.054 Uiso 1 1 calc R . .
C12 C 0.7479(7) 0.7989(7) 0.4177(5) 0.0367(14) Uani 1 1 d . . .
C13 C 0.8567(8) 0.8866(8) 0.4549(5) 0.0496(17) Uani 1 1 d . . .
C14 C 0.8158(7) 0.7006(7) 0.3602(5) 0.0426(16) Uani 1 1 d . . .
H14 H 0.9315 0.6849 0.3472 0.051 Uiso 1 1 calc R . .
C15 C 0.7121(7) 0.6254(7) 0.3221(4) 0.0407(15) Uani 1 1 d . . .
H15 H 0.7582 0.5588 0.2840 0.049 Uiso 1 1 calc R . .
C16 C 0.4556(8) 1.1007(8) 0.2204(5) 0.0502(17) Uani 1 1 d . . .
H16 H 0.3518 1.0687 0.2508 0.060 Uiso 1 1 calc R . .
C17 C 0.5559(8) 1.1674(8) 0.2629(5) 0.0517(17) Uani 1 1 d . . .
H17 H 0.5348 1.1900 0.3264 0.062 Uiso 1 1 calc R . .
C18 C 0.6736(7) 1.1461(7) 0.1132(5) 0.0375(14) Uani 1 1 d . . .
C19 C 0.7809(7) 1.1498(7) 0.0196(5) 0.0411(15) Uani 1 1 d . . .
C20 C 0.9820(7) 1.1809(8) -0.1062(5) 0.0456(16) Uani 1 1 d . . .
H20 H 1.0814 1.2071 -0.1466 0.055 Uiso 1 1 calc R . .
C21 C 0.8610(7) 1.1094(8) -0.1292(5) 0.0429(16) Uani 1 1 d . . .
H21 H 0.8635 1.0783 -0.1891 0.052 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
Co1 N4 2.126(5) 2_675 ?
Co1 N4 2.126(5) . ?
Co1 N1 2.129(5) 2_675 ?
Co1 N1 2.129(5) . ?
Co1 O1 2.210(4) 2_675 ?
Co1 O1 2.210(4) . ?
N1 C18 1.330(7) . ?
N1 C16 1.366(8) . ?
N2 C18 1.330(7) . ?
N2 C17 1.369(8) . ?
N2 H4 0.8600 . ?
N3 C19 1.346(7) . ?
N3 C20 1.352(8) . ?
N3 H5 0.8600 . ?
N4 C19 1.325(8) . ?
N4 C21 1.370(8) . ?
O1 C1 1.218(8) . ?
O2 C1 1.346(9) . ?
O2 H1 0.8200 . ?
O3 C5 1.244(8) . ?
O4 C5 1.256(7) . ?
O5 C13 1.252(7) . ?
O6 C13 1.277(7) . ?
O6 H2 0.8200 . ?
C1 C2 1.551(9) . ?
C2 C8 1.378(9) . ?
C2 C3 1.380(8) . ?
C3 C4 1.392(8) . ?
C3 H3 0.9300 . ?
C4 C6 1.390(8) . ?
C4 C5 1.507(8) . ?
C6 C7 1.388(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.380(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.505(7) . ?
C9 C15 1.385(8) . ?
C9 C10 1.390(8) . ?
C10 C11 1.373(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(8) . ?
C11 H11 0.9300 . ?
C12 C14 1.383(8) . ?
C12 C13 1.488(8) . ?
C14 C15 1.383(8) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.347(9) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.434(9) . ?
C20 C21 1.360(8) . ?
C20 H20 0.9300 . ?
C21 H21 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
N4 Co1 N4 179.999(1) 2_675 . ?
N4 Co1 N1 79.61(19) 2_675 2_675 ?
N4 Co1 N1 100.39(19) . 2_675 ?
N4 Co1 N1 100.39(19) 2_675 . ?
N4 Co1 N1 79.61(19) . . ?
N1 Co1 N1 180.0(2) 2_675 . ?
N4 Co1 O1 91.44(17) 2_675 2_675 ?
N4 Co1 O1 88.56(17) . 2_675 ?
N1 Co1 O1 90.10(18) 2_675 2_675 ?
N1 Co1 O1 89.90(18) . 2_675 ?
N4 Co1 O1 88.56(17) 2_675 . ?
N4 Co1 O1 91.44(17) . . ?
N1 Co1 O1 89.90(18) 2_675 . ?
N1 Co1 O1 90.10(18) . . ?
O1 Co1 O1 179.999(1) 2_675 . ?
C18 N1 C16 105.0(5) . . ?
C18 N1 Co1 111.1(4) . . ?
C16 N1 Co1 143.8(4) . . ?
C18 N2 C17 107.3(5) . . ?
C18 N2 H4 126.4 . . ?
C17 N2 H4 126.4 . . ?
C19 N3 C20 107.8(5) . . ?
C19 N3 H5 126.1 . . ?
C20 N3 H5 126.1 . . ?
C19 N4 C21 106.1(5) . . ?
C19 N4 Co1 111.1(4) . . ?
C21 N4 Co1 142.8(4) . . ?
C1 O1 Co1 135.2(4) . . ?
C1 O2 H1 109.5 . . ?
C13 O6 H2 109.5 . . ?
O1 C1 O2 116.2(7) . . ?
O1 C1 C2 131.1(7) . . ?
O2 C1 C2 112.7(6) . . ?
C8 C2 C3 119.8(6) . . ?
C8 C2 C1 126.3(5) . . ?
C3 C2 C1 113.8(6) . . ?
C2 C3 C4 121.6(6) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C6 117.9(5) . . ?
C3 C4 C5 122.3(6) . . ?
C6 C4 C5 119.9(6) . . ?
O3 C5 O4 124.2(6) . . ?
O3 C5 C4 116.9(6) . . ?
O4 C5 C4 118.9(6) . . ?
C7 C6 C4 120.6(6) . . ?
C7 C6 H6 119.7 . . ?
C4 C6 H6 119.7 . . ?
C8 C7 C6 120.5(6) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C2 C8 C7 119.7(5) . . ?
C2 C8 C9 120.6(5) . . ?
C7 C8 C9 119.7(5) . . ?
C15 C9 C10 119.7(5) . . ?
C15 C9 C8 121.4(5) . . ?
C10 C9 C8 118.8(5) . . ?
C11 C10 C9 119.8(6) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 120.8(6) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C14 119.4(5) . . ?
C11 C12 C13 119.5(6) . . ?
C14 C12 C13 121.1(5) . . ?
O5 C13 O6 123.2(6) . . ?
O5 C13 C12 119.8(6) . . ?
O6 C13 C12 117.0(6) . . ?
C15 C14 C12 120.2(5) . . ?
C15 C14 H14 119.9 . . ?
C12 C14 H14 119.9 . . ?
C14 C15 C9 120.0(6) . . ?
C14 C15 H15 120.0 . . ?
C9 C15 H15 120.0 . . ?
C17 C16 N1 110.1(6) . . ?
C17 C16 H16 124.9 . . ?
N1 C16 H16 124.9 . . ?
C16 C17 N2 106.1(6) . . ?
C16 C17 H17 126.9 . . ?
N2 C17 H17 126.9 . . ?
N2 C18 N1 111.4(5) . . ?
N2 C18 C19 129.8(5) . . ?
N1 C18 C19 118.8(5) . . ?
N4 C19 N3 110.4(6) . . ?
N4 C19 C18 119.4(5) . . ?
N3 C19 C18 130.2(6) . . ?
N3 C20 C21 106.7(5) . . ?
N3 C20 H20 126.6 . . ?
C21 C20 H20 126.6 . . ?
C20 C21 N4 109.0(5) . . ?
C20 C21 H21 125.5 . . ?
N4 C21 H21 125.5 . . ?

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
N4 Co1 N1 C18 177.9(4) 2_675 . . . ?
N4 Co1 N1 C18 -2.1(4) . . . . ?
N1 Co1 N1 C18 -153(38) 2_675 . . . ?
O1 Co1 N1 C18 -90.6(4) 2_675 . . . ?
O1 Co1 N1 C18 89.4(4) . . . . ?
N4 Co1 N1 C16 1.5(8) 2_675 . . . ?
N4 Co1 N1 C16 -178.5(8) . . . . ?
N1 Co1 N1 C16 31(38) 2_675 . . . ?
O1 Co1 N1 C16 93.0(7) 2_675 . . . ?
O1 Co1 N1 C16 -87.0(7) . . . . ?
N4 Co1 N4 C19 -54(48) 2_675 . . . ?
N1 Co1 N4 C19 -178.9(4) 2_675 . . . ?
N1 Co1 N4 C19 1.2(4) . . . . ?
O1 Co1 N4 C19 91.3(4) 2_675 . . . ?
O1 Co1 N4 C19 -88.7(4) . . . . ?
N4 Co1 N4 C21 125(48) 2_675 . . . ?
N1 Co1 N4 C21 0.3(7) 2_675 . . . ?
N1 Co1 N4 C21 -179.7(7) . . . . ?
O1 Co1 N4 C21 -89.5(7) 2_675 . . . ?
O1 Co1 N4 C21 90.5(7) . . . . ?
N4 Co1 O1 C1 23.8(7) 2_675 . . . ?
N4 Co1 O1 C1 -156.2(7) . . . . ?
N1 Co1 O1 C1 -55.8(7) 2_675 . . . ?
N1 Co1 O1 C1 124.2(7) . . . . ?
O1 Co1 O1 C1 -19(23) 2_675 . . . ?
Co1 O1 C1 O2 111.6(7) . . . . ?
Co1 O1 C1 C2 -66.9(10) . . . . ?
O1 C1 C2 C8 -51.5(11) . . . . ?
O2 C1 C2 C8 130.0(8) . . . . ?
O1 C1 C2 C3 124.2(8) . . . . ?
O2 C1 C2 C3 -54.3(8) . . . . ?
C8 C2 C3 C4 1.0(9) . . . . ?
C1 C2 C3 C4 -175.0(6) . . . . ?
C2 C3 C4 C6 -0.3(9) . . . . ?
C2 C3 C4 C5 179.9(6) . . . . ?
C3 C4 C5 O3 -173.3(6) . . . . ?
C6 C4 C5 O3 6.9(9) . . . . ?
C3 C4 C5 O4 6.3(9) . . . . ?
C6 C4 C5 O4 -173.5(6) . . . . ?
C3 C4 C6 C7 -0.6(9) . . . . ?
C5 C4 C6 C7 179.3(6) . . . . ?
C4 C6 C7 C8 0.8(10) . . . . ?
C3 C2 C8 C7 -0.8(9) . . . . ?
C1 C2 C8 C7 174.6(6) . . . . ?
C3 C2 C8 C9 179.6(6) . . . . ?
C1 C2 C8 C9 -5.0(10) . . . . ?
C6 C7 C8 C2 -0.1(10) . . . . ?
C6 C7 C8 C9 179.5(6) . . . . ?
C2 C8 C9 C15 -44.0(9) . . . . ?
C7 C8 C9 C15 136.3(6) . . . . ?
C2 C8 C9 C10 135.9(6) . . . . ?
C7 C8 C9 C10 -43.7(9) . . . . ?
C15 C9 C10 C11 2.5(10) . . . . ?
C8 C9 C10 C11 -177.5(6) . . . . ?
C9 C10 C11 C12 -0.1(10) . . . . ?
C10 C11 C12 C14 -2.0(10) . . . . ?
C10 C11 C12 C13 176.8(6) . . . . ?
C11 C12 C13 O5 0.7(10) . . . . ?
C14 C12 C13 O5 179.5(6) . . . . ?
C11 C12 C13 O6 -179.8(6) . . . . ?
C14 C12 C13 O6 -1.0(10) . . . . ?
C11 C12 C14 C15 1.8(10) . . . . ?
C13 C12 C14 C15 -177.0(6) . . . . ?
C12 C14 C15 C9 0.5(9) . . . . ?
C10 C9 C15 C14 -2.6(10) . . . . ?
C8 C9 C15 C14 177.3(5) . . . . ?
C18 N1 C16 C17 0.0(7) . . . . ?
Co1 N1 C16 C17 176.6(5) . . . . ?
N1 C16 C17 N2 -0.3(8) . . . . ?
C18 N2 C17 C16 0.4(7) . . . . ?
C17 N2 C18 N1 -0.4(7) . . . . ?
C17 N2 C18 C19 179.3(6) . . . . ?
C16 N1 C18 N2 0.2(7) . . . . ?
Co1 N1 C18 N2 -177.6(4) . . . . ?
C16 N1 C18 C19 -179.5(5) . . . . ?
Co1 N1 C18 C19 2.7(7) . . . . ?
C21 N4 C19 N3 0.6(7) . . . . ?
Co1 N4 C19 N3 -179.9(4) . . . . ?
C21 N4 C19 C18 -179.6(5) . . . . ?
Co1 N4 C19 C18 -0.1(7) . . . . ?
C20 N3 C19 N4 -0.9(7) . . . . ?
C20 N3 C19 C18 179.4(6) . . . . ?
N2 C18 C19 N4 178.5(6) . . . . ?
N1 C18 C19 N4 -1.8(9) . . . . ?
N2 C18 C19 N3 -1.8(11) . . . . ?
N1 C18 C19 N3 177.9(6) . . . . ?
C19 N3 C20 C21 0.7(7) . . . . ?
N3 C20 C21 N4 -0.4(7) . . . . ?
C19 N4 C21 C20 -0.2(7) . . . . ?
Co1 N4 C21 C20 -179.3(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H4 O3 0.86 1.84 2.696(6) 173.4 1_665
N3 H5 O4 0.86 1.90 2.762(6) 174.3 1_665
O2 H1 O4 0.82 1.68 2.482(8) 166.8 2_665
O6 H2 O5 0.82 1.82 2.629(6) 168.4 2_776

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.086
####################################################################### 
# 
# 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_241-10cd3
_database_code_depnum_ccdc_archive 'CCDC 1430227'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H30 Cd N8 O12'
_chemical_formula_weight         951.14

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.0767(4)
_cell_length_b                   9.4789(8)
_cell_length_c                   13.3988(11)
_cell_angle_alpha                73.886(7)
_cell_angle_beta                 83.844(5)
_cell_angle_gamma                80.810(6)
_cell_volume                     970.70(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             482
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8612
_exptl_absorpt_correction_T_max  0.8878
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6260
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.1045
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.63
_diffrn_reflns_theta_max         25.04
_reflns_number_total             3446
_reflns_number_gt                2256
_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)+(0.0468P)²+0.0182P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3446
_refine_ls_number_parameters     287
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1428
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.066
_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
Cd1 Cd 0.5000 0.5000 0.5000 0.0532(3) Uani 1 2 d S . .
N1 N 0.2526(5) 0.4026(5) 0.5506(4) 0.0445(13) Uani 1 1 d . . .
N2 N 0.0656(5) 0.2858(5) 0.5124(4) 0.0446(13) Uani 1 1 d . . .
H4 H 0.0151 0.2414 0.4791 0.054 Uiso 1 1 calc R . .
N3 N 0.2801(5) 0.3027(5) 0.3034(4) 0.0464(13) Uani 1 1 d . . .
H5 H 0.1938 0.2629 0.2986 0.056 Uiso 1 1 calc R . .
N4 N 0.4556(5) 0.4026(5) 0.3675(4) 0.0459(13) Uani 1 1 d . . .
O1 O 0.6286(4) 0.2580(4) 0.6001(3) 0.0545(9) Uani 1 1 d U . .
O2 O 0.6795(6) 0.0409(5) 0.5649(4) 0.0745(15) Uani 1 1 d . . .
H1 H 0.7381 0.0871 0.5170 0.112 Uiso 1 1 calc R . .
O3 O 0.7941(5) 0.4752(5) 1.0069(4) 0.0671(14) Uani 1 1 d . . .
O4 O 1.0195(5) 0.3621(5) 0.9356(4) 0.0772(16) Uani 1 1 d . . .
H2 H 1.0662 0.4151 0.9593 0.116 Uiso 1 1 calc R . .
O5 O -0.0201(5) -0.1860(6) 0.7383(3) 0.0734(16) Uani 1 1 d . . .
O6 O 0.1250(4) -0.1517(5) 0.5857(3) 0.0536(12) Uani 1 1 d . . .
C1 C 0.5985(7) 0.1315(7) 0.6186(5) 0.0503(10) Uani 1 1 d U . .
C2 C 0.4631(6) 0.0620(6) 0.6978(5) 0.0448(11) Uani 1 1 d U . .
C3 C 0.3549(6) -0.0066(6) 0.6584(4) 0.0390(14) Uani 1 1 d . . .
H3 H 0.3740 -0.0137 0.5902 0.047 Uiso 1 1 calc R . .
C4 C 0.2178(6) -0.0651(6) 0.7198(4) 0.0353(13) Uani 1 1 d . . .
C5 C 0.1000(6) -0.1394(6) 0.6777(5) 0.0402(15) Uani 1 1 d . . .
C6 C 0.1945(6) -0.0561(6) 0.8212(4) 0.0397(14) Uani 1 1 d . . .
H6 H 0.1050 -0.0954 0.8637 0.048 Uiso 1 1 calc R . .
C7 C 0.3033(6) 0.0111(6) 0.8606(4) 0.0409(15) Uani 1 1 d . . .
H7 H 0.2859 0.0156 0.9294 0.049 Uiso 1 1 calc R . .
C8 C 0.4376(6) 0.0716(6) 0.7995(4) 0.0376(14) Uani 1 1 d . . .
C9 C 0.5498(6) 0.1460(6) 0.8443(4) 0.0335(13) Uani 1 1 d . . .
C10 C 0.4818(6) 0.2438(6) 0.9017(4) 0.0424(15) Uani 1 1 d . . .
H10 H 0.3659 0.2596 0.9150 0.051 Uiso 1 1 calc R . .
C11 C 0.5829(7) 0.3188(6) 0.9397(4) 0.0429(15) Uani 1 1 d . . .
H11 H 0.5347 0.3851 0.9778 0.052 Uiso 1 1 calc R . .
C12 C 0.7547(6) 0.2957(6) 0.9215(4) 0.0388(14) Uani 1 1 d . . .
C13 C 0.8625(7) 0.3826(7) 0.9580(5) 0.0461(16) Uani 1 1 d . . .
C14 C 0.8242(6) 0.1936(6) 0.8671(4) 0.0383(14) Uani 1 1 d . . .
H14 H 0.9404 0.1762 0.8556 0.046 Uiso 1 1 calc R . .
C15 C 0.7255(6) 0.1177(6) 0.8298(4) 0.0396(14) Uani 1 1 d . . .
H15 H 0.7746 0.0476 0.7950 0.047 Uiso 1 1 calc R . .
C16 C 0.1304(7) 0.3801(7) 0.6318(5) 0.0510(17) Uani 1 1 d . . .
H16 H 0.1278 0.4086 0.6930 0.061 Uiso 1 1 calc R . .
C17 C 0.0148(7) 0.3088(7) 0.6059(5) 0.0492(17) Uani 1 1 d . . .
H17 H -0.0820 0.2811 0.6459 0.059 Uiso 1 1 calc R . .
C18 C 0.2092(6) 0.3442(6) 0.4799(4) 0.0386(14) Uani 1 1 d . . .
C19 C 0.3090(6) 0.3479(6) 0.3848(4) 0.0380(14) Uani 1 1 d . . .
C20 C 0.4081(7) 0.3292(7) 0.2292(5) 0.0526(17) Uani 1 1 d . . .
H20 H 0.4194 0.3093 0.1645 0.063 Uiso 1 1 calc R . .
C21 C 0.5169(7) 0.3915(7) 0.2702(5) 0.0530(17) Uani 1 1 d . . .
H21 H 0.6174 0.4217 0.2370 0.064 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.292(4) . ?
Cd1 N1 2.292(4) 2_666 ?
Cd1 N4 2.299(5) . ?
Cd1 N4 2.299(5) 2_666 ?
Cd1 O1 2.443(4) . ?
Cd1 O1 2.443(4) 2_666 ?
N1 C18 1.323(6) . ?
N1 C16 1.382(7) . ?
N2 C17 1.342(7) . ?
N2 C18 1.344(6) . ?
N2 H4 0.8600 . ?
N3 C19 1.331(6) . ?
N3 C20 1.358(7) . ?
N3 H5 0.8600 . ?
N4 C19 1.340(6) . ?
N4 C21 1.370(7) . ?
O1 C1 1.214(7) . ?
O2 C1 1.321(7) . ?
O2 H1 0.8200 . ?
O3 C13 1.262(6) . ?
O4 C13 1.268(6) . ?
O4 H2 0.8200 . ?
O5 C5 1.251(6) . ?
O6 C5 1.263(6) . ?
C1 C2 1.532(8) . ?
C2 C8 1.382(7) . ?
C2 C3 1.391(6) . ?
C3 C4 1.399(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.376(7) . ?
C4 C5 1.506(6) . ?
C6 C7 1.386(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.494(6) . ?
C9 C10 1.376(7) . ?
C9 C15 1.404(7) . ?
C10 C11 1.382(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.376(7) . ?
C11 H11 0.9300 . ?
C12 C14 1.384(7) . ?
C12 C13 1.490(7) . ?
C14 C15 1.368(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.360(7) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.427(7) . ?
C20 C21 1.368(8) . ?
C20 H20 0.9300 . ?
C21 H21 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
N1 Cd1 N1 180.0(2) . 2_666 ?
N1 Cd1 N4 75.18(15) . . ?
N1 Cd1 N4 104.82(15) 2_666 . ?
N1 Cd1 N4 104.82(15) . 2_666 ?
N1 Cd1 N4 75.18(15) 2_666 2_666 ?
N4 Cd1 N4 180.000(1) . 2_666 ?
N1 Cd1 O1 84.45(15) . . ?
N1 Cd1 O1 95.55(15) 2_666 . ?
N4 Cd1 O1 91.22(15) . . ?
N4 Cd1 O1 88.78(15) 2_666 . ?
N1 Cd1 O1 95.55(15) . 2_666 ?
N1 Cd1 O1 84.45(15) 2_666 2_666 ?
N4 Cd1 O1 88.78(15) . 2_666 ?
N4 Cd1 O1 91.22(15) 2_666 2_666 ?
O1 Cd1 O1 179.999(1) . 2_666 ?
C18 N1 C16 106.5(4) . . ?
C18 N1 Cd1 111.5(3) . . ?
C16 N1 Cd1 142.0(4) . . ?
C17 N2 C18 107.9(4) . . ?
C17 N2 H4 126.0 . . ?
C18 N2 H4 126.0 . . ?
C19 N3 C20 109.4(4) . . ?
C19 N3 H5 125.3 . . ?
C20 N3 H5 125.3 . . ?
C19 N4 C21 105.7(4) . . ?
C19 N4 Cd1 111.1(4) . . ?
C21 N4 Cd1 142.8(3) . . ?
C1 O1 Cd1 135.3(4) . . ?
C1 O2 H1 109.5 . . ?
C13 O4 H2 109.5 . . ?
O1 C1 O2 120.6(6) . . ?
O1 C1 C2 126.2(6) . . ?
O2 C1 C2 113.1(5) . . ?
C8 C2 C3 120.1(5) . . ?
C8 C2 C1 124.9(4) . . ?
C3 C2 C1 114.9(5) . . ?
C2 C3 C4 121.1(5) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C6 C4 C3 118.3(4) . . ?
C6 C4 C5 120.3(5) . . ?
C3 C4 C5 121.4(5) . . ?
O5 C5 O6 123.5(5) . . ?
O5 C5 C4 116.4(5) . . ?
O6 C5 C4 120.1(5) . . ?
C4 C6 C7 120.5(5) . . ?
C4 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C6 C7 C8 121.4(5) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C2 C8 C7 118.6(4) . . ?
C2 C8 C9 121.7(5) . . ?
C7 C8 C9 119.7(5) . . ?
C10 C9 C15 118.5(4) . . ?
C10 C9 C8 120.2(5) . . ?
C15 C9 C8 121.3(5) . . ?
C9 C10 C11 121.1(5) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C12 C11 C10 120.2(5) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C14 118.9(5) . . ?
C11 C12 C13 120.0(5) . . ?
C14 C12 C13 121.1(5) . . ?
O3 C13 O4 123.2(5) . . ?
O3 C13 C12 119.1(5) . . ?
O4 C13 C12 117.7(5) . . ?
C15 C14 C12 121.3(5) . . ?
C15 C14 H14 119.3 . . ?
C12 C14 H14 119.3 . . ?
C14 C15 C9 119.8(5) . . ?
C14 C15 H15 120.1 . . ?
C9 C15 H15 120.1 . . ?
C17 C16 N1 107.7(5) . . ?
C17 C16 H16 126.1 . . ?
N1 C16 H16 126.1 . . ?
N2 C17 C16 107.6(5) . . ?
N2 C17 H17 126.2 . . ?
C16 C17 H17 126.2 . . ?
N1 C18 N2 110.2(5) . . ?
N1 C18 C19 121.4(4) . . ?
N2 C18 C19 128.4(5) . . ?
N3 C19 N4 109.9(5) . . ?
N3 C19 C18 129.5(4) . . ?
N4 C19 C18 120.6(5) . . ?
N3 C20 C21 105.2(5) . . ?
N3 C20 H20 127.4 . . ?
C21 C20 H20 127.4 . . ?
C20 C21 N4 109.8(5) . . ?
C20 C21 H21 125.1 . . ?
N4 C21 H21 125.1 . . ?

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 Cd1 N1 C18 -144(16) 2_666 . . . ?
N4 Cd1 N1 C18 -1.1(4) . . . . ?
N4 Cd1 N1 C18 178.9(4) 2_666 . . . ?
O1 Cd1 N1 C18 -93.9(4) . . . . ?
O1 Cd1 N1 C18 86.1(4) 2_666 . . . ?
N1 Cd1 N1 C16 35(16) 2_666 . . . ?
N4 Cd1 N1 C16 177.2(7) . . . . ?
N4 Cd1 N1 C16 -2.8(7) 2_666 . . . ?
O1 Cd1 N1 C16 84.5(7) . . . . ?
O1 Cd1 N1 C16 -95.5(7) 2_666 . . . ?
N1 Cd1 N4 C19 3.1(4) . . . . ?
N1 Cd1 N4 C19 -176.9(4) 2_666 . . . ?
N4 Cd1 N4 C19 -135(38) 2_666 . . . ?
O1 Cd1 N4 C19 87.0(4) . . . . ?
O1 Cd1 N4 C19 -93.0(4) 2_666 . . . ?
N1 Cd1 N4 C21 174.2(7) . . . . ?
N1 Cd1 N4 C21 -5.8(7) 2_666 . . . ?
N4 Cd1 N4 C21 36(38) 2_666 . . . ?
O1 Cd1 N4 C21 -101.9(7) . . . . ?
O1 Cd1 N4 C21 78.1(7) 2_666 . . . ?
N1 Cd1 O1 C1 33.2(6) . . . . ?
N1 Cd1 O1 C1 -146.8(6) 2_666 . . . ?
N4 Cd1 O1 C1 -41.7(6) . . . . ?
N4 Cd1 O1 C1 138.3(6) 2_666 . . . ?
O1 Cd1 O1 C1 -56(22) 2_666 . . . ?
Cd1 O1 C1 O2 98.4(7) . . . . ?
Cd1 O1 C1 C2 -77.9(9) . . . . ?
O1 C1 C2 C8 -48.3(10) . . . . ?
O2 C1 C2 C8 135.2(6) . . . . ?
O1 C1 C2 C3 127.7(7) . . . . ?
O2 C1 C2 C3 -48.9(8) . . . . ?
C8 C2 C3 C4 0.9(9) . . . . ?
C1 C2 C3 C4 -175.2(5) . . . . ?
C2 C3 C4 C6 -1.4(8) . . . . ?
C2 C3 C4 C5 180.0(5) . . . . ?
C6 C4 C5 O5 2.5(8) . . . . ?
C3 C4 C5 O5 -179.0(5) . . . . ?
C6 C4 C5 O6 -177.7(5) . . . . ?
C3 C4 C5 O6 0.9(9) . . . . ?
C3 C4 C6 C7 0.8(8) . . . . ?
C5 C4 C6 C7 179.4(5) . . . . ?
C4 C6 C7 C8 0.4(9) . . . . ?
C3 C2 C8 C7 0.3(9) . . . . ?
C1 C2 C8 C7 176.0(6) . . . . ?
C3 C2 C8 C9 -179.3(5) . . . . ?
C1 C2 C8 C9 -3.5(9) . . . . ?
C6 C7 C8 C2 -0.9(9) . . . . ?
C6 C7 C8 C9 178.6(5) . . . . ?
C2 C8 C9 C10 134.3(6) . . . . ?
C7 C8 C9 C10 -45.3(8) . . . . ?
C2 C8 C9 C15 -46.2(8) . . . . ?
C7 C8 C9 C15 134.3(6) . . . . ?
C15 C9 C10 C11 3.4(9) . . . . ?
C8 C9 C10 C11 -177.0(5) . . . . ?
C9 C10 C11 C12 -0.6(9) . . . . ?
C10 C11 C12 C14 -1.7(9) . . . . ?
C10 C11 C12 C13 176.8(6) . . . . ?
C11 C12 C13 O3 1.1(9) . . . . ?
C14 C12 C13 O3 179.7(6) . . . . ?
C11 C12 C13 O4 -177.1(6) . . . . ?
C14 C12 C13 O4 1.5(9) . . . . ?
C11 C12 C14 C15 1.2(9) . . . . ?
C13 C12 C14 C15 -177.4(5) . . . . ?
C12 C14 C15 C9 1.7(9) . . . . ?
C10 C9 C15 C14 -3.9(8) . . . . ?
C8 C9 C15 C14 176.5(5) . . . . ?
C18 N1 C16 C17 -0.6(7) . . . . ?
Cd1 N1 C16 C17 -179.0(5) . . . . ?
C18 N2 C17 C16 -1.0(7) . . . . ?
N1 C16 C17 N2 1.0(7) . . . . ?
C16 N1 C18 N2 0.0(7) . . . . ?
Cd1 N1 C18 N2 178.9(4) . . . . ?
C16 N1 C18 C19 -179.9(5) . . . . ?
Cd1 N1 C18 C19 -1.0(7) . . . . ?
C17 N2 C18 N1 0.7(7) . . . . ?
C17 N2 C18 C19 -179.4(6) . . . . ?
C20 N3 C19 N4 -0.9(7) . . . . ?
C20 N3 C19 C18 179.2(6) . . . . ?
C21 N4 C19 N3 0.8(6) . . . . ?
Cd1 N4 C19 N3 175.2(4) . . . . ?
C21 N4 C19 C18 -179.3(5) . . . . ?
Cd1 N4 C19 C18 -4.9(7) . . . . ?
N1 C18 C19 N3 -175.8(6) . . . . ?
N2 C18 C19 N3 4.3(10) . . . . ?
N1 C18 C19 N4 4.3(9) . . . . ?
N2 C18 C19 N4 -175.6(5) . . . . ?
C19 N3 C20 C21 0.5(7) . . . . ?
N3 C20 C21 N4 -0.1(7) . . . . ?
C19 N4 C21 C20 -0.4(7) . . . . ?
Cd1 N4 C21 C20 -171.8(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H4 O6 0.86 1.92 2.774(5) 172.2 2_556
N3 H5 O5 0.86 1.85 2.699(5) 169.2 2_556
O2 H1 O6 0.82 1.71 2.517(5) 169.4 2_656
O4 H2 O3 0.82 1.82 2.625(5) 168.0 2_767

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_239-4ni
_database_code_depnum_ccdc_archive 'CCDC 1430228'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H30 N4 Ni O9'
_chemical_formula_weight         757.38

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           Orthorhombic
_symmetry_space_group_name_H-M   Pna21

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

_cell_length_a                   14.400(2)
_cell_length_b                   13.9197(17)
_cell_length_c                   17.1576(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3439.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8485
_exptl_absorpt_correction_T_max  0.8637
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12889
_diffrn_reflns_av_R_equivalents  0.1370
_diffrn_reflns_av_sigmaI/netI    0.2096
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         25.05
_reflns_number_total             5728
_reflns_number_gt                2681
_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)+(0.0687P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         5728
_refine_ls_number_parameters     478
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1888
_refine_ls_R_factor_gt           0.0937
_refine_ls_wR_factor_ref         0.2294
_refine_ls_wR_factor_gt          0.1745
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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
Ni1 Ni 0.38985(10) 0.52076(9) 0.71747(8) 0.0363(4) Uani 1 1 d . . .
N1 N 0.4052(7) 0.3726(6) 0.7339(5) 0.043(3) Uani 1 1 d . . .
N2 N 0.5291(7) 0.5015(7) 0.6830(4) 0.038(3) Uani 1 1 d . . .
N3 N 0.3980(7) 0.6691(6) 0.7025(6) 0.045(3) Uani 1 1 d . . .
N4 N 0.4278(7) 0.5634(7) 0.8298(5) 0.044(3) Uani 1 1 d . . .
O1 O 0.3524(7) 0.4976(5) 0.6024(4) 0.048(2) Uani 1 1 d . . .
O2 O 0.1981(6) 0.5062(6) 0.6030(4) 0.054(2) Uani 1 1 d . . .
O3 O 0.2716(7) 0.1549(5) 0.4533(5) 0.056(3) Uani 1 1 d . . .
O4 O 0.2860(7) 0.1740(5) 0.3241(4) 0.056(3) Uani 1 1 d . . .
O5 O 0.2586(7) 0.9767(5) 0.4489(5) 0.059(3) Uani 1 1 d . . .
H5 H 0.2707 1.0343 0.4497 0.088 Uiso 1 1 calc R . .
O6 O 0.4111(8) 0.9604(6) 0.4244(6) 0.075(3) Uani 1 1 d . . .
O7 O 0.2531(6) 0.5089(4) 0.7516(4) 0.044(2) Uani 1 1 d . . .
H1W H 0.2194 0.5120 0.7132 0.052 Uiso 1 1 d R . .
H2W H 0.2407 0.5612 0.7748 0.052 Uiso 1 1 d R . .
O8 O 0.1571(7) 0.7171(7) 0.6661(6) 0.098(4) Uani 1 1 d . . .
H3W H 0.1739 0.7051 0.7125 0.117 Uiso 1 1 d R . .
H4W H 0.1680 0.6610 0.6487 0.117 Uiso 1 1 d R . .
O9 O 0.0097(9) 0.4747(8) 0.5663(7) 0.119(5) Uani 1 1 d . . .
H5W H 0.0665 0.4838 0.5775 0.143 Uiso 1 1 d R . .
H6W H -0.0190 0.4930 0.5256 0.143 Uiso 1 1 d R . .
C1 C 0.2744(9) 0.4896(7) 0.5703(6) 0.031(3) Uani 1 1 d . . .
C2 C 0.2760(8) 0.4528(8) 0.4868(6) 0.036(3) Uani 1 1 d . . .
C3 C 0.2738(8) 0.3532(7) 0.4757(5) 0.032(3) Uani 1 1 d . . .
H3 H 0.2692 0.3131 0.5189 0.038 Uiso 1 1 calc R . .
C4 C 0.2783(7) 0.3127(7) 0.4019(6) 0.026(2) Uani 1 1 d . . .
C5 C 0.2770(8) 0.2055(8) 0.3912(7) 0.039(3) Uani 1 1 d . . .
C6 C 0.2884(10) 0.3741(8) 0.3388(6) 0.052(4) Uani 1 1 d . . .
H6 H 0.2906 0.3484 0.2888 0.063 Uiso 1 1 calc R . .
C7 C 0.2952(10) 0.4728(8) 0.3482(6) 0.050(4) Uani 1 1 d . . .
H7A H 0.3048 0.5118 0.3049 0.060 Uiso 1 1 calc R . .
C8 C 0.2876(9) 0.5146(7) 0.4226(6) 0.037(3) Uani 1 1 d . . .
C9 C 0.2948(8) 0.6185(7) 0.4284(6) 0.033(3) Uani 1 1 d . . .
C10 C 0.3731(10) 0.6646(7) 0.3988(7) 0.055(4) Uani 1 1 d . . .
H10 H 0.4193 0.6268 0.3766 0.066 Uiso 1 1 calc R . .
C11 C 0.3867(9) 0.7632(7) 0.4002(7) 0.050(3) Uani 1 1 d . . .
H11 H 0.4404 0.7903 0.3796 0.060 Uiso 1 1 calc R . .
C12 C 0.3173(10) 0.8212(8) 0.4333(7) 0.044(3) Uani 1 1 d . . .
C13 C 0.3341(11) 0.9281(8) 0.4360(6) 0.044(3) Uani 1 1 d . . .
C14 C 0.2413(10) 0.7791(8) 0.4638(7) 0.048(3) Uani 1 1 d . . .
H14 H 0.1952 0.8172 0.4859 0.058 Uiso 1 1 calc R . .
C15 C 0.2302(10) 0.6789(7) 0.4629(6) 0.041(3) Uani 1 1 d . . .
H15 H 0.1780 0.6522 0.4862 0.049 Uiso 1 1 calc R . .
C16 C 0.3444(10) 0.3103(9) 0.7642(6) 0.047(3) Uani 1 1 d . . .
H16 H 0.2886 0.3326 0.7847 0.057 Uiso 1 1 calc R . .
C17 C 0.3642(11) 0.2120(9) 0.7652(7) 0.054(4) Uani 1 1 d . . .
H17 H 0.3191 0.1694 0.7828 0.065 Uiso 1 1 calc R . .
C18 C 0.4439(14) 0.1785(10) 0.7423(9) 0.081(6) Uani 1 1 d . . .
H18 H 0.4567 0.1133 0.7471 0.097 Uiso 1 1 calc R . .
C19 C 0.5118(11) 0.2419(8) 0.7098(8) 0.059(4) Uani 1 1 d . . .
C20 C 0.4910(8) 0.3391(7) 0.7091(7) 0.039(3) Uani 1 1 d . . .
C21 C 0.6027(14) 0.2132(12) 0.6817(9) 0.080(5) Uani 1 1 d . . .
H21 H 0.6188 0.1485 0.6821 0.096 Uiso 1 1 calc R . .
C22 C 0.6634(12) 0.2772(13) 0.6556(9) 0.078(5) Uani 1 1 d . . .
H22 H 0.7202 0.2562 0.6362 0.093 Uiso 1 1 calc R . .
C23 C 0.6429(11) 0.3801(10) 0.6566(7) 0.058(4) Uani 1 1 d . . .
C24 C 0.5564(9) 0.4100(9) 0.6816(6) 0.045(3) Uani 1 1 d . . .
C25 C 0.7034(11) 0.4523(15) 0.6290(7) 0.076(5) Uani 1 1 d . . .
H25 H 0.7609 0.4357 0.6084 0.092 Uiso 1 1 calc R . .
C26 C 0.6767(12) 0.5485(12) 0.6328(7) 0.069(4) Uani 1 1 d . . .
H26 H 0.7165 0.5977 0.6177 0.083 Uiso 1 1 calc R . .
C27 C 0.5904(10) 0.5667(10) 0.6595(7) 0.056(4) Uani 1 1 d . . .
H27 H 0.5722 0.6307 0.6617 0.067 Uiso 1 1 calc R . .
C28 C 0.3884(10) 0.7174(9) 0.6362(7) 0.056(4) Uani 1 1 d . . .
H28 H 0.3713 0.6851 0.5909 0.067 Uiso 1 1 calc R . .
C29 C 0.4039(12) 0.8154(11) 0.6343(9) 0.079(5) Uani 1 1 d . . .
H29 H 0.3962 0.8488 0.5878 0.095 Uiso 1 1 calc R . .
C30 C 0.4312(11) 0.8651(9) 0.7021(13) 0.094(6) Uani 1 1 d . . .
H30 H 0.4424 0.9309 0.7004 0.113 Uiso 1 1 calc R . .
C31 C 0.4410(11) 0.8155(8) 0.7698(8) 0.052(4) Uani 1 1 d . . .
C32 C 0.4291(9) 0.7178(9) 0.7674(7) 0.043(3) Uani 1 1 d . . .
C33 C 0.4703(11) 0.8588(11) 0.8384(9) 0.081(5) Uani 1 1 d . . .
H33 H 0.4802 0.9249 0.8394 0.097 Uiso 1 1 calc R . .
C34 C 0.4848(11) 0.8076(10) 0.9031(9) 0.070(4) Uani 1 1 d . . .
H34 H 0.5053 0.8390 0.9477 0.084 Uiso 1 1 calc R . .
C35 C 0.4693(9) 0.7030(10) 0.9063(6) 0.052(4) Uani 1 1 d . . .
C36 C 0.4425(9) 0.6594(9) 0.8355(7) 0.046(3) Uani 1 1 d . . .
C37 C 0.4819(11) 0.6459(12) 0.9703(7) 0.080(5) Uani 1 1 d . . .
H37 H 0.4983 0.6732 1.0178 0.095 Uiso 1 1 calc R . .
C38 C 0.4705(9) 0.5486(11) 0.9645(6) 0.060(4) Uani 1 1 d . . .
H38 H 0.4829 0.5088 1.0068 0.071 Uiso 1 1 calc R . .
C39 C 0.4395(9) 0.5097(9) 0.8933(7) 0.053(3) Uani 1 1 d . . .
H39 H 0.4268 0.4443 0.8905 0.063 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
Ni1 O1 2.073(7) . ?
Ni1 O7 2.061(8) . ?
Ni1 N3 2.084(9) . ?
Ni1 N1 2.093(9) . ?
Ni1 N2 2.107(10) . ?
Ni1 N4 2.089(9) . ?
N1 C16 1.338(14) . ?
N1 C20 1.387(14) . ?
N2 C27 1.329(14) . ?
N2 C24 1.333(14) . ?
N3 C28 1.327(14) . ?
N3 C32 1.379(15) . ?
N4 C39 1.333(14) . ?
N4 C36 1.357(14) . ?
O1 C1 1.256(13) . ?
O2 C1 1.255(14) . ?
O3 C5 1.280(14) . ?
O4 C5 1.239(13) . ?
O5 C13 1.300(15) . ?
O5 H5 0.8200 . ?
O6 C13 1.212(15) . ?
O7 H1W 0.8200 . ?
O7 H2W 0.8490 . ?
O8 H3W 0.8493 . ?
O8 H4W 0.8501 . ?
O9 H5W 0.8504 . ?
O9 H6W 0.8497 . ?
C1 C2 1.520(14) . ?
C2 C8 1.409(14) . ?
C2 C3 1.400(13) . ?
C3 C4 1.387(13) . ?
C3 H3 0.9300 . ?
C4 C6 1.388(13) . ?
C4 C5 1.503(13) . ?
C6 C7 1.387(14) . ?
C6 H6 0.9300 . ?
C7 C8 1.407(14) . ?
C7 H7A 0.9300 . ?
C8 C9 1.452(13) . ?
C9 C15 1.386(15) . ?
C9 C10 1.394(16) . ?
C10 C11 1.387(14) . ?
C10 H10 0.9300 . ?
C11 C12 1.405(16) . ?
C11 H11 0.9300 . ?
C12 C14 1.348(16) . ?
C12 C13 1.508(15) . ?
C14 C15 1.405(14) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.398(16) . ?
C16 H16 0.9300 . ?
C17 C18 1.299(19) . ?
C17 H17 0.9300 . ?
C18 C19 1.43(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.386(14) . ?
C19 C21 1.45(2) . ?
C20 C24 1.444(16) . ?
C21 C22 1.33(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.463(19) . ?
C22 H22 0.9300 . ?
C23 C24 1.382(17) . ?
C23 C25 1.411(19) . ?
C25 C26 1.40(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.348(18) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.383(17) . ?
C28 H28 0.9300 . ?
C29 C30 1.41(2) . ?
C29 H29 0.9300 . ?
C30 C31 1.36(2) . ?
C30 H30 0.9300 . ?
C31 C32 1.372(16) . ?
C31 C33 1.388(18) . ?
C32 C36 1.437(16) . ?
C33 C34 1.336(18) . ?
C33 H33 0.9300 . ?
C34 C35 1.473(17) . ?
C34 H34 0.9300 . ?
C35 C37 1.368(18) . ?
C35 C36 1.412(15) . ?
C37 C38 1.368(17) . ?
C37 H37 0.9300 . ?
C38 C39 1.409(15) . ?
C38 H38 0.9300 . ?
C39 H39 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
O1 Ni1 O7 90.6(3) . . ?
O1 Ni1 N3 92.9(4) . . ?
O7 Ni1 N3 99.7(3) . . ?
O1 Ni1 N1 90.1(3) . . ?
O7 Ni1 N1 89.1(3) . . ?
N3 Ni1 N1 170.7(4) . . ?
O1 Ni1 N2 87.7(3) . . ?
O7 Ni1 N2 168.1(3) . . ?
N3 Ni1 N2 92.2(4) . . ?
N1 Ni1 N2 79.2(4) . . ?
O1 Ni1 N4 172.4(4) . . ?
O7 Ni1 N4 90.6(3) . . ?
N3 Ni1 N4 79.5(4) . . ?
N1 Ni1 N4 97.4(4) . . ?
N2 Ni1 N4 92.6(4) . . ?
C16 N1 C20 119.0(10) . . ?
C16 N1 Ni1 128.4(9) . . ?
C20 N1 Ni1 112.6(8) . . ?
C27 N2 C24 116.8(12) . . ?
C27 N2 Ni1 129.1(10) . . ?
C24 N2 Ni1 114.0(8) . . ?
C28 N3 C32 118.5(10) . . ?
C28 N3 Ni1 127.0(8) . . ?
C32 N3 Ni1 113.9(8) . . ?
C39 N4 C36 118.3(10) . . ?
C39 N4 Ni1 128.9(8) . . ?
C36 N4 Ni1 112.8(7) . . ?
C1 O1 Ni1 131.6(8) . . ?
C13 O5 H5 109.5 . . ?
Ni1 O7 H1W 109.5 . . ?
Ni1 O7 H2W 105.4 . . ?
H1W O7 H2W 101.9 . . ?
H3W O8 H4W 95.6 . . ?
H5W O9 H6W 127.6 . . ?
O1 C1 O2 124.8(10) . . ?
O1 C1 C2 115.4(11) . . ?
O2 C1 C2 119.8(11) . . ?
C8 C2 C3 120.1(9) . . ?
C8 C2 C1 122.2(9) . . ?
C3 C2 C1 117.5(9) . . ?
C4 C3 C2 121.7(9) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C6 117.9(9) . . ?
C3 C4 C5 120.9(9) . . ?
C6 C4 C5 121.2(9) . . ?
O4 C5 O3 125.8(10) . . ?
O4 C5 C4 117.6(11) . . ?
O3 C5 C4 116.5(9) . . ?
C7 C6 C4 121.8(9) . . ?
C7 C6 H6 119.1 . . ?
C4 C6 H6 119.1 . . ?
C6 C7 C8 120.6(10) . . ?
C6 C7 H7A 119.7 . . ?
C8 C7 H7A 119.7 . . ?
C2 C8 C7 117.8(10) . . ?
C2 C8 C9 124.2(10) . . ?
C7 C8 C9 118.0(9) . . ?
C15 C9 C10 114.7(10) . . ?
C15 C9 C8 125.8(10) . . ?
C10 C9 C8 119.4(10) . . ?
C9 C10 C11 124.4(11) . . ?
C9 C10 H10 117.8 . . ?
C11 C10 H10 117.8 . . ?
C10 C11 C12 118.4(12) . . ?
C10 C11 H11 120.8 . . ?
C12 C11 H11 120.8 . . ?
C14 C12 C11 119.0(11) . . ?
C14 C12 C13 123.2(12) . . ?
C11 C12 C13 117.7(12) . . ?
O6 C13 O5 126.9(11) . . ?
O6 C13 C12 120.5(13) . . ?
O5 C13 C12 112.6(12) . . ?
C12 C14 C15 121.3(11) . . ?
C12 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C9 C15 C14 122.1(11) . . ?
C9 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
N1 C16 C17 120.3(12) . . ?
N1 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C18 C17 C16 121.9(13) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 120.0(13) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 117.3(14) . . ?
C20 C19 C21 117.4(13) . . ?
C18 C19 C21 125.3(13) . . ?
C19 C20 N1 121.1(12) . . ?
C19 C20 C24 122.0(12) . . ?
N1 C20 C24 116.8(10) . . ?
C22 C21 C19 121.5(15) . . ?
C22 C21 H21 119.2 . . ?
C19 C21 H21 119.2 . . ?
C21 C22 C23 121.4(15) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C24 C23 C25 116.5(14) . . ?
C24 C23 C22 118.7(14) . . ?
C25 C23 C22 124.7(16) . . ?
N2 C24 C23 124.0(12) . . ?
N2 C24 C20 117.0(11) . . ?
C23 C24 C20 118.9(12) . . ?
C23 C25 C26 119.8(14) . . ?
C23 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C27 C26 C25 116.8(15) . . ?
C27 C26 H26 121.6 . . ?
C25 C26 H26 121.6 . . ?
N2 C27 C26 126.0(14) . . ?
N2 C27 H27 117.0 . . ?
C26 C27 H27 117.0 . . ?
N3 C28 C29 120.2(12) . . ?
N3 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C28 C29 C30 120.7(14) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C29 C30 C31 119.0(13) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C32 C31 C30 117.7(13) . . ?
C32 C31 C33 119.6(13) . . ?
C30 C31 C33 122.4(13) . . ?
N3 C32 C31 123.5(12) . . ?
N3 C32 C36 115.0(10) . . ?
C31 C32 C36 121.3(12) . . ?
C34 C33 C31 121.3(14) . . ?
C34 C33 H33 119.3 . . ?
C31 C33 H33 119.3 . . ?
C33 C34 C35 122.4(13) . . ?
C33 C34 H34 118.8 . . ?
C35 C34 H34 118.8 . . ?
C37 C35 C36 118.5(13) . . ?
C37 C35 C34 125.8(12) . . ?
C36 C35 C34 115.7(12) . . ?
N4 C36 C35 121.9(11) . . ?
N4 C36 C32 118.5(10) . . ?
C35 C36 C32 119.6(12) . . ?
C35 C37 C38 120.1(12) . . ?
C35 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C39 C38 C37 118.8(12) . . ?
C39 C38 H38 120.6 . . ?
C37 C38 H38 120.6 . . ?
N4 C39 C38 122.3(12) . . ?
N4 C39 H39 118.9 . . ?
C38 C39 H39 118.9 . . ?

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 Ni1 N1 C16 -97.2(10) . . . . ?
O7 Ni1 N1 C16 -6.6(9) . . . . ?
N3 Ni1 N1 C16 154(2) . . . . ?
N2 Ni1 N1 C16 175.2(10) . . . . ?
N4 Ni1 N1 C16 83.9(10) . . . . ?
O1 Ni1 N1 C20 82.9(7) . . . . ?
O7 Ni1 N1 C20 173.5(7) . . . . ?
N3 Ni1 N1 C20 -26(3) . . . . ?
N2 Ni1 N1 C20 -4.7(7) . . . . ?
N4 Ni1 N1 C20 -96.0(7) . . . . ?
O1 Ni1 N2 C27 91.2(9) . . . . ?
O7 Ni1 N2 C27 173.0(13) . . . . ?
N3 Ni1 N2 C27 -1.7(9) . . . . ?
N1 Ni1 N2 C27 -178.3(10) . . . . ?
N4 Ni1 N2 C27 -81.3(9) . . . . ?
O1 Ni1 N2 C24 -85.5(7) . . . . ?
O7 Ni1 N2 C24 -3.6(18) . . . . ?
N3 Ni1 N2 C24 -178.3(7) . . . . ?
N1 Ni1 N2 C24 5.1(7) . . . . ?
N4 Ni1 N2 C24 102.1(7) . . . . ?
O1 Ni1 N3 C28 -5.0(11) . . . . ?
O7 Ni1 N3 C28 -96.1(11) . . . . ?
N1 Ni1 N3 C28 104(3) . . . . ?
N2 Ni1 N3 C28 82.8(11) . . . . ?
N4 Ni1 N3 C28 175.1(12) . . . . ?
O1 Ni1 N3 C32 -175.6(9) . . . . ?
O7 Ni1 N3 C32 93.3(9) . . . . ?
N1 Ni1 N3 C32 -67(3) . . . . ?
N2 Ni1 N3 C32 -87.8(9) . . . . ?
N4 Ni1 N3 C32 4.5(9) . . . . ?
O1 Ni1 N4 C39 177(3) . . . . ?
O7 Ni1 N4 C39 77.9(11) . . . . ?
N3 Ni1 N4 C39 177.6(12) . . . . ?
N1 Ni1 N4 C39 -11.3(12) . . . . ?
N2 Ni1 N4 C39 -90.7(11) . . . . ?
O1 Ni1 N4 C36 -4(3) . . . . ?
O7 Ni1 N4 C36 -102.7(8) . . . . ?
N3 Ni1 N4 C36 -3.0(8) . . . . ?
N1 Ni1 N4 C36 168.1(8) . . . . ?
N2 Ni1 N4 C36 88.7(8) . . . . ?
O7 Ni1 O1 C1 5.9(9) . . . . ?
N3 Ni1 O1 C1 -93.8(9) . . . . ?
N1 Ni1 O1 C1 95.0(10) . . . . ?
N2 Ni1 O1 C1 174.2(9) . . . . ?
N4 Ni1 O1 C1 -93(3) . . . . ?
Ni1 O1 C1 O2 9.1(16) . . . . ?
Ni1 O1 C1 C2 -168.1(7) . . . . ?
O1 C1 C2 C8 -86.6(14) . . . . ?
O2 C1 C2 C8 96.0(14) . . . . ?
O1 C1 C2 C3 87.8(13) . . . . ?
O2 C1 C2 C3 -89.5(13) . . . . ?
C8 C2 C3 C4 -3.1(18) . . . . ?
C1 C2 C3 C4 -177.7(10) . . . . ?
C2 C3 C4 C6 2.1(17) . . . . ?
C2 C3 C4 C5 179.2(10) . . . . ?
C3 C4 C5 O4 -176.4(11) . . . . ?
C6 C4 C5 O4 0.6(17) . . . . ?
C3 C4 C5 O3 0.0(16) . . . . ?
C6 C4 C5 O3 177.0(11) . . . . ?
C3 C4 C6 C7 0.9(18) . . . . ?
C5 C4 C6 C7 -176.2(11) . . . . ?
C4 C6 C7 C8 -3(2) . . . . ?
C3 C2 C8 C7 1.0(18) . . . . ?
C1 C2 C8 C7 175.3(12) . . . . ?
C3 C2 C8 C9 -177.3(11) . . . . ?
C1 C2 C8 C9 -2.9(19) . . . . ?
C6 C7 C8 C2 2(2) . . . . ?
C6 C7 C8 C9 -179.7(11) . . . . ?
C2 C8 C9 C15 -56.3(18) . . . . ?
C7 C8 C9 C15 125.5(14) . . . . ?
C2 C8 C9 C10 122.5(13) . . . . ?
C7 C8 C9 C10 -55.7(17) . . . . ?
C15 C9 C10 C11 -2.0(17) . . . . ?
C8 C9 C10 C11 179.0(11) . . . . ?
C9 C10 C11 C12 -0.2(18) . . . . ?
C10 C11 C12 C14 1.3(18) . . . . ?
C10 C11 C12 C13 178.7(10) . . . . ?
C14 C12 C13 O6 163.1(12) . . . . ?
C11 C12 C13 O6 -14.2(17) . . . . ?
C14 C12 C13 O5 -19.0(16) . . . . ?
C11 C12 C13 O5 163.7(11) . . . . ?
C11 C12 C14 C15 -0.1(18) . . . . ?
C13 C12 C14 C15 -177.3(10) . . . . ?
C10 C9 C15 C14 3.3(16) . . . . ?
C8 C9 C15 C14 -177.9(11) . . . . ?
C12 C14 C15 C9 -2.4(18) . . . . ?
C20 N1 C16 C17 -5.0(16) . . . . ?
Ni1 N1 C16 C17 175.2(8) . . . . ?
N1 C16 C17 C18 5.0(19) . . . . ?
C16 C17 C18 C19 -5(2) . . . . ?
C17 C18 C19 C20 4(2) . . . . ?
C17 C18 C19 C21 -179.6(14) . . . . ?
C18 C19 C20 N1 -4.5(18) . . . . ?
C21 C19 C20 N1 179.1(11) . . . . ?
C18 C19 C20 C24 176.5(12) . . . . ?
C21 C19 C20 C24 0.1(18) . . . . ?
C16 N1 C20 C19 4.9(16) . . . . ?
Ni1 N1 C20 C19 -175.2(9) . . . . ?
C16 N1 C20 C24 -176.0(10) . . . . ?
Ni1 N1 C20 C24 3.9(12) . . . . ?
C20 C19 C21 C22 -1(2) . . . . ?
C18 C19 C21 C22 -176.9(14) . . . . ?
C19 C21 C22 C23 2(2) . . . . ?
C21 C22 C23 C24 -3(2) . . . . ?
C21 C22 C23 C25 -179.2(14) . . . . ?
C27 N2 C24 C23 -0.9(16) . . . . ?
Ni1 N2 C24 C23 176.2(9) . . . . ?
C27 N2 C24 C20 178.3(10) . . . . ?
Ni1 N2 C24 C20 -4.6(12) . . . . ?
C25 C23 C24 N2 -1.9(17) . . . . ?
C22 C23 C24 N2 -178.0(10) . . . . ?
C25 C23 C24 C20 178.9(11) . . . . ?
C22 C23 C24 C20 2.7(17) . . . . ?
C19 C20 C24 N2 179.5(10) . . . . ?
N1 C20 C24 N2 0.5(15) . . . . ?
C19 C20 C24 C23 -1.2(17) . . . . ?
N1 C20 C24 C23 179.8(10) . . . . ?
C24 C23 C25 C26 4.1(18) . . . . ?
C22 C23 C25 C26 180.0(12) . . . . ?
C23 C25 C26 C27 -3.5(19) . . . . ?
C24 N2 C27 C26 1.7(18) . . . . ?
Ni1 N2 C27 C26 -174.9(10) . . . . ?
C25 C26 C27 N2 1(2) . . . . ?
C32 N3 C28 C29 -4(2) . . . . ?
Ni1 N3 C28 C29 -174.2(11) . . . . ?
N3 C28 C29 C30 1(2) . . . . ?
C28 C29 C30 C31 -1(2) . . . . ?
C29 C30 C31 C32 4(2) . . . . ?
C29 C30 C31 C33 178.0(16) . . . . ?
C28 N3 C32 C31 8(2) . . . . ?
Ni1 N3 C32 C31 179.0(11) . . . . ?
C28 N3 C32 C36 -176.7(12) . . . . ?
Ni1 N3 C32 C36 -5.3(14) . . . . ?
C30 C31 C32 N3 -7(2) . . . . ?
C33 C31 C32 N3 178.3(13) . . . . ?
C30 C31 C32 C36 177.0(14) . . . . ?
C33 C31 C32 C36 3(2) . . . . ?
C32 C31 C33 C34 -2(2) . . . . ?
C30 C31 C33 C34 -175.9(16) . . . . ?
C31 C33 C34 C35 -1(3) . . . . ?
C33 C34 C35 C37 -179.6(16) . . . . ?
C33 C34 C35 C36 3(2) . . . . ?
C39 N4 C36 C35 -0.1(18) . . . . ?
Ni1 N4 C36 C35 -179.6(10) . . . . ?
C39 N4 C36 C32 -179.4(12) . . . . ?
Ni1 N4 C36 C32 1.1(14) . . . . ?
C37 C35 C36 N4 1.0(19) . . . . ?
C34 C35 C36 N4 178.6(11) . . . . ?
C37 C35 C36 C32 -179.8(13) . . . . ?
C34 C35 C36 C32 -2.1(18) . . . . ?
N3 C32 C36 N4 2.8(17) . . . . ?
C31 C32 C36 N4 178.7(12) . . . . ?
N3 C32 C36 C35 -176.5(11) . . . . ?
C31 C32 C36 C35 -1(2) . . . . ?
C36 C35 C37 C38 1(2) . . . . ?
C34 C35 C37 C38 -176.1(14) . . . . ?
C35 C37 C38 C39 -4(2) . . . . ?
C36 N4 C39 C38 -3.0(19) . . . . ?
Ni1 N4 C39 C38 176.4(9) . . . . ?
C37 C38 C39 N4 5(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O3 0.82 1.68 2.488(10) 168.1 1_565
O7 H1W O2 0.82 1.92 2.670(10) 152.2 .
O7 H2W O4 0.85 1.82 2.674(9) 179.7 3
O8 H3W O4 0.85 2.05 2.895(13) 179.1 3
O8 H4W O2 0.85 2.33 3.184(13) 179.0 .
O9 H5W O2 0.85 1.97 2.820(16) 179.4 .
O9 H6W O6 0.85 2.11 2.959(15) 179.3 4_465

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.100
####################################################################### 
# 
# 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_239-1cd9
_database_code_depnum_ccdc_archive 'CCDC 1430229'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H23 Cd2 Cl N4 O6'
_chemical_formula_weight         903.86

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pca21

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

_cell_length_a                   20.3729(6)
_cell_length_b                   9.7388(3)
_cell_length_c                   17.7787(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3527.44(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7062
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14089
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0788
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         25.05
_reflns_number_total             5698
_reflns_number_gt                4632
_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)+(0.0705P)²+0.5992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_number_reflns         5698
_refine_ls_number_parameters     469
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1411
_refine_ls_wR_factor_gt          0.1234
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.043
_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
Cd1 Cd 0.36141(3) 0.28555(6) 0.16831(5) 0.03030(19) Uani 1 1 d . . .
Cd2 Cd 0.32601(3) -0.00541(7) 0.28886(6) 0.02815(18) Uani 1 1 d . . .
Cl1 Cl 0.39712(12) 0.2074(2) 0.30375(16) 0.0387(7) Uani 1 1 d . . .
N1 N 0.2526(4) 0.2233(9) 0.1295(5) 0.038(2) Uani 1 1 d . . .
N2 N 0.2821(4) 0.4221(9) 0.2343(5) 0.041(2) Uani 1 1 d . . .
N3 N 0.2302(4) -0.0963(9) 0.2338(5) 0.037(2) Uani 1 1 d . . .
N4 N 0.2352(4) 0.1038(9) 0.3416(5) 0.034(2) Uani 1 1 d . . .
O1 O 0.4333(3) 0.4776(6) 0.1716(5) 0.0380(17) Uani 1 1 d . . .
O2 O 0.3720(4) 0.4484(8) 0.0715(5) 0.049(2) Uani 1 1 d . . .
O3 O 0.4260(4) 1.1373(7) 0.1010(5) 0.055(2) Uani 1 1 d . . .
O4 O 0.3563(4) 1.0056(6) 0.1647(5) 0.0431(18) Uani 1 1 d . . .
O5 O 0.6115(4) 0.1978(7) -0.2017(4) 0.0407(18) Uani 1 1 d . . .
O6 O 0.6420(4) 0.1185(9) -0.0924(5) 0.064(3) Uani 1 1 d . . .
C1 C 0.4140(5) 0.5162(9) 0.1074(6) 0.026(2) Uani 1 1 d . . .
C2 C 0.4367(4) 0.6477(9) 0.0739(5) 0.026(2) Uani 1 1 d . . .
C3 C 0.4152(5) 0.7682(9) 0.1094(6) 0.028(2) Uani 1 1 d . . .
H3 H 0.3921 0.7613 0.1544 0.033 Uiso 1 1 calc R . .
C4 C 0.4273(4) 0.8968(10) 0.0796(6) 0.029(2) Uani 1 1 d . . .
C5 C 0.4035(5) 1.0238(10) 0.1175(6) 0.029(2) Uani 1 1 d . . .
C6 C 0.4653(5) 0.9072(9) 0.0138(5) 0.031(2) Uani 1 1 d . . .
H6 H 0.4747 0.9931 -0.0064 0.037 Uiso 1 1 calc R . .
C7 C 0.4891(4) 0.7876(9) -0.0219(6) 0.028(2) Uani 1 1 d . . .
H7 H 0.5139 0.7948 -0.0656 0.034 Uiso 1 1 calc R . .
C8 C 0.4756(5) 0.6597(10) 0.0083(6) 0.031(2) Uani 1 1 d . . .
C9 C 0.5065(5) 0.5347(9) -0.0287(6) 0.028(2) Uani 1 1 d . . .
C10 C 0.5115(5) 0.5236(9) -0.1049(6) 0.030(2) Uani 1 1 d . . .
H10 H 0.4930 0.5918 -0.1347 0.036 Uiso 1 1 calc R . .
C11 C 0.5422(5) 0.4173(10) -0.1387(6) 0.030(2) Uani 1 1 d . . .
H11 H 0.5438 0.4127 -0.1910 0.036 Uiso 1 1 calc R . .
C12 C 0.5716(4) 0.3143(10) -0.0958(6) 0.032(2) Uani 1 1 d . . .
C13 C 0.6102(5) 0.2029(10) -0.1322(6) 0.032(2) Uani 1 1 d . . .
C14 C 0.5654(5) 0.3183(11) -0.0200(6) 0.039(3) Uani 1 1 d . . .
H14 H 0.5821 0.2473 0.0093 0.047 Uiso 1 1 calc R . .
C15 C 0.5337(5) 0.4306(11) 0.0141(6) 0.039(3) Uani 1 1 d . . .
H15 H 0.5309 0.4348 0.0662 0.047 Uiso 1 1 calc R . .
C16 C 0.2383(6) 0.1325(12) 0.0806(8) 0.055(3) Uani 1 1 d . . .
H16 H 0.2723 0.0871 0.0562 0.066 Uiso 1 1 calc R . .
C17 C 0.1704(8) 0.0964(15) 0.0610(8) 0.071(5) Uani 1 1 d . . .
H17 H 0.1614 0.0287 0.0256 0.085 Uiso 1 1 calc R . .
C18 C 0.1215(7) 0.1647(16) 0.0962(9) 0.065(4) Uani 1 1 d . . .
H18 H 0.0780 0.1442 0.0849 0.078 Uiso 1 1 calc R . .
C19 C 0.1358(5) 0.2646(15) 0.1487(7) 0.053(4) Uani 1 1 d . . .
C20 C 0.2040(4) 0.2920(10) 0.1640(8) 0.036(2) Uani 1 1 d . . .
C21 C 0.0858(6) 0.3405(17) 0.1874(9) 0.075(5) Uani 1 1 d . . .
H21 H 0.0420 0.3222 0.1766 0.090 Uiso 1 1 calc R . .
C22 C 0.1000(6) 0.4362(18) 0.2381(10) 0.077(5) Uani 1 1 d . . .
H22 H 0.0664 0.4849 0.2613 0.093 Uiso 1 1 calc R . .
C23 C 0.1685(5) 0.4655(15) 0.2577(8) 0.052(4) Uani 1 1 d . . .
C24 C 0.2191(5) 0.3973(11) 0.2190(6) 0.039(3) Uani 1 1 d . . .
C25 C 0.1874(8) 0.5592(15) 0.3120(8) 0.066(4) Uani 1 1 d . . .
H25 H 0.1561 0.6070 0.3397 0.079 Uiso 1 1 calc R . .
C26 C 0.2513(6) 0.5797(12) 0.3241(8) 0.055(3) Uani 1 1 d . . .
H26 H 0.2645 0.6452 0.3590 0.066 Uiso 1 1 calc R . .
C27 C 0.2967(5) 0.5077(11) 0.2869(10) 0.051(3) Uani 1 1 d . . .
H27 H 0.3406 0.5199 0.2994 0.061 Uiso 1 1 calc R . .
C28 C 0.2280(6) -0.1893(11) 0.1800(7) 0.046(3) Uani 1 1 d . . .
H28 H 0.2670 -0.2240 0.1604 0.055 Uiso 1 1 calc R . .
C29 C 0.1669(6) -0.2373(15) 0.1517(9) 0.068(3) Uani 1 1 d U . .
H29 H 0.1666 -0.3003 0.1124 0.082 Uiso 1 1 calc R . .
C30 C 0.1104(7) -0.1942(13) 0.1803(9) 0.067(3) Uani 1 1 d U . .
H30 H 0.0709 -0.2297 0.1626 0.081 Uiso 1 1 calc R . .
C31 C 0.1107(6) -0.0977(15) 0.2355(8) 0.059(4) Uani 1 1 d . . .
C32 C 0.1719(5) -0.0461(13) 0.2624(7) 0.044(3) Uani 1 1 d . . .
C33 C 0.0531(7) -0.0392(19) 0.2702(13) 0.095(7) Uani 1 1 d . . .
H33 H 0.0120 -0.0695 0.2546 0.114 Uiso 1 1 calc R . .
C34 C 0.0563(7) 0.055(2) 0.3230(11) 0.079(5) Uani 1 1 d U . .
H34 H 0.0175 0.0879 0.3437 0.094 Uiso 1 1 calc R . .
C35 C 0.1171(6) 0.1085(14) 0.3496(8) 0.053(3) Uani 1 1 d . . .
C36 C 0.1756(5) 0.0576(13) 0.3200(7) 0.037(3) Uani 1 1 d . . .
C37 C 0.1219(8) 0.2096(17) 0.4032(10) 0.077(5) Uani 1 1 d . . .
H37 H 0.0839 0.2443 0.4252 0.092 Uiso 1 1 calc R . .
C38 C 0.1817(8) 0.2599(14) 0.4250(7) 0.061(4) Uani 1 1 d . . .
H38 H 0.1841 0.3301 0.4603 0.073 Uiso 1 1 calc R . .
C39 C 0.2392(6) 0.2053(12) 0.3938(7) 0.051(3) Uani 1 1 d . . .
H39 H 0.2800 0.2383 0.4089 0.061 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O3 2.291(7) 1_545 ?
Cd1 O2 2.350(8) . ?
Cd1 O1 2.377(6) . ?
Cd1 N1 2.399(9) . ?
Cd1 N2 2.399(9) . ?
Cd1 Cl1 2.628(3) . ?
Cd2 O5 2.271(6) 2_655 ?
Cd2 O4 2.294(8) 1_545 ?
Cd2 N4 2.331(8) . ?
Cd2 N3 2.357(9) . ?
Cd2 O6 2.468(9) 2_655 ?
Cd2 Cl1 2.543(2) . ?
Cd2 C13 2.713(10) 2_655 ?
N1 C16 1.274(15) . ?
N1 C20 1.343(15) . ?
N2 C27 1.287(16) . ?
N2 C24 1.335(12) . ?
N3 C28 1.317(14) . ?
N3 C32 1.381(14) . ?
N4 C36 1.351(13) . ?
N4 C39 1.359(14) . ?
O1 C1 1.265(13) . ?
O2 C1 1.256(12) . ?
O3 C5 1.233(12) . ?
O3 Cd1 2.291(7) 1_565 ?
O4 C5 1.288(13) . ?
O4 Cd2 2.294(8) 1_565 ?
O5 C13 1.237(13) . ?
O5 Cd2 2.271(6) 2_654 ?
O6 C13 1.263(13) . ?
O6 Cd2 2.468(9) 2_654 ?
C1 C2 1.486(13) . ?
C2 C3 1.403(13) . ?
C2 C8 1.415(13) . ?
C3 C4 1.382(13) . ?
C3 H3 0.9300 . ?
C4 C6 1.407(13) . ?
C4 C5 1.490(13) . ?
C6 C7 1.412(13) . ?
C6 H6 0.9300 . ?
C7 C8 1.383(13) . ?
C7 H7 0.9300 . ?
C8 C9 1.521(13) . ?
C9 C10 1.362(14) . ?
C9 C15 1.383(14) . ?
C10 C11 1.352(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.396(14) . ?
C11 H11 0.9300 . ?
C12 C14 1.353(15) . ?
C12 C13 1.487(13) . ?
C13 Cd2 2.713(10) 2_654 ?
C14 C15 1.407(14) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.468(17) . ?
C16 H16 0.9300 . ?
C17 C18 1.35(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.38(2) . ?
C18 H18 0.9300 . ?
C19 C21 1.435(19) . ?
C19 C20 1.441(13) . ?
C20 C24 1.449(17) . ?
C21 C22 1.33(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.466(19) . ?
C22 H22 0.9300 . ?
C23 C25 1.384(19) . ?
C23 C24 1.406(15) . ?
C25 C26 1.334(19) . ?
C25 H25 0.9300 . ?
C26 C27 1.336(16) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.422(17) . ?
C28 H28 0.9300 . ?
C29 C30 1.33(2) . ?
C29 H29 0.9300 . ?
C30 C31 1.359(19) . ?
C30 H30 0.9300 . ?
C31 C32 1.428(16) . ?
C31 C33 1.44(2) . ?
C32 C36 1.439(16) . ?
C33 C34 1.31(2) . ?
C33 H33 0.9300 . ?
C34 C35 1.42(2) . ?
C34 H34 0.9300 . ?
C35 C37 1.37(2) . ?
C35 C36 1.394(16) . ?
C37 C38 1.37(2) . ?
C37 H37 0.9300 . ?
C38 C39 1.401(17) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cd1 O2 89.4(3) 1_545 . ?
O3 Cd1 O1 98.9(3) 1_545 . ?
O2 Cd1 O1 55.3(3) . . ?
O3 Cd1 N1 102.8(3) 1_545 . ?
O2 Cd1 N1 92.6(3) . . ?
O1 Cd1 N1 140.9(3) . . ?
O3 Cd1 N2 172.6(3) 1_545 . ?
O2 Cd1 N2 92.6(3) . . ?
O1 Cd1 N2 88.1(3) . . ?
N1 Cd1 N2 70.0(3) . . ?
O3 Cd1 Cl1 97.9(2) 1_545 . ?
O2 Cd1 Cl1 147.2(2) . . ?
O1 Cd1 Cl1 92.0(2) . . ?
N1 Cd1 Cl1 116.5(2) . . ?
N2 Cd1 Cl1 84.2(2) . . ?
O5 Cd2 O4 87.6(2) 2_655 1_545 ?
O5 Cd2 N4 142.4(3) 2_655 . ?
O4 Cd2 N4 125.4(3) 1_545 . ?
O5 Cd2 N3 100.7(3) 2_655 . ?
O4 Cd2 N3 80.8(3) 1_545 . ?
N4 Cd2 N3 71.4(3) . . ?
O5 Cd2 O6 54.6(3) 2_655 2_655 ?
O4 Cd2 O6 140.5(2) 1_545 2_655 ?
N4 Cd2 O6 94.0(3) . 2_655 ?
N3 Cd2 O6 114.0(3) . 2_655 ?
O5 Cd2 Cl1 110.2(2) 2_655 . ?
O4 Cd2 Cl1 84.75(19) 1_545 . ?
N4 Cd2 Cl1 92.2(2) . . ?
N3 Cd2 Cl1 145.2(2) . . ?
O6 Cd2 Cl1 97.1(2) 2_655 . ?
O5 Cd2 C13 26.9(3) 2_655 2_655 ?
O4 Cd2 C13 113.7(3) 1_545 2_655 ?
N4 Cd2 C13 119.7(3) . 2_655 ?
N3 Cd2 C13 110.2(3) . 2_655 ?
O6 Cd2 C13 27.7(3) 2_655 2_655 ?
Cl1 Cd2 C13 104.5(2) . 2_655 ?
Cd2 Cl1 Cd1 89.02(8) . . ?
C16 N1 C20 119.2(10) . . ?
C16 N1 Cd1 125.7(8) . . ?
C20 N1 Cd1 115.1(7) . . ?
C27 N2 C24 119.2(10) . . ?
C27 N2 Cd1 124.0(7) . . ?
C24 N2 Cd1 116.6(7) . . ?
C28 N3 C32 118.9(10) . . ?
C28 N3 Cd2 125.9(7) . . ?
C32 N3 Cd2 115.2(8) . . ?
C36 N4 C39 119.4(10) . . ?
C36 N4 Cd2 116.6(7) . . ?
C39 N4 Cd2 123.9(7) . . ?
C1 O1 Cd1 91.1(6) . . ?
C1 O2 Cd1 92.6(6) . . ?
C5 O3 Cd1 103.1(6) . 1_565 ?
C5 O4 Cd2 146.6(7) . 1_565 ?
C13 O5 Cd2 96.8(6) . 2_654 ?
C13 O6 Cd2 87.0(7) . 2_654 ?
O2 C1 O1 121.0(9) . . ?
O2 C1 C2 117.4(9) . . ?
O1 C1 C2 121.5(8) . . ?
C3 C2 C8 118.5(9) . . ?
C3 C2 C1 116.3(8) . . ?
C8 C2 C1 125.2(9) . . ?
C4 C3 C2 122.0(9) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C6 118.9(9) . . ?
C3 C4 C5 121.4(9) . . ?
C6 C4 C5 119.7(9) . . ?
O3 C5 O4 123.8(9) . . ?
O3 C5 C4 121.0(9) . . ?
O4 C5 C4 115.1(9) . . ?
C4 C6 C7 120.2(9) . . ?
C4 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 120.1(9) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C2 120.3(9) . . ?
C7 C8 C9 118.1(9) . . ?
C2 C8 C9 121.5(9) . . ?
C10 C9 C15 117.3(9) . . ?
C10 C9 C8 121.6(8) . . ?
C15 C9 C8 121.0(9) . . ?
C11 C10 C9 122.6(9) . . ?
C11 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
C10 C11 C12 120.4(10) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C14 C12 C11 118.9(9) . . ?
C14 C12 C13 120.2(9) . . ?
C11 C12 C13 120.8(10) . . ?
O5 C13 O6 121.4(9) . . ?
O5 C13 C12 118.4(9) . . ?
O6 C13 C12 120.1(10) . . ?
O5 C13 Cd2 56.2(5) . 2_654 ?
O6 C13 Cd2 65.3(6) . 2_654 ?
C12 C13 Cd2 174.4(8) . 2_654 ?
C12 C14 C15 119.6(10) . . ?
C12 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C9 C15 C14 121.1(10) . . ?
C9 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
N1 C16 C17 123.0(13) . . ?
N1 C16 H16 118.5 . . ?
C17 C16 H16 118.5 . . ?
C18 C17 C16 117.8(13) . . ?
C18 C17 H17 121.1 . . ?
C16 C17 H17 121.1 . . ?
C17 C18 C19 120.3(12) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C21 122.5(12) . . ?
C18 C19 C20 117.5(12) . . ?
C21 C19 C20 119.9(13) . . ?
N1 C20 C19 122.2(12) . . ?
N1 C20 C24 120.3(8) . . ?
C19 C20 C24 117.5(11) . . ?
C22 C21 C19 122.1(13) . . ?
C22 C21 H21 118.9 . . ?
C19 C21 H21 118.9 . . ?
C21 C22 C23 120.4(14) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C25 C23 C24 116.7(12) . . ?
C25 C23 C22 124.0(13) . . ?
C24 C23 C22 119.3(15) . . ?
N2 C24 C23 121.3(12) . . ?
N2 C24 C20 118.0(9) . . ?
C23 C24 C20 120.7(10) . . ?
C26 C25 C23 118.9(12) . . ?
C26 C25 H25 120.6 . . ?
C23 C25 H25 120.6 . . ?
C25 C26 C27 121.1(13) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
N2 C27 C26 122.7(12) . . ?
N2 C27 H27 118.7 . . ?
C26 C27 H27 118.7 . . ?
N3 C28 C29 120.8(11) . . ?
N3 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
C30 C29 C28 121.3(13) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C29 C30 C31 119.5(12) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
C30 C31 C32 119.3(13) . . ?
C30 C31 C33 125.4(14) . . ?
C32 C31 C33 115.4(14) . . ?
N3 C32 C31 120.2(13) . . ?
N3 C32 C36 117.8(10) . . ?
C31 C32 C36 122.0(11) . . ?
C34 C33 C31 122.7(15) . . ?
C34 C33 H33 118.7 . . ?
C31 C33 H33 118.7 . . ?
C33 C34 C35 122.4(15) . . ?
C33 C34 H34 118.8 . . ?
C35 C34 H34 118.8 . . ?
C37 C35 C36 117.1(13) . . ?
C37 C35 C34 123.7(14) . . ?
C36 C35 C34 119.2(15) . . ?
N4 C36 C35 122.9(13) . . ?
N4 C36 C32 118.8(9) . . ?
C35 C36 C32 118.3(11) . . ?
C38 C37 C35 121.0(13) . . ?
C38 C37 H37 119.5 . . ?
C35 C37 H37 119.5 . . ?
C37 C38 C39 119.8(14) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
N4 C39 C38 119.7(13) . . ?
N4 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?

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
O5 Cd2 Cl1 Cd1 119.9(2) 2_655 . . . ?
O4 Cd2 Cl1 Cd1 34.36(18) 1_545 . . . ?
N4 Cd2 Cl1 Cd1 -91.0(2) . . . . ?
N3 Cd2 Cl1 Cd1 -31.3(4) . . . . ?
O6 Cd2 Cl1 Cd1 174.72(18) 2_655 . . . ?
C13 Cd2 Cl1 Cd1 147.5(2) 2_655 . . . ?
O3 Cd1 Cl1 Cd2 -76.1(2) 1_545 . . . ?
O2 Cd1 Cl1 Cd2 -177.4(4) . . . . ?
O1 Cd1 Cl1 Cd2 -175.34(18) . . . . ?
N1 Cd1 Cl1 Cd2 32.5(3) . . . . ?
N2 Cd1 Cl1 Cd2 96.8(2) . . . . ?
O3 Cd1 N1 C16 -2.6(10) 1_545 . . . ?
O2 Cd1 N1 C16 87.4(10) . . . . ?
O1 Cd1 N1 C16 119.4(9) . . . . ?
N2 Cd1 N1 C16 179.3(10) . . . . ?
Cl1 Cd1 N1 C16 -108.3(9) . . . . ?
O3 Cd1 N1 C20 177.0(8) 1_545 . . . ?
O2 Cd1 N1 C20 -93.0(8) . . . . ?
O1 Cd1 N1 C20 -61.0(10) . . . . ?
N2 Cd1 N1 C20 -1.1(8) . . . . ?
Cl1 Cd1 N1 C20 71.4(8) . . . . ?
O3 Cd1 N2 C27 161(2) 1_545 . . . ?
O2 Cd1 N2 C27 -93.3(11) . . . . ?
O1 Cd1 N2 C27 -38.1(11) . . . . ?
N1 Cd1 N2 C27 175.0(11) . . . . ?
Cl1 Cd1 N2 C27 54.0(10) . . . . ?
O3 Cd1 N2 C24 -14(3) 1_545 . . . ?
O2 Cd1 N2 C24 92.6(8) . . . . ?
O1 Cd1 N2 C24 147.7(8) . . . . ?
N1 Cd1 N2 C24 0.8(7) . . . . ?
Cl1 Cd1 N2 C24 -120.1(8) . . . . ?
O5 Cd2 N3 C28 -40.6(9) 2_655 . . . ?
O4 Cd2 N3 C28 45.2(9) 1_545 . . . ?
N4 Cd2 N3 C28 177.5(10) . . . . ?
O6 Cd2 N3 C28 -96.5(9) 2_655 . . . ?
Cl1 Cd2 N3 C28 112.0(9) . . . . ?
C13 Cd2 N3 C28 -66.8(10) 2_655 . . . ?
O5 Cd2 N3 C32 138.7(7) 2_655 . . . ?
O4 Cd2 N3 C32 -135.5(8) 1_545 . . . ?
N4 Cd2 N3 C32 -3.2(8) . . . . ?
O6 Cd2 N3 C32 82.8(8) 2_655 . . . ?
Cl1 Cd2 N3 C32 -68.8(9) . . . . ?
C13 Cd2 N3 C32 112.5(8) 2_655 . . . ?
O5 Cd2 N4 C36 -79.0(9) 2_655 . . . ?
O4 Cd2 N4 C36 67.9(8) 1_545 . . . ?
N3 Cd2 N4 C36 4.3(8) . . . . ?
O6 Cd2 N4 C36 -109.7(8) 2_655 . . . ?
Cl1 Cd2 N4 C36 153.0(7) . . . . ?
C13 Cd2 N4 C36 -98.9(8) 2_655 . . . ?
O5 Cd2 N4 C39 98.3(9) 2_655 . . . ?
O4 Cd2 N4 C39 -114.8(8) 1_545 . . . ?
N3 Cd2 N4 C39 -178.4(9) . . . . ?
O6 Cd2 N4 C39 67.6(9) 2_655 . . . ?
Cl1 Cd2 N4 C39 -29.7(8) . . . . ?
C13 Cd2 N4 C39 78.4(9) 2_655 . . . ?
O3 Cd1 O1 C1 83.7(6) 1_545 . . . ?
O2 Cd1 O1 C1 0.6(5) . . . . ?
N1 Cd1 O1 C1 -39.5(8) . . . . ?
N2 Cd1 O1 C1 -93.9(6) . . . . ?
Cl1 Cd1 O1 C1 -178.0(5) . . . . ?
O3 Cd1 O2 C1 -101.9(6) 1_545 . . . ?
O1 Cd1 O2 C1 -0.6(5) . . . . ?
N1 Cd1 O2 C1 155.4(6) . . . . ?
N2 Cd1 O2 C1 85.2(6) . . . . ?
Cl1 Cd1 O2 C1 1.9(8) . . . . ?
Cd1 O2 C1 O1 1.1(9) . . . . ?
Cd1 O2 C1 C2 -174.9(7) . . . . ?
Cd1 O1 C1 O2 -1.1(9) . . . . ?
Cd1 O1 C1 C2 174.8(8) . . . . ?
O2 C1 C2 C3 108.4(10) . . . . ?
O1 C1 C2 C3 -67.6(12) . . . . ?
O2 C1 C2 C8 -69.0(13) . . . . ?
O1 C1 C2 C8 114.9(11) . . . . ?
C8 C2 C3 C4 4.2(15) . . . . ?
C1 C2 C3 C4 -173.4(9) . . . . ?
C2 C3 C4 C6 -3.3(15) . . . . ?
C2 C3 C4 C5 179.3(9) . . . . ?
Cd1 O3 C5 O4 -2.5(12) 1_565 . . . ?
Cd1 O3 C5 C4 173.8(8) 1_565 . . . ?
Cd2 O4 C5 O3 -78.3(15) 1_565 . . . ?
Cd2 O4 C5 C4 105.1(11) 1_565 . . . ?
C3 C4 C5 O3 163.7(10) . . . . ?
C6 C4 C5 O3 -13.7(15) . . . . ?
C3 C4 C5 O4 -19.6(14) . . . . ?
C6 C4 C5 O4 163.0(9) . . . . ?
C3 C4 C6 C7 1.4(14) . . . . ?
C5 C4 C6 C7 178.9(9) . . . . ?
C4 C6 C7 C8 -0.5(15) . . . . ?
C6 C7 C8 C2 1.4(14) . . . . ?
C6 C7 C8 C9 -175.5(9) . . . . ?
C3 C2 C8 C7 -3.2(14) . . . . ?
C1 C2 C8 C7 174.2(9) . . . . ?
C3 C2 C8 C9 173.6(9) . . . . ?
C1 C2 C8 C9 -8.9(15) . . . . ?
C7 C8 C9 C10 -40.0(14) . . . . ?
C2 C8 C9 C10 143.1(10) . . . . ?
C7 C8 C9 C15 136.8(10) . . . . ?
C2 C8 C9 C15 -40.1(14) . . . . ?
C15 C9 C10 C11 -0.9(15) . . . . ?
C8 C9 C10 C11 176.0(9) . . . . ?
C9 C10 C11 C12 -1.2(16) . . . . ?
C10 C11 C12 C14 3.9(15) . . . . ?
C10 C11 C12 C13 -175.0(9) . . . . ?
Cd2 O5 C13 O6 3.7(11) 2_654 . . . ?
Cd2 O5 C13 C12 -178.1(8) 2_654 . . . ?
Cd2 O6 C13 O5 -3.4(10) 2_654 . . . ?
Cd2 O6 C13 C12 178.4(9) 2_654 . . . ?
C14 C12 C13 O5 175.7(10) . . . . ?
C11 C12 C13 O5 -5.4(15) . . . . ?
C14 C12 C13 O6 -6.1(16) . . . . ?
C11 C12 C13 O6 172.8(10) . . . . ?
C14 C12 C13 Cd2 159(7) . . . 2_654 ?
C11 C12 C13 Cd2 -22(8) . . . 2_654 ?
C11 C12 C14 C15 -4.4(16) . . . . ?
C13 C12 C14 C15 174.5(9) . . . . ?
C10 C9 C15 C14 0.3(15) . . . . ?
C8 C9 C15 C14 -176.6(9) . . . . ?
C12 C14 C15 C9 2.4(16) . . . . ?
C20 N1 C16 C17 -1.5(18) . . . . ?
Cd1 N1 C16 C17 178.1(8) . . . . ?
N1 C16 C17 C18 1(2) . . . . ?
C16 C17 C18 C19 0(2) . . . . ?
C17 C18 C19 C21 179.7(13) . . . . ?
C17 C18 C19 C20 0(2) . . . . ?
C16 N1 C20 C19 1.3(17) . . . . ?
Cd1 N1 C20 C19 -178.4(8) . . . . ?
C16 N1 C20 C24 -179.0(10) . . . . ?
Cd1 N1 C20 C24 1.4(13) . . . . ?
C18 C19 C20 N1 -0.5(18) . . . . ?
C21 C19 C20 N1 179.7(11) . . . . ?
C18 C19 C20 C24 179.8(11) . . . . ?
C21 C19 C20 C24 0.0(17) . . . . ?
C18 C19 C21 C22 179.7(15) . . . . ?
C20 C19 C21 C22 0(2) . . . . ?
C19 C21 C22 C23 -1(2) . . . . ?
C21 C22 C23 C25 -177.2(14) . . . . ?
C21 C22 C23 C24 4(2) . . . . ?
C27 N2 C24 C23 1.7(17) . . . . ?
Cd1 N2 C24 C23 176.2(8) . . . . ?
C27 N2 C24 C20 -174.9(11) . . . . ?
Cd1 N2 C24 C20 -0.4(13) . . . . ?
C25 C23 C24 N2 0.1(16) . . . . ?
C22 C23 C24 N2 179.1(11) . . . . ?
C25 C23 C24 C20 176.6(10) . . . . ?
C22 C23 C24 C20 -4.3(17) . . . . ?
N1 C20 C24 N2 -0.7(16) . . . . ?
C19 C20 C24 N2 179.1(10) . . . . ?
N1 C20 C24 C23 -177.3(11) . . . . ?
C19 C20 C24 C23 2.5(16) . . . . ?
C24 C23 C25 C26 0.4(18) . . . . ?
C22 C23 C25 C26 -178.6(13) . . . . ?
C23 C25 C26 C27 -3(2) . . . . ?
C24 N2 C27 C26 -4(2) . . . . ?
Cd1 N2 C27 C26 -178.2(10) . . . . ?
C25 C26 C27 N2 5(2) . . . . ?
C32 N3 C28 C29 0.1(17) . . . . ?
Cd2 N3 C28 C29 179.4(9) . . . . ?
N3 C28 C29 C30 -3(2) . . . . ?
C28 C29 C30 C31 3(2) . . . . ?
C29 C30 C31 C32 -1(2) . . . . ?
C29 C30 C31 C33 178.3(15) . . . . ?
C28 N3 C32 C31 1.9(17) . . . . ?
Cd2 N3 C32 C31 -177.5(9) . . . . ?
C28 N3 C32 C36 -178.7(10) . . . . ?
Cd2 N3 C32 C36 2.0(12) . . . . ?
C30 C31 C32 N3 -1.6(19) . . . . ?
C33 C31 C32 N3 179.2(12) . . . . ?
C30 C31 C32 C36 179.0(12) . . . . ?
C33 C31 C32 C36 -0.3(18) . . . . ?
C30 C31 C33 C34 -179.3(16) . . . . ?
C32 C31 C33 C34 0(2) . . . . ?
C31 C33 C34 C35 1(3) . . . . ?
C33 C34 C35 C37 178.2(16) . . . . ?
C33 C34 C35 C36 -1(2) . . . . ?
C39 N4 C36 C35 -0.7(16) . . . . ?
Cd2 N4 C36 C35 176.8(8) . . . . ?
C39 N4 C36 C32 177.6(9) . . . . ?
Cd2 N4 C36 C32 -5.0(12) . . . . ?
C37 C35 C36 N4 -0.3(18) . . . . ?
C34 C35 C36 N4 179.3(12) . . . . ?
C37 C35 C36 C32 -178.6(11) . . . . ?
C34 C35 C36 C32 1.0(17) . . . . ?
N3 C32 C36 N4 2.0(14) . . . . ?
C31 C32 C36 N4 -178.6(12) . . . . ?
N3 C32 C36 C35 -179.7(11) . . . . ?
C31 C32 C36 C35 -0.2(15) . . . . ?
C36 C35 C37 C38 1.6(19) . . . . ?
C34 C35 C37 C38 -178.0(13) . . . . ?
C35 C37 C38 C39 -2(2) . . . . ?
C36 N4 C39 C38 0.4(16) . . . . ?
Cd2 N4 C39 C38 -176.8(8) . . . . ?
C37 C38 C39 N4 0.8(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.613
_refine_diff_density_min         -0.628
_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_239-9ni1
_database_code_depnum_ccdc_archive 'CCDC 1430230'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2015-09-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C196 H168 N16 Ni12 O64)'
_chemical_formula_sum            'C49 H42 N4 Ni3 O16'
_chemical_formula_weight         1118.99
_chemical_melting_point          ?
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'
Ni Ni 0.3393 1.1124 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   20.505(2)
_cell_length_b                   10.3482(9)
_cell_length_c                   29.521(4)
_cell_angle_alpha                90
_cell_angle_beta                 113.518(15)
_cell_angle_gamma                90
_cell_volume                     5743.7(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    896
_cell_measurement_temperature    293.64(10)
_cell_measurement_theta_max      20.8940
_cell_measurement_theta_min      3.9450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_av_unetI/netI     0.2309
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            12802
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.393
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.64(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    8.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000 -180.0000 33

#__ type_ start__ end____ width___ exp.time_
  2 omega  -42.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -77.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
  3 omega   -7.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   77.0000  150.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0252333000
_diffrn_orient_matrix_UB_12      -0.0498091000
_diffrn_orient_matrix_UB_13      0.0031802000
_diffrn_orient_matrix_UB_21      0.0274750000
_diffrn_orient_matrix_UB_22      0.0467619000
_diffrn_orient_matrix_UB_23      0.0062477000
_diffrn_orient_matrix_UB_31      0.0056784000
_diffrn_orient_matrix_UB_32      -0.0053146000
_diffrn_orient_matrix_UB_33      0.0252598000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2601
_reflns_number_total             5648
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.0837
_refine_ls_restrained_S_all      0.934
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0784P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.2257
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
2. Restrained distances
 H7B-O7
 0.86 with sigma of 0.01
 H7A-O7
 0.86 with sigma of 0.01
 H7B-H7A
 1.46 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C23B) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C25A) \\sim Ueq,
Uanis(C21A) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C24B) \\sim Ueq,
Uanis(C21B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C21A(0.5) H21A(0.5) C22A(0.5) H22A(0.5) C24A(0.5) H24A(0.5)
 C25A(0.5) H25A(0.5) C21B(0.5) H21B(0.5) C22B(0.5) H22B(0.5) C23(0.5) H23(0.5)
 H23A(0.5) C23B(0.5) H23B(0.5) C24B(0.5) H24B(0.5)
5.a Riding coordinates:
 O8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C21A(H21A), C22A(H22A), C24A(H24A),
 C25A(H25A), C21B(H21B), C22B(H22B), C23(H23), C23(H23A), C23B(H23B), C24B(H24B)
5.c Fitted hexagon refined as free rotating group:
 C21B(C22B,C23,C23B,C24B,N2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.33655(4) 0.67752(9) 0.16392(3) 0.0259(3) Uani 1 1 d . . . . .
Ni2 Ni 0.5000 0.84253(12) 0.2500 0.0223(3) Uani 1 2 d S T P A .
O1 O 0.2507(2) 0.7949(5) 0.14907(18) 0.0328(12) Uani 1 1 d . . . . .
O2 O 0.3032(3) 0.9848(5) 0.1718(2) 0.0489(16) Uani 1 1 d . . . . .
O3 O 0.1552(2) 1.1627(5) 0.26472(17) 0.0348(13) Uani 1 1 d . . . . .
O4 O 0.0395(2) 1.1986(5) 0.21910(17) 0.0313(12) Uani 1 1 d . . . . .
O5 O 0.0861(3) 0.6678(5) -0.0994(2) 0.0499(16) Uani 1 1 d . . . . .
O6 O 0.1689(3) 0.8126(5) -0.09295(17) 0.0389(14) Uani 1 1 d . . . . .
O7 O 0.4090(2) 0.8373(5) 0.18528(17) 0.0261(11) Uani 1 1 d D . . . .
O8 O 0.4185(2) 0.5425(5) 0.18141(19) 0.0451(15) Uani 1 1 d . . . . .
H8A H 0.4296 0.5837 0.2083 0.054 Uiso 1 1 d R . . . .
H8B H 0.4442 0.5894 0.1928 0.054 Uiso 1 1 d R . . . .
N1 N 0.2650(3) 0.5263(6) 0.1396(2) 0.0356(16) Uani 1 1 d . . . . .
C1 C 0.2495(4) 0.9124(8) 0.1569(2) 0.0258(17) Uani 1 1 d . . . . .
C2 C 0.1780(3) 0.9706(7) 0.1476(3) 0.0268(17) Uani 1 1 d . . . . .
C3 C 0.1712(3) 1.0329(6) 0.1871(2) 0.0253(16) Uani 1 1 d . . . . .
H3 H 0.2105 1.0387 0.2171 0.030 Uiso 1 1 calc R . . . .
C4 C 0.1068(4) 1.0869(7) 0.1829(3) 0.0297(17) Uani 1 1 d . . . . .
C5 C 0.1001(4) 1.1546(7) 0.2258(3) 0.0297(18) Uani 1 1 d . . . . .
C6 C 0.0499(4) 1.0789(8) 0.1365(3) 0.0349(19) Uani 1 1 d . . . . .
H6 H 0.0070 1.1175 0.1324 0.042 Uiso 1 1 calc R . . . .
C7 C 0.0549(4) 1.0176(8) 0.0976(3) 0.0367(19) Uani 1 1 d . . . . .
H7 H 0.0155 1.0126 0.0677 0.044 Uiso 1 1 calc R . . . .
C8 C 0.1199(4) 0.9612(7) 0.1025(2) 0.0282(17) Uani 1 1 d . . . . .
C9 C 0.1248(4) 0.8968(8) 0.0588(3) 0.0336(19) Uani 1 1 d . . . . .
C10 C 0.1813(4) 0.9279(8) 0.0453(3) 0.045(2) Uani 1 1 d . . . . .
H10 H 0.2174 0.9833 0.0646 0.054 Uiso 1 1 calc R . . . .
C11 C 0.1821(4) 0.8753(9) 0.0031(3) 0.047(2) Uani 1 1 d . . . . .
H11 H 0.2205 0.8945 -0.0049 0.057 Uiso 1 1 calc R . . . .
C12 C 0.1300(4) 0.7958(8) -0.0282(2) 0.0310(18) Uani 1 1 d . . . . .
C13 C 0.1289(4) 0.7543(8) -0.0767(3) 0.0340(19) Uani 1 1 d . . . . .
C14 C 0.0774(4) 0.7605(8) -0.0126(3) 0.041(2) Uani 1 1 d . . . . .
H14 H 0.0430 0.7011 -0.0310 0.049 Uiso 1 1 calc R . . . .
C15 C 0.0746(4) 0.8119(8) 0.0299(2) 0.035(2) Uani 1 1 d . . . . .
H15 H 0.0378 0.7880 0.0390 0.043 Uiso 1 1 calc R . . . .
C16 C 0.2766(5) 0.4164(9) 0.1638(4) 0.064(3) Uani 1 1 d . . . . .
H16 H 0.3158 0.4116 0.1939 0.077 Uiso 1 1 calc R . . . .
C17 C 0.2362(7) 0.3117(13) 0.1485(6) 0.112(5) Uani 1 1 d . . . . .
H17 H 0.2468 0.2352 0.1665 0.135 Uiso 1 1 calc R . . . .
C18 C 0.1788(8) 0.3222(13) 0.1052(7) 0.126(6) Uani 1 1 d . . . . .
H18 H 0.1489 0.2511 0.0939 0.151 Uiso 1 1 calc R . . . .
C19 C 0.1622(7) 0.4338(13) 0.0769(5) 0.109(5) Uani 1 1 d . . . . .
H19 H 0.1227 0.4412 0.0472 0.131 Uiso 1 1 calc R . . . .
C20 C 0.2101(4) 0.5327(8) 0.0969(4) 0.056(3) Uani 1 1 d . . . . .
H20 H 0.2032 0.6092 0.0791 0.067 Uiso 1 1 calc R . . . .
C21A C 0.5586(8) 0.9542(17) 0.1799(6) 0.042(4) Uani 0.5 1 d . U . A 1
H21A H 0.5431 0.8764 0.1633 0.051 Uiso 0.5 1 calc R . . A 1
C22A C 0.5981(10) 1.054(2) 0.1629(8) 0.075(6) Uani 0.5 1 d . U . A 1
H22A H 0.6174 1.0306 0.1403 0.089 Uiso 0.5 1 calc R . . A 1
C24A C 0.6150(12) 1.175(2) 0.2247(9) 0.080(6) Uani 0.5 1 d . U . A 1
H24A H 0.6469 1.2342 0.2457 0.096 Uiso 0.5 1 calc R . . A 1
C25A C 0.5766(8) 1.0853(15) 0.2454(6) 0.038(4) Uani 0.5 1 d . U . A 1
H25A H 0.5741 1.1021 0.2756 0.045 Uiso 0.5 1 calc R . . A 1
C21B C 0.5085(4) 1.0954(9) 0.1991(4) 0.095(8) Uani 0.5 1 d . U . A 2
H21B H 0.4631 1.1065 0.1984 0.114 Uiso 0.5 1 calc R . . A 2
C22B C 0.5375(7) 1.1891(8) 0.1789(5) 0.138(11) Uani 0.5 1 d G U . A 2
H22B H 0.5115 1.2629 0.1647 0.165 Uiso 0.5 1 calc R . . A 2
C23 C 0.6054(7) 1.1725(10) 0.1799(4) 0.043(4) Uani 0.5 1 d G U . . .
H23 H 0.6036 1.2457 0.1612 0.052 Uiso 0.5 1 calc R . . A 1
H23A H 0.6248 1.2353 0.1664 0.052 Uiso 0.5 1 calc R . . A 2
C23B C 0.6442(5) 1.0622(12) 0.2012(5) 0.099(8) Uani 0.5 1 d G U . A 2
H23B H 0.6896 1.0511 0.2018 0.119 Uiso 0.5 1 calc R . . A 2
C24B C 0.6152(4) 0.9685(9) 0.2213(4) 0.078(6) Uani 0.5 1 d G U . A 2
H24B H 0.6412 0.8947 0.2355 0.094 Uiso 0.5 1 calc R . . A 2
N2 N 0.5474(3) 0.9851(6) 0.2203(2) 0.0347(15) Uani 1 1 d G . . . .
H7A H 0.381(3) 0.898(4) 0.186(2) 0.04(2) Uiso 1 1 d D . . . .
H7B H 0.409(4) 0.817(7) 0.1573(11) 0.07(3) Uiso 1 1 d 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
Ni1 O1 2.038(5) . ?
Ni1 O3 2.050(4) 4_545 ?
Ni1 O6 2.056(5) 7_565 ?
Ni1 O7 2.144(5) . ?
Ni1 O8 2.086(5) . ?
Ni1 N1 2.068(6) . ?
Ni2 O4 2.072(4) 3_545 ?
Ni2 O4 2.072(4) 4_545 ?
Ni2 O7 2.071(5) . ?
Ni2 O7 2.071(5) 2_655 ?
Ni2 N2 2.137(13) 2_655 ?
Ni2 N2 2.137(5) . ?
O1 C1 1.240(8) . ?
O2 C1 1.257(8) . ?
O3 Ni1 2.051(4) 4 ?
O3 C5 1.251(8) . ?
O4 Ni2 2.072(4) 3_455 ?
O4 C5 1.262(7) . ?
O5 C13 1.246(9) . ?
O6 Ni1 2.056(5) 7_565 ?
O6 C13 1.258(8) . ?
O7 H7A 0.858(10) . ?
O7 H7B 0.852(10) . ?
O8 H8A 0.8475 . ?
O8 H8B 0.6971 . ?
N1 C16 1.313(10) . ?
N1 C20 1.314(10) . ?
C1 C2 1.504(9) . ?
C2 C3 1.389(8) . ?
C2 C8 1.392(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.394(8) . ?
C4 C5 1.502(9) . ?
C4 C6 1.402(10) . ?
C6 H6 0.9300 . ?
C6 C7 1.351(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.409(9) . ?
C8 C9 1.489(9) . ?
C9 C10 1.406(9) . ?
C9 C15 1.363(10) . ?
C10 H10 0.9300 . ?
C10 C11 1.363(9) . ?
C11 H11 0.9300 . ?
C11 C12 1.372(10) . ?
C12 C13 1.486(9) . ?
C12 C14 1.381(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.384(9) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.329(14) . ?
C17 H17 0.9300 . ?
C17 C18 1.352(19) . ?
C18 H18 0.9300 . ?
C18 C19 1.387(17) . ?
C19 H19 0.9300 . ?
C19 C20 1.378(13) . ?
C20 H20 0.9300 . ?
C21A H21A 0.9300 . ?
C21A C22A 1.51(2) . ?
C21A N2 1.341(15) . ?
C22A H22A 0.9300 . ?
C22A C23 1.31(2) . ?
C24A H24A 0.9300 . ?
C24A C25A 1.49(2) . ?
C24A C23 1.26(2) . ?
C25A H25A 0.9300 . ?
C25A N2 1.276(16) . ?
C21B H21B 0.9300 . ?
C21B C22B 1.3900 . ?
C21B N2 1.3900 . ?
C22B H22B 0.9300 . ?
C22B C23 1.3900 . ?
C23 H23 0.9300 . ?
C23 H23A 0.9300 . ?
C23 C23B 1.3900 . ?
C23B H23B 0.9300 . ?
C23B C24B 1.3900 . ?
C24B H24B 0.9300 . ?
C24B N2 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O3 88.62(19) . 4_545 ?
O1 Ni1 O6 93.4(2) . 7_565 ?
O1 Ni1 O7 92.38(19) . . ?
O1 Ni1 O8 173.9(2) . . ?
O1 Ni1 N1 86.8(2) . . ?
O3 Ni1 O6 177.9(2) 4_545 7_565 ?
O3 Ni1 O7 89.54(19) 4_545 . ?
O3 Ni1 O8 88.1(2) 4_545 . ?
O3 Ni1 N1 93.2(2) 4_545 . ?
O6 Ni1 O7 90.61(19) 7_565 . ?
O6 Ni1 O8 89.8(2) 7_565 . ?
O6 Ni1 N1 86.7(2) 7_565 . ?
O8 Ni1 O7 92.79(19) . . ?
N1 Ni1 O7 177.1(2) . . ?
N1 Ni1 O8 88.2(2) . . ?
O4 Ni2 O4 88.1(3) 3_545 4_545 ?
O4 Ni2 N2 176.3(6) 3_545 2_655 ?
O4 Ni2 N2 89.7(2) 3_545 . ?
O4 Ni2 N2 89.7(5) 4_545 2_655 ?
O4 Ni2 N2 176.3(2) 4_545 . ?
O7 Ni2 O4 91.22(18) 2_655 3_545 ?
O7 Ni2 O4 86.64(19) . 3_545 ?
O7 Ni2 O4 86.64(19) 2_655 4_545 ?
O7 Ni2 O4 91.22(19) . 4_545 ?
O7 Ni2 O7 177.0(3) . 2_655 ?
O7 Ni2 N2 91.7(2) . . ?
O7 Ni2 N2 91.6(7) 2_655 2_655 ?
O7 Ni2 N2 90.4(2) 2_655 . ?
O7 Ni2 N2 90.4(7) . 2_655 ?
N2 Ni2 N2 92.7(6) 2_655 . ?
C1 O1 Ni1 128.6(5) . . ?
C5 O3 Ni1 128.5(4) . 4 ?
C5 O4 Ni2 136.3(5) . 3_455 ?
C13 O6 Ni1 129.4(5) . 7_565 ?
Ni1 O7 H7A 100(5) . . ?
Ni1 O7 H7B 78(6) . . ?
Ni2 O7 Ni1 123.7(2) . . ?
Ni2 O7 H7A 108(4) . . ?
Ni2 O7 H7B 124(5) . . ?
H7A O7 H7B 118(2) . . ?
Ni1 O8 H8A 77.5 . . ?
Ni1 O8 H8B 91.9 . . ?
H8A O8 H8B 47.9 . . ?
C16 N1 Ni1 121.2(6) . . ?
C16 N1 C20 117.7(8) . . ?
C20 N1 Ni1 120.8(6) . . ?
O1 C1 O2 124.8(7) . . ?
O1 C1 C2 116.6(6) . . ?
O2 C1 C2 118.6(7) . . ?
C3 C2 C1 116.7(6) . . ?
C3 C2 C8 120.1(6) . . ?
C8 C2 C1 123.2(6) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.4(6) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 120.9(6) . . ?
C3 C4 C6 116.9(6) . . ?
C6 C4 C5 122.1(6) . . ?
O3 C5 O4 126.3(6) . . ?
O3 C5 C4 116.9(6) . . ?
O4 C5 C4 116.8(6) . . ?
C4 C6 H6 118.5 . . ?
C7 C6 C4 122.9(6) . . ?
C7 C6 H6 118.5 . . ?
C6 C7 H7 120.1 . . ?
C6 C7 C8 119.8(7) . . ?
C8 C7 H7 120.1 . . ?
C2 C8 C7 118.9(6) . . ?
C2 C8 C9 122.1(6) . . ?
C7 C8 C9 119.0(6) . . ?
C10 C9 C8 119.5(7) . . ?
C15 C9 C8 122.3(6) . . ?
C15 C9 C10 118.1(7) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.6(8) . . ?
C11 C10 H10 120.7 . . ?
C10 C11 H11 117.8 . . ?
C10 C11 C12 124.4(7) . . ?
C12 C11 H11 117.8 . . ?
C11 C12 C13 122.1(6) . . ?
C11 C12 C14 115.8(6) . . ?
C14 C12 C13 122.1(7) . . ?
O5 C13 O6 124.4(7) . . ?
O5 C13 C12 117.6(7) . . ?
O6 C13 C12 117.9(7) . . ?
C12 C14 H14 119.3 . . ?
C12 C14 C15 121.3(8) . . ?
C15 C14 H14 119.3 . . ?
C9 C15 C14 121.4(7) . . ?
C9 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
N1 C16 H16 117.7 . . ?
N1 C16 C17 124.6(11) . . ?
C17 C16 H16 117.7 . . ?
C16 C17 H17 121.8 . . ?
C16 C17 C18 116.5(13) . . ?
C18 C17 H17 121.8 . . ?
C17 C18 H18 118.4 . . ?
C17 C18 C19 123.2(13) . . ?
C19 C18 H18 118.4 . . ?
C18 C19 H19 123.3 . . ?
C20 C19 C18 113.5(12) . . ?
C20 C19 H19 123.3 . . ?
N1 C20 C19 124.4(10) . . ?
N1 C20 H20 117.8 . . ?
C19 C20 H20 117.8 . . ?
C22A C21A H21A 122.0 . . ?
N2 C21A H21A 122.0 . . ?
N2 C21A C22A 116.0(15) . . ?
C21A C22A H22A 119.9 . . ?
C23 C22A C21A 120.2(15) . . ?
C23 C22A H22A 119.9 . . ?
C25A C24A H24A 119.0 . . ?
C23 C24A H24A 119.0 . . ?
C23 C24A C25A 122.0(19) . . ?
C24A C25A H25A 121.0 . . ?
N2 C25A C24A 118.0(15) . . ?
N2 C25A H25A 121.0 . . ?
C22B C21B H21B 120.0 . . ?
C22B C21B N2 120.0 . . ?
N2 C21B H21B 120.0 . . ?
C21B C22B H22B 120.0 . . ?
C21B C22B C23 120.0 . . ?
C23 C22B H22B 120.0 . . ?
C22A C23 H23 124.2 . . ?
C24A C23 C22A 111.5(14) . . ?
C24A C23 H23 124.2 . . ?
C22B C23 H23A 120.0 . . ?
C23B C23 C22B 120.0 . . ?
C23B C23 H23A 120.0 . . ?
C23 C23B H23B 120.0 . . ?
C24B C23B C23 120.0 . . ?
C24B C23B H23B 120.0 . . ?
C23B C24B H24B 120.0 . . ?
C23B C24B N2 120.0 . . ?
N2 C24B H24B 120.0 . . ?
C21A N2 Ni2 117.9(8) . . ?
C25A N2 Ni2 120.5(8) . . ?
C25A N2 C21A 120.1(11) . . ?
C21B N2 Ni2 118.6(4) . . ?
C24B N2 Ni2 121.4(4) . . ?
C24B N2 C21B 120.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O8 H8A O3 0.85 2.33 2.876(7) 122.5 4_545
O8 H8B O4 0.70 2.12 2.794(7) 163.6 3_545
O7 H7A O2 0.858(10) 1.73(3) 2.551(7) 159(6) .
O7 H7B O5 0.852(10) 1.76(3) 2.578(7) 160(7) 7_565
O7 H7B O6 0.852(10) 2.35(6) 2.986(7) 132(7) 7_565

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
Ni1 O1 C1 O2 7.3(10) . . . . ?
Ni1 O1 C1 C2 -172.9(4) . . . . ?
Ni1 O3 C5 O4 27.4(11) 4 . . . ?
Ni1 O3 C5 C4 -153.1(5) 4 . . . ?
Ni1 O6 C13 O5 16.2(12) 7_565 . . . ?
Ni1 O6 C13 C12 -160.6(5) 7_565 . . . ?
Ni1 N1 C16 C17 -174.3(10) . . . . ?
Ni1 N1 C20 C19 176.4(9) . . . . ?
Ni2 O4 C5 O3 23.4(12) 3_455 . . . ?
Ni2 O4 C5 C4 -156.2(5) 3_455 . . . ?
O1 C1 C2 C3 122.4(7) . . . . ?
O1 C1 C2 C8 -55.9(10) . . . . ?
O2 C1 C2 C3 -57.8(9) . . . . ?
O2 C1 C2 C8 123.9(8) . . . . ?
N1 C16 C17 C18 -1(2) . . . . ?
C1 C2 C3 C4 -178.1(7) . . . . ?
C1 C2 C8 C7 179.2(7) . . . . ?
C1 C2 C8 C9 -2.6(12) . . . . ?
C2 C3 C4 C5 -179.7(7) . . . . ?
C2 C3 C4 C6 -2.0(11) . . . . ?
C2 C8 C9 C10 -48.0(11) . . . . ?
C2 C8 C9 C15 134.8(8) . . . . ?
C3 C2 C8 C7 1.0(11) . . . . ?
C3 C2 C8 C9 179.2(7) . . . . ?
C3 C4 C5 O3 1.7(11) . . . . ?
C3 C4 C5 O4 -178.7(7) . . . . ?
C3 C4 C6 C7 2.8(12) . . . . ?
C4 C6 C7 C8 -1.7(12) . . . . ?
C5 C4 C6 C7 -179.5(7) . . . . ?
C6 C4 C5 O3 -175.9(7) . . . . ?
C6 C4 C5 O4 3.7(11) . . . . ?
C6 C7 C8 C2 -0.3(11) . . . . ?
C6 C7 C8 C9 -178.5(7) . . . . ?
C7 C8 C9 C10 130.1(8) . . . . ?
C7 C8 C9 C15 -47.1(11) . . . . ?
C8 C2 C3 C4 0.1(11) . . . . ?
C8 C9 C10 C11 -175.2(7) . . . . ?
C8 C9 C15 C14 175.1(7) . . . . ?
C9 C10 C11 C12 1.9(13) . . . . ?
C10 C9 C15 C14 -2.1(12) . . . . ?
C10 C11 C12 C13 172.2(8) . . . . ?
C10 C11 C12 C14 -5.6(13) . . . . ?
C11 C12 C13 O5 169.8(8) . . . . ?
C11 C12 C13 O6 -13.2(12) . . . . ?
C11 C12 C14 C15 5.4(12) . . . . ?
C12 C14 C15 C9 -1.7(12) . . . . ?
C13 C12 C14 C15 -172.4(7) . . . . ?
C14 C12 C13 O5 -12.6(12) . . . . ?
C14 C12 C13 O6 164.4(7) . . . . ?
C15 C9 C10 C11 2.1(12) . . . . ?
C16 N1 C20 C19 2.8(14) . . . . ?
C16 C17 C18 C19 1(2) . . . . ?
C17 C18 C19 C20 0(2) . . . . ?
C18 C19 C20 N1 -2.5(18) . . . . ?
C20 N1 C16 C17 -0.8(15) . . . . ?
C21A C22A C23 C24A 37(2) . . . . ?
C22A C21A N2 Ni2 -174.8(10) . . . . ?
C22A C21A N2 C25A -8.2(18) . . . . ?
C24A C25A N2 Ni2 174.1(11) . . . . ?
C24A C25A N2 C21A 8(2) . . . . ?
C25A C24A C23 C22A -39(3) . . . . ?
C21B C22B C23 C23B 0.0 . . . . ?
C22B C21B N2 Ni2 -179.2(5) . . . . ?
C22B C21B N2 C24B 0.0 . . . . ?
C22B C23 C23B C24B 0.0 . . . . ?
C23 C24A C25A N2 17(3) . . . . ?
C23 C23B C24B N2 0.0 . . . . ?
C23B C24B N2 Ni2 179.2(5) . . . . ?
C23B C24B N2 C21B 0.0 . . . . ?
N2 C21A C22A C23 -15(2) . . . . ?
N2 C21B C22B C23 0.0 . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.150 0.750 10.1 0.6 ?
2 -0.625 -0.125 0.500 591.1 9.1 ?
3 -0.029 0.529 1.000 591.1 9.1 ?
4 0.000 0.850 0.250 10.1 0.4 ?
5 0.500 0.350 0.250 10.1 0.4 ?
6 0.500 0.650 0.750 10.1 0.6 ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-06-04
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_241-8co1
_database_code_depnum_ccdc_archive 'CCDC 1430231'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2015-09-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C200 H168 Co12 N16 O64), 2(C5 H5 N)'
_chemical_formula_sum            'C60 H52 Co3 N6 O16'
_chemical_formula_weight         1289.86
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   20.600(5)
_cell_length_b                   10.4271(11)
_cell_length_c                   29.646(5)
_cell_angle_alpha                90
_cell_angle_beta                 113.51(2)
_cell_angle_gamma                90
_cell_volume                     5840(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    895
_cell_measurement_temperature    297.16(10)
_cell_measurement_theta_max      21.1820
_cell_measurement_theta_min      3.8920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_av_unetI/netI     0.1848
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            10401
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         3.374
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.16(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -20.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000   30.0000 33

#__ type_ start__ end____ width___ exp.time_
  2 omega  -19.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   19.0000  -90.0000 107

#__ type_ start__ end____ width___ exp.time_
  3 omega  -32.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -38.0000   60.0000 78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0291518000
_diffrn_orient_matrix_UB_12      0.0360804000
_diffrn_orient_matrix_UB_13      -0.0000599000
_diffrn_orient_matrix_UB_21      -0.0200984000
_diffrn_orient_matrix_UB_22      0.0181828000
_diffrn_orient_matrix_UB_23      -0.0247472000
_diffrn_orient_matrix_UB_31      -0.0125588000
_diffrn_orient_matrix_UB_32      0.0546788000
_diffrn_orient_matrix_UB_33      0.0082758000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2598
_reflns_number_total             5169
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         5169
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.0829
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0665P)²+2.2581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.2278
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H8A-O8
 0.86 with sigma of 0.01
 O8-H8B
 0.86 with sigma of 0.01
 H8A-H8B
 1.48 with sigma of 0.01
3. Rigid bond restraints
 N3, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C30 \\sim N3: within 1.2A with sigma of 0.02 and sigma for terminal atoms of
0.04
C16 \\sim N1: within 1.2A with sigma of 0.02 and sigma for terminal atoms of
0.05
C20 \\sim N1: within 1.2A with sigma of 0.02 and sigma for terminal atoms of
0.05
Uanis(C26') \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C27') \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C29') \\sim Ueq, Uanis(C30') \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H28(0.5) H28A(0.5) C26'(0.5) H26'(0.5) C27'(0.5) H27'(0.5)
 C29'(0.5) H29'(0.5) C30'(0.5) H30'(0.5) C29(0.5) H29(0.5) C26(0.5) H26(0.5)
 C27(0.5) H27(0.5) C30(0.5) H30(0.5)
6.a Rotating group:
 O7(H7A,H7B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C28(H28A), C26'(H26'), C27'(H27'), C29'(H29'), C30'(H30'),
  C29(H29), C26(H26), C27(H27), C30(H30)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.65927(12) 0.2500 0.0235(4) Uani 1 2 d S T P . .
Co2 Co 0.16514(5) 0.82583(9) 0.33702(4) 0.0243(3) Uani 1 1 d . . . . .
O1 O 0.0402(3) 0.8053(4) 0.21925(18) 0.0287(13) Uani 1 1 d . . . . .
O2 O 0.1552(3) 0.8441(5) 0.26513(19) 0.0356(14) Uani 1 1 d . . . . .
O3 O 0.3022(3) 1.0175(5) 0.1728(2) 0.0441(16) Uani 1 1 d . . . . .
O4 O 0.2496(3) 1.2088(5) 0.14893(18) 0.0321(13) Uani 1 1 d . . . . .
O5 O 0.0850(3) 1.3292(5) -0.0990(2) 0.0441(16) Uani 1 1 d . . . . .
O6 O 0.1694(3) 1.1875(5) -0.09162(19) 0.0397(15) Uani 1 1 d . . . . .
O7 O 0.0810(3) 0.9554(5) 0.31836(19) 0.0393(15) Uani 1 1 d . . . . .
H7A H 0.0871 1.0112 0.3425 0.059 Uiso 1 1 d GR . . . .
H7B H 0.0402 0.9154 0.3122 0.059 Uiso 1 1 d GR . . . .
O8 O 0.0904(3) 0.6623(5) 0.31578(18) 0.0243(12) Uani 1 1 d D . . . .
N1 N 0.0503(4) 0.5137(6) 0.2220(2) 0.0364(18) Uani 1 1 d . U . . .
N2 N 0.2385(4) 0.9792(6) 0.3628(3) 0.0403(19) Uani 1 1 d . . . . .
C1 C 0.1006(4) 0.8506(7) 0.2257(3) 0.0291(19) Uani 1 1 d . . . . .
C2 C 0.1073(4) 0.9133(7) 0.1832(3) 0.0260(18) Uani 1 1 d . . . . .
C3 C 0.1704(4) 0.9692(6) 0.1871(3) 0.0220(17) Uani 1 1 d . . . . .
H3 H 0.2091 0.9648 0.2172 0.026 Uiso 1 1 calc R . . . .
C4 C 0.1786(4) 1.0312(6) 0.1485(3) 0.0235(18) Uani 1 1 d . . . . .
C5 C 0.2492(4) 1.0896(7) 0.1575(3) 0.0271(19) Uani 1 1 d . . . . .
C6 C 0.1208(4) 1.0394(7) 0.1026(3) 0.0260(18) Uani 1 1 d . . . . .
C7 C 0.0588(4) 0.9817(7) 0.0988(3) 0.037(2) Uani 1 1 d . . . . .
H7 H 0.0203 0.9829 0.0686 0.044 Uiso 1 1 calc R . . . .
C8 C 0.0512(4) 0.9229(7) 0.1376(3) 0.035(2) Uani 1 1 d . . . . .
H8 H 0.0075 0.8884 0.1334 0.042 Uiso 1 1 calc R . . . .
C9 C 0.1255(4) 1.1014(7) 0.0589(3) 0.0281(19) Uani 1 1 d . . . . .
C10 C 0.1821(5) 1.0716(7) 0.0464(3) 0.037(2) Uani 1 1 d . . . . .
H10 H 0.2184 1.0186 0.0665 0.044 Uiso 1 1 calc R . . . .
C11 C 0.1840(5) 1.1222(8) 0.0033(3) 0.037(2) Uani 1 1 d . . . . .
H11 H 0.2218 1.1024 -0.0050 0.045 Uiso 1 1 calc R . . . .
C12 C 0.1299(4) 1.2021(7) -0.0277(3) 0.0297(19) Uani 1 1 d . . . . .
C13 C 0.1289(5) 1.2447(8) -0.0761(3) 0.031(2) Uani 1 1 d . . . . .
C14 C 0.0771(5) 1.2336(8) -0.0134(3) 0.036(2) Uani 1 1 d . . . . .
H14 H 0.0416 1.2891 -0.0329 0.043 Uiso 1 1 calc R . . . .
C15 C 0.0741(4) 1.1855(8) 0.0299(3) 0.042(2) Uani 1 1 d . . . . .
H15 H 0.0376 1.2101 0.0390 0.050 Uiso 1 1 calc R . . . .
C16 C 0.0728(8) 0.4074(12) 0.2432(5) 0.109(5) Uani 1 1 d . U . . .
H16 H 0.0656 0.3872 0.2714 0.131 Uiso 1 1 calc R . . . .
C17 C 0.1111(10) 0.3125(16) 0.2240(7) 0.153(7) Uani 1 1 d . U . . .
H17 H 0.1253 0.2321 0.2381 0.184 Uiso 1 1 calc R . . . .
C18 C 0.1224(10) 0.3513(17) 0.1867(7) 0.136(6) Uani 1 1 d . U . . .
H18 H 0.1480 0.2981 0.1747 0.163 Uiso 1 1 calc R . . . .
C19 C 0.1010(12) 0.456(2) 0.1655(8) 0.175(8) Uani 1 1 d . U . . .
H19 H 0.1069 0.4788 0.1370 0.210 Uiso 1 1 calc R . . . .
C20 C 0.0685(8) 0.5355(14) 0.1865(6) 0.121(5) Uani 1 1 d . U . . .
H20 H 0.0582 0.6173 0.1730 0.146 Uiso 1 1 calc R . . . .
C21 C 0.2925(6) 0.9695(10) 0.4057(4) 0.068(3) Uani 1 1 d . . . . .
H21 H 0.3005 0.8926 0.4229 0.082 Uiso 1 1 calc R . . . .
C22 C 0.3383(8) 1.0737(14) 0.4258(6) 0.129(6) Uani 1 1 d . . . . .
H22 H 0.3755 1.0675 0.4565 0.155 Uiso 1 1 calc R . . . .
C23 C 0.3265(9) 1.1856(14) 0.3986(7) 0.129(7) Uani 1 1 d . . . . .
H23 H 0.3583 1.2535 0.4094 0.155 Uiso 1 1 calc R . . . .
C24 C 0.2694(9) 1.1949(12) 0.3570(6) 0.116(6) Uani 1 1 d . . . . .
H24 H 0.2574 1.2720 0.3400 0.139 Uiso 1 1 calc R . . . .
C25 C 0.2288(6) 1.0884(9) 0.3400(4) 0.071(3) Uani 1 1 d . . . . .
H25 H 0.1910 1.0942 0.3095 0.085 Uiso 1 1 calc R . . . .
N3 N -0.0981(6) 1.1424(9) 0.1129(4) 0.080(3) Uani 1 1 d . U . . .
C28 C -0.1372(12) 1.3615(19) 0.0575(8) 0.164(8) Uani 1 1 d . U . . .
H28 H -0.1457 1.4336 0.0375 0.197 Uiso 0.5 1 calc R . . A 1
H28A H -0.1479 1.4335 0.0374 0.197 Uiso 0.5 1 calc R . . B 2
C26' C -0.1490(16) 1.139(3) 0.0756(11) 0.081(8) Uani 0.5 1 d . U . C 2
H26' H -0.1735 1.0618 0.0674 0.098 Uiso 0.5 1 calc R . . C 2
C27' C -0.178(2) 1.251(4) 0.0392(13) 0.148(13) Uani 0.5 1 d . U . C 2
H27' H -0.2177 1.2467 0.0095 0.177 Uiso 0.5 1 calc R . . C 2
C29' C -0.0890(16) 1.370(2) 0.0972(10) 0.086(8) Uani 0.5 1 d . U . C 2
H29' H -0.0687 1.4494 0.1093 0.103 Uiso 0.5 1 calc R . . C 2
C30' C -0.0630(19) 1.252(3) 0.1262(12) 0.112(10) Uani 0.5 1 d . U . C 2
H30' H -0.0212 1.2549 0.1543 0.134 Uiso 0.5 1 calc R . . C 2
C29 C -0.1476(16) 1.379(2) 0.0988(10) 0.086(8) Uani 0.5 1 d . U . C 1
H29 H -0.1729 1.4445 0.1057 0.103 Uiso 0.5 1 calc R . . C 1
C26 C -0.109(3) 1.136(4) 0.0662(18) 0.164(17) Uani 0.5 1 d . U . C 1
H26 H -0.1140 1.0553 0.0521 0.196 Uiso 0.5 1 calc R . . C 1
C27 C -0.113(2) 1.238(4) 0.0367(14) 0.149(13) Uani 0.5 1 d . U . C 1
H27 H -0.1025 1.2361 0.0088 0.179 Uiso 0.5 1 calc R . . C 1
C30 C -0.113(2) 1.279(4) 0.1289(15) 0.146(11) Uani 0.5 1 d . U . C 1
H30 H -0.0957 1.2938 0.1626 0.176 Uiso 0.5 1 calc R . . C 1
H8A H 0.083(4) 0.668(6) 0.3423(15) 0.05(3) Uiso 1 1 d D . . . .
H8B H 0.123(3) 0.609(5) 0.316(2) 0.03(2) Uiso 1 1 d 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
Co1 O1 2.107(5) . ?
Co1 O1 2.107(5) 2 ?
Co1 O8 2.092(5) 2 ?
Co1 O8 2.092(5) . ?
Co1 N1 2.179(6) . ?
Co1 N1 2.179(6) 2 ?
Co2 O2 2.067(5) . ?
Co2 O4 2.040(5) 4_545 ?
Co2 O6 2.087(5) 6_576 ?
Co2 O7 2.091(5) . ?
Co2 O8 2.214(5) . ?
Co2 N2 2.122(7) . ?
O1 C1 1.271(9) . ?
O2 C1 1.260(9) . ?
O3 C5 1.252(9) . ?
O4 Co2 2.040(5) 4 ?
O4 C5 1.270(8) . ?
O5 C13 1.252(9) . ?
O6 Co2 2.087(5) 6_575 ?
O6 C13 1.253(9) . ?
O7 H7A 0.8915 . ?
O7 H7B 0.8898 . ?
O8 H8A 0.864(10) . ?
O8 H8B 0.863(10) . ?
N1 C16 1.268(13) . ?
N1 C20 1.273(14) . ?
N2 C21 1.316(11) . ?
N2 C25 1.299(10) . ?
C1 C2 1.475(10) . ?
C2 C3 1.387(10) . ?
C2 C8 1.386(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.384(9) . ?
C4 C5 1.498(10) . ?
C4 C6 1.409(10) . ?
C6 C7 1.376(10) . ?
C6 C9 1.485(10) . ?
C7 H7 0.9300 . ?
C7 C8 1.367(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.393(11) . ?
C9 C15 1.380(10) . ?
C10 H10 0.9300 . ?
C10 C11 1.397(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.402(10) . ?
C12 C13 1.494(10) . ?
C12 C14 1.357(11) . ?
C14 H14 0.9300 . ?
C14 C15 1.401(10) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.512(19) . ?
C17 H17 0.9300 . ?
C17 C18 1.28(2) . ?
C18 H18 0.9300 . ?
C18 C19 1.25(2) . ?
C19 H19 0.9300 . ?
C19 C20 1.360(18) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.406(14) . ?
C22 H22 0.9300 . ?
C22 C23 1.383(19) . ?
C23 H23 0.9300 . ?
C23 C24 1.325(19) . ?
C24 H24 0.9300 . ?
C24 C25 1.361(14) . ?
C25 H25 0.9300 . ?
N3 C26' 1.18(3) . ?
N3 C30' 1.33(3) . ?
N3 C26 1.32(4) . ?
N3 C30 1.56(4) . ?
C28 H28 0.9300 . ?
C28 H28A 0.9300 . ?
C28 C27' 1.40(4) . ?
C28 C29' 1.20(3) . ?
C28 C29 1.34(3) . ?
C28 C27 1.59(4) . ?
C26' H26' 0.9300 . ?
C26' C27' 1.54(4) . ?
C27' H27' 0.9300 . ?
C29' H29' 0.9300 . ?
C29' C30' 1.47(4) . ?
C30' H30' 0.9300 . ?
C29 H29 0.9300 . ?
C29 C30 1.38(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.35(5) . ?
C27 H27 0.9300 . ?
C30 H30 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
O1 Co1 O1 87.4(3) 2 . ?
O1 Co1 N1 175.3(2) . 2 ?
O1 Co1 N1 90.6(2) 2 2 ?
O1 Co1 N1 175.3(2) 2 . ?
O1 Co1 N1 90.6(2) . . ?
O8 Co1 O1 86.8(2) 2 . ?
O8 Co1 O1 86.8(2) . 2 ?
O8 Co1 O1 92.0(2) 2 2 ?
O8 Co1 O1 92.0(2) . . ?
O8 Co1 O8 178.3(3) . 2 ?
O8 Co1 N1 89.1(2) . . ?
O8 Co1 N1 89.1(2) 2 2 ?
O8 Co1 N1 92.2(2) 2 . ?
O8 Co1 N1 92.2(2) . 2 ?
N1 Co1 N1 91.7(4) . 2 ?
O2 Co2 O6 176.7(2) . 6_576 ?
O2 Co2 O7 86.4(2) . . ?
O2 Co2 O8 90.3(2) . . ?
O2 Co2 N2 93.8(2) . . ?
O4 Co2 O2 89.4(2) 4_545 . ?
O4 Co2 O6 93.9(2) 4_545 6_576 ?
O4 Co2 O7 174.7(2) 4_545 . ?
O4 Co2 O8 92.4(2) 4_545 . ?
O4 Co2 N2 86.9(2) 4_545 . ?
O6 Co2 O7 90.4(2) 6_576 . ?
O6 Co2 O8 88.9(2) 6_576 . ?
O6 Co2 N2 87.1(3) 6_576 . ?
O7 Co2 O8 90.8(2) . . ?
O7 Co2 N2 90.3(2) . . ?
N2 Co2 O8 175.8(2) . . ?
C1 O1 Co1 137.2(5) . . ?
C1 O2 Co2 130.3(5) . . ?
C5 O4 Co2 128.2(5) . 4 ?
C13 O6 Co2 129.7(5) . 6_575 ?
Co2 O7 H7A 111.9 . . ?
Co2 O7 H7B 111.5 . . ?
H7A O7 H7B 106.9 . . ?
Co1 O8 Co2 122.4(2) . . ?
Co1 O8 H8A 116(5) . . ?
Co1 O8 H8B 113(4) . . ?
Co2 O8 H8A 92(5) . . ?
Co2 O8 H8B 93(5) . . ?
H8A O8 H8B 117(2) . . ?
C16 N1 Co1 123.8(8) . . ?
C16 N1 C20 113.3(11) . . ?
C20 N1 Co1 122.2(8) . . ?
C21 N2 Co2 119.8(6) . . ?
C25 N2 Co2 122.2(7) . . ?
C25 N2 C21 117.7(9) . . ?
O1 C1 C2 117.1(7) . . ?
O2 C1 O1 125.3(7) . . ?
O2 C1 C2 117.6(7) . . ?
C3 C2 C1 121.2(7) . . ?
C8 C2 C1 122.5(7) . . ?
C8 C2 C3 116.2(7) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 C2 123.1(7) . . ?
C4 C3 H3 118.5 . . ?
C3 C4 C5 118.1(7) . . ?
C3 C4 C6 119.5(7) . . ?
C6 C4 C5 122.4(6) . . ?
O3 C5 O4 125.8(7) . . ?
O3 C5 C4 117.8(6) . . ?
O4 C5 C4 116.4(7) . . ?
C4 C6 C9 122.9(7) . . ?
C7 C6 C4 116.9(7) . . ?
C7 C6 C9 120.1(7) . . ?
C6 C7 H7 118.6 . . ?
C8 C7 C6 122.8(7) . . ?
C8 C7 H7 118.6 . . ?
C2 C8 H8 119.3 . . ?
C7 C8 C2 121.4(7) . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C6 119.3(7) . . ?
C15 C9 C6 121.2(7) . . ?
C15 C9 C10 119.5(7) . . ?
C9 C10 H10 120.3 . . ?
C9 C10 C11 119.4(8) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 H11 119.4 . . ?
C10 C11 C12 121.3(8) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C13 120.5(8) . . ?
C14 C12 C11 117.8(7) . . ?
C14 C12 C13 121.6(8) . . ?
O5 C13 O6 125.4(8) . . ?
O5 C13 C12 117.4(8) . . ?
O6 C13 C12 117.1(8) . . ?
C12 C14 H14 118.9 . . ?
C12 C14 C15 122.2(8) . . ?
C15 C14 H14 118.9 . . ?
C9 C15 C14 119.7(8) . . ?
C9 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
N1 C16 H16 119.0 . . ?
N1 C16 C17 121.9(14) . . ?
C17 C16 H16 119.0 . . ?
C16 C17 H17 122.6 . . ?
C18 C17 C16 114.8(16) . . ?
C18 C17 H17 122.6 . . ?
C17 C18 H18 117.9 . . ?
C19 C18 C17 124(2) . . ?
C19 C18 H18 117.9 . . ?
C18 C19 H19 122.0 . . ?
C18 C19 C20 116(2) . . ?
C20 C19 H19 122.0 . . ?
N1 C20 C19 129.2(17) . . ?
N1 C20 H20 115.4 . . ?
C19 C20 H20 115.4 . . ?
N2 C21 H21 119.5 . . ?
N2 C21 C22 121.1(11) . . ?
C22 C21 H21 119.5 . . ?
C21 C22 H22 120.9 . . ?
C23 C22 C21 118.2(14) . . ?
C23 C22 H22 120.9 . . ?
C22 C23 H23 120.4 . . ?
C24 C23 C22 119.2(13) . . ?
C24 C23 H23 120.4 . . ?
C23 C24 H24 120.9 . . ?
C23 C24 C25 118.2(13) . . ?
C25 C24 H24 120.9 . . ?
N2 C25 C24 125.3(12) . . ?
N2 C25 H25 117.4 . . ?
C24 C25 H25 117.4 . . ?
C26' N3 C30' 118(2) . . ?
C26 N3 C30 113(3) . . ?
C27' C28 H28A 117.4 . . ?
C29' C28 H28A 117.4 . . ?
C29' C28 C27' 125(3) . . ?
C29 C28 H28 114.5 . . ?
C29 C28 C27 131(2) . . ?
C27 C28 H28 114.5 . . ?
N3 C26' H26' 117.0 . . ?
N3 C26' C27' 126(3) . . ?
C27' C26' H26' 117.0 . . ?
C28 C27' C26' 110(3) . . ?
C28 C27' H27' 125.0 . . ?
C26' C27' H27' 125.0 . . ?
C28 C29' H29' 120.9 . . ?
C28 C29' C30' 118(2) . . ?
C30' C29' H29' 120.9 . . ?
N3 C30' C29' 121(3) . . ?
N3 C30' H30' 119.3 . . ?
C29' C30' H30' 119.3 . . ?
C28 C29 H29 127.5 . . ?
C28 C29 C30 105(3) . . ?
C30 C29 H29 127.5 . . ?
N3 C26 H26 117.1 . . ?
N3 C26 C27 126(4) . . ?
C27 C26 H26 117.1 . . ?
C28 C27 H27 125.4 . . ?
C26 C27 C28 109(3) . . ?
C26 C27 H27 125.4 . . ?
N3 C30 H30 116.3 . . ?
C29 C30 N3 127(3) . . ?
C29 C30 H30 116.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A N3 0.89 1.85 2.739(10) 173.1 2
O7 H7B O1 0.89 1.92 2.776(8) 160.1 2
O8 H8A O5 0.864(10) 1.722(19) 2.575(7) 169(6) 6_576
O8 H8B O3 0.863(10) 1.733(19) 2.585(7) 169(7) 4_545

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
Co1 O1 C1 O2 -24.8(13) . . . . ?
Co1 O1 C1 C2 153.8(5) . . . . ?
Co1 N1 C16 C17 -176.5(11) . . . . ?
Co1 N1 C20 C19 179.0(16) . . . . ?
Co2 O2 C1 O1 -25.3(12) . . . . ?
Co2 O2 C1 C2 156.1(5) . . . . ?
Co2 O4 C5 O3 -6.6(11) 4 . . . ?
Co2 O4 C5 C4 173.3(5) 4 . . . ?
Co2 O6 C13 O5 -16.2(12) 6_575 . . . ?
Co2 O6 C13 C12 159.5(5) 6_575 . . . ?
Co2 N2 C21 C22 -174.2(10) . . . . ?
Co2 N2 C25 C24 172.6(11) . . . . ?
O1 C1 C2 C3 177.9(7) . . . . ?
O1 C1 C2 C8 -0.5(11) . . . . ?
O2 C1 C2 C3 -3.4(11) . . . . ?
O2 C1 C2 C8 178.3(7) . . . . ?
N1 C16 C17 C18 4(3) . . . . ?
N2 C21 C22 C23 -2(2) . . . . ?
C1 C2 C3 C4 -178.7(7) . . . . ?
C1 C2 C8 C7 179.8(7) . . . . ?
C2 C3 C4 C5 179.1(7) . . . . ?
C2 C3 C4 C6 0.2(11) . . . . ?
C3 C2 C8 C7 1.4(12) . . . . ?
C3 C4 C5 O3 57.3(10) . . . . ?
C3 C4 C5 O4 -122.7(7) . . . . ?
C3 C4 C6 C7 -1.3(11) . . . . ?
C3 C4 C6 C9 -178.5(6) . . . . ?
C4 C6 C7 C8 2.5(12) . . . . ?
C4 C6 C9 C10 47.1(11) . . . . ?
C4 C6 C9 C15 -134.4(8) . . . . ?
C5 C4 C6 C7 179.9(7) . . . . ?
C5 C4 C6 C9 2.7(11) . . . . ?
C6 C4 C5 O3 -123.8(8) . . . . ?
C6 C4 C5 O4 56.2(10) . . . . ?
C6 C7 C8 C2 -2.6(13) . . . . ?
C6 C9 C10 C11 175.2(7) . . . . ?
C6 C9 C15 C14 -174.5(7) . . . . ?
C7 C6 C9 C10 -130.0(9) . . . . ?
C7 C6 C9 C15 48.5(11) . . . . ?
C8 C2 C3 C4 -0.2(11) . . . . ?
C9 C6 C7 C8 179.8(7) . . . . ?
C9 C10 C11 C12 -0.1(12) . . . . ?
C10 C9 C15 C14 3.9(12) . . . . ?
C10 C11 C12 C13 -173.8(7) . . . . ?
C10 C11 C12 C14 2.9(12) . . . . ?
C11 C12 C13 O5 -170.7(7) . . . . ?
C11 C12 C13 O6 13.3(11) . . . . ?
C11 C12 C14 C15 -2.3(12) . . . . ?
C12 C14 C15 C9 -1.1(13) . . . . ?
C13 C12 C14 C15 174.4(7) . . . . ?
C14 C12 C13 O5 12.8(11) . . . . ?
C14 C12 C13 O6 -163.3(8) . . . . ?
C15 C9 C10 C11 -3.3(12) . . . . ?
C16 N1 C20 C19 8(2) . . . . ?
C16 C17 C18 C19 -4(3) . . . . ?
C17 C18 C19 C20 5(4) . . . . ?
C18 C19 C20 N1 -8(3) . . . . ?
C20 N1 C16 C17 -6(2) . . . . ?
C21 N2 C25 C24 -1.0(18) . . . . ?
C21 C22 C23 C24 6(3) . . . . ?
C22 C23 C24 C25 -7(3) . . . . ?
C23 C24 C25 N2 5(2) . . . . ?
C25 N2 C21 C22 -0.4(17) . . . . ?
N3 C26' C27' C28 -2(5) . . . . ?
N3 C26 C27 C28 -25(6) . . . . ?
C28 C29' C30' N3 -10(5) . . . . ?
C28 C29 C30 N3 -28(5) . . . . ?
C26' N3 C30' C29' 4(4) . . . . ?
C27' C28 C29' C30' 10(5) . . . . ?
C29' C28 C27' C26' -5(5) . . . . ?
C30' N3 C26' C27' 2(4) . . . . ?
C29 C28 C27 C26 6(6) . . . . ?
C26 N3 C30 C29 14(5) . . . . ?
C27 C28 C29 C30 18(5) . . . . ?
C30 N3 C26 C27 17(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_239-8co
_database_code_depnum_ccdc_archive 'CCDC 1430232'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2015-12-17 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 H33 Co3.50 N2 O17'
_chemical_formula_weight         1019.94

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                   12.0580(7)
_cell_length_b                   12.3182(6)
_cell_length_c                   15.3976(8)
_cell_angle_alpha                67.945(5)
_cell_angle_beta                 88.887(4)
_cell_angle_gamma                80.778(4)
_cell_volume                     2090.23(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1035
_exptl_absorpt_coefficient_mu    1.446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6963
_exptl_absorpt_correction_T_max  0.7322
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12260
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_sigmaI/netI    0.1278
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         25.05
_reflns_number_total             7125
_reflns_number_gt                4434
_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)+(0.1000P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7125
_refine_ls_number_parameters     560
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0704
_refine_ls_wR_factor_ref         0.2193
_refine_ls_wR_factor_gt          0.1741
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.009
_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 -0.02169(9) 0.70262(8) 0.02011(6) 0.0232(3) Uani 1 1 d . . .
Co2 Co 0.21917(9) 0.75625(8) 0.02563(6) 0.0252(3) Uani 1 1 d . . .
Co3 Co 0.0000 1.0000 0.0000 0.0322(4) Uani 1 2 d S . .
Co4 Co 0.51165(9) 0.02720(8) 0.57992(6) 0.0248(3) Uani 1 1 d . . .
N1 N 0.3851(6) 0.6628(6) 0.0600(5) 0.0379(17) Uani 1 1 d . . .
N2 N 0.5115(6) 0.0551(6) 0.7047(4) 0.0330(16) Uani 1 1 d . . .
O1 O 0.2137(5) 0.7339(5) -0.1022(3) 0.0387(14) Uani 1 1 d . . .
O2 O 0.0404(4) 0.6921(4) -0.1078(3) 0.0292(12) Uani 1 1 d . . .
O3 O 0.3876(5) 0.9276(6) -0.3849(4) 0.0522(17) Uani 1 1 d . . .
O4 O 0.3711(5) 0.8799(5) -0.5097(4) 0.0439(15) Uani 1 1 d . . .
O5 O 0.2142(5) 0.7860(4) -0.8522(3) 0.0312(13) Uani 1 1 d . . .
O6 O 0.1379(5) 0.9771(4) -0.8977(3) 0.0385(15) Uani 1 1 d . . .
O7 O 0.0565(4) 0.8506(4) -0.0164(3) 0.0266(12) Uani 1 1 d . . .
H1 H 0.0525 0.8742 -0.0754 0.032 Uiso 1 1 d R . .
O8 O -0.1739(5) 0.7958(5) -0.0655(4) 0.0415(15) Uani 1 1 d . . .
H1W H -0.1767 0.8675 -0.0807 0.050 Uiso 1 1 d R . .
H2W H -0.1105 0.7651 -0.0783 0.050 Uiso 1 1 d R . .
O9 O -0.0941(4) 0.5523(4) 0.0563(3) 0.0313(13) Uani 1 1 d . . .
H3W H -0.1314 0.5553 0.0112 0.038 Uiso 1 1 d R . .
H4W H -0.0609 0.4897 0.0772 0.038 Uiso 1 1 d R . .
O10 O 0.2890(5) 0.9178(5) -0.0484(4) 0.0551(18) Uani 1 1 d . . .
H5W H 0.2377 0.9733 -0.0730 0.066 Uiso 1 1 d R . .
H6W H 0.2499 0.9458 -0.0227 0.066 Uiso 1 1 d R . .
O11 O 0.1353(4) 0.6084(4) 0.0933(3) 0.0274(12) Uani 1 1 d . . .
O12 O 0.2031(5) 0.4285(5) 0.0964(3) 0.0415(15) Uani 1 1 d . . .
O13 O 0.3920(5) 0.1693(5) 0.5096(3) 0.0384(15) Uani 1 1 d . . .
O14 O 0.3711(5) 0.1216(5) 0.3852(4) 0.0455(16) Uani 1 1 d . . .
O15 O 0.0934(5) 0.0842(4) 0.8795(3) 0.0355(14) Uani 1 1 d . . .
O16 O 0.0827(5) 0.2745(4) 0.8632(3) 0.0365(14) Uani 1 1 d . . .
C1 C 0.1323(7) 0.7213(6) -0.1440(5) 0.0287(18) Uani 1 1 d . . .
C2 C 0.1418(7) 0.7452(7) -0.2463(5) 0.0287(18) Uani 1 1 d . . .
C3 C 0.2296(7) 0.7976(6) -0.2940(5) 0.0303(18) Uani 1 1 d . . .
H3 H 0.2833 0.8146 -0.2606 0.036 Uiso 1 1 calc R . .
C4 C 0.2412(7) 0.8263(7) -0.3908(5) 0.0300(18) Uani 1 1 d . . .
C5 C 0.3411(7) 0.8806(7) -0.4321(5) 0.0331(19) Uani 1 1 d . . .
C6 C 0.1618(7) 0.8017(7) -0.4406(5) 0.036(2) Uani 1 1 d . . .
C7 C 0.0723(8) 0.7486(9) -0.3935(6) 0.053(3) Uani 1 1 d . . .
H7 H 0.0184 0.7314 -0.4266 0.064 Uiso 1 1 calc R . .
C8 C 0.0629(8) 0.7212(8) -0.2974(5) 0.052(3) Uani 1 1 d . . .
H8A H 0.0027 0.6862 -0.2673 0.063 Uiso 1 1 calc R . .
C9 C 0.1680(7) 0.8225(7) -0.5418(5) 0.036(2) Uani 1 1 d . . .
C10 C 0.2070(10) 0.7351(8) -0.5711(6) 0.064(3) Uani 1 1 d . . .
H10A H 0.2316 0.6596 -0.5265 0.077 Uiso 1 1 calc R . .
C11 C 0.2125(9) 0.7523(7) -0.6655(5) 0.056(3) Uani 1 1 d . . .
H11 H 0.2431 0.6892 -0.6824 0.067 Uiso 1 1 calc R . .
C12 C 0.1735(7) 0.8606(7) -0.7342(5) 0.0321(19) Uani 1 1 d . . .
C13 C 0.1763(6) 0.8760(7) -0.8342(5) 0.0283(18) Uani 1 1 d . . .
C14 C 0.1272(8) 0.9526(7) -0.7054(5) 0.044(2) Uani 1 1 d . . .
H14 H 0.0981 1.0266 -0.7503 0.053 Uiso 1 1 calc R . .
C15 C 0.1239(8) 0.9356(8) -0.6130(6) 0.051(3) Uani 1 1 d . . .
H15 H 0.0927 0.9981 -0.5956 0.061 Uiso 1 1 calc R . .
C16 C 0.1752(6) 0.4983(6) 0.1356(5) 0.0251(17) Uani 1 1 d . . .
C17 C 0.1835(6) 0.4522(6) 0.2402(4) 0.0242(17) Uani 1 1 d . . .
C18 C 0.2506(6) 0.3442(6) 0.2896(5) 0.0239(17) Uani 1 1 d . . .
H18 H 0.2911 0.3032 0.2562 0.029 Uiso 1 1 calc R . .
C19 C 0.2601(6) 0.2945(6) 0.3876(5) 0.0267(18) Uani 1 1 d . . .
C20 C 0.3467(6) 0.1869(6) 0.4322(5) 0.0272(18) Uani 1 1 d . . .
C21 C 0.1933(6) 0.3540(6) 0.4384(5) 0.0263(18) Uani 1 1 d . . .
C22 C 0.1250(7) 0.4613(7) 0.3887(5) 0.035(2) Uani 1 1 d . . .
H22 H 0.0810 0.5008 0.4215 0.042 Uiso 1 1 calc R . .
C23 C 0.1207(6) 0.5119(6) 0.2902(5) 0.0288(18) Uani 1 1 d . . .
H23 H 0.0759 0.5850 0.2586 0.035 Uiso 1 1 calc R . .
C24 C 0.1836(6) 0.3034(6) 0.5432(5) 0.0273(18) Uani 1 1 d . . .
C25 C 0.1621(7) 0.1905(6) 0.5902(5) 0.0286(18) Uani 1 1 d . . .
H25 H 0.1640 0.1391 0.5586 0.034 Uiso 1 1 calc R . .
C26 C 0.1376(7) 0.1520(6) 0.6840(5) 0.0300(19) Uani 1 1 d . . .
H26 H 0.1230 0.0752 0.7149 0.036 Uiso 1 1 calc R . .
C27 C 0.1349(6) 0.2289(6) 0.7329(5) 0.0235(17) Uani 1 1 d . . .
C28 C 0.1002(6) 0.1909(7) 0.8339(5) 0.0266(18) Uani 1 1 d . . .
C29 C 0.1604(7) 0.3415(6) 0.6863(5) 0.037(2) Uani 1 1 d . . .
H29 H 0.1620 0.3918 0.7185 0.044 Uiso 1 1 calc R . .
C30 C 0.1835(7) 0.3793(7) 0.5929(5) 0.035(2) Uani 1 1 d . . .
H30 H 0.1992 0.4557 0.5621 0.042 Uiso 1 1 calc R . .
C31 C 0.4212(8) 0.5971(9) 0.1483(7) 0.056(3) Uani 1 1 d . . .
H31 H 0.3701 0.5889 0.1955 0.068 Uiso 1 1 calc R . .
C32 C 0.5295(11) 0.5414(12) 0.1725(9) 0.090(4) Uani 1 1 d . . .
H32 H 0.5513 0.4960 0.2349 0.108 Uiso 1 1 calc R . .
C33 C 0.6059(11) 0.5527(13) 0.1040(11) 0.104(5) Uani 1 1 d . . .
H33 H 0.6806 0.5164 0.1191 0.124 Uiso 1 1 calc R . .
C34 C 0.5708(11) 0.6171(13) 0.0150(11) 0.103(5) Uani 1 1 d . . .
H34 H 0.6215 0.6253 -0.0325 0.124 Uiso 1 1 calc R . .
C35 C 0.4596(9) 0.6718(10) -0.0073(7) 0.069(3) Uani 1 1 d . . .
H35 H 0.4364 0.7153 -0.0698 0.082 Uiso 1 1 calc R . .
C36 C 0.4451(9) 0.1468(9) 0.7145(6) 0.062(3) Uani 1 1 d . . .
H36 H 0.3988 0.1990 0.6635 0.074 Uiso 1 1 calc R . .
C37 C 0.4411(10) 0.1683(9) 0.7947(7) 0.077(4) Uani 1 1 d . . .
H37 H 0.3905 0.2309 0.7996 0.092 Uiso 1 1 calc R . .
C38 C 0.5143(10) 0.0947(10) 0.8692(6) 0.065(3) Uani 1 1 d . . .
H38 H 0.5182 0.1112 0.9231 0.078 Uiso 1 1 calc R . .
C39 C 0.5798(9) -0.0014(10) 0.8627(7) 0.066(3) Uani 1 1 d . . .
H39 H 0.6251 -0.0559 0.9134 0.079 Uiso 1 1 calc R . .
C40 C 0.5773(8) -0.0159(9) 0.7772(6) 0.056(3) Uani 1 1 d . . .
H40 H 0.6250 -0.0798 0.7714 0.067 Uiso 1 1 calc R . .
O17 O 0.492(3) 0.431(3) 0.458(2) 0.496(19) Uiso 1 1 d . . .
H7W H 0.5159 0.3794 0.5211 0.595 Uiso 1 1 d R . .
H8W H 0.4661 0.5123 0.4214 0.595 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
Co1 O16 2.028(5) 2_566 ?
Co1 O9 2.056(5) . ?
Co1 O7 2.071(5) . ?
Co1 O2 2.136(5) . ?
Co1 O11 2.144(5) . ?
Co1 O8 2.169(5) . ?
Co1 H2W 1.7203 . ?
Co2 O5 2.046(5) 1_556 ?
Co2 O7 2.090(5) . ?
Co2 O1 2.091(5) . ?
Co2 N1 2.110(7) . ?
Co2 O11 2.133(5) . ?
Co2 O10 2.182(5) . ?
Co3 O7 1.964(5) 2_575 ?
Co3 O7 1.964(5) . ?
Co3 O15 2.153(5) 1_564 ?
Co3 O15 2.153(5) 2_566 ?
Co3 O6 2.224(6) 2_574 ?
Co3 O6 2.224(6) 1_556 ?
Co4 O4 2.002(6) 2_665 ?
Co4 O3 2.024(6) 1_546 ?
Co4 O14 2.026(5) 2_656 ?
Co4 O13 2.035(5) . ?
Co4 N2 2.074(6) . ?
Co4 Co4 2.8126(19) 2_656 ?
N1 C31 1.333(10) . ?
N1 C35 1.343(11) . ?
N2 C40 1.312(10) . ?
N2 C36 1.332(10) . ?
O1 C1 1.246(9) . ?
O2 C1 1.273(9) . ?
O3 C5 1.270(9) . ?
O3 Co4 2.024(6) 1_564 ?
O4 C5 1.245(9) . ?
O4 Co4 2.002(6) 2_665 ?
O5 C13 1.257(9) . ?
O5 Co2 2.045(5) 1_554 ?
O6 C13 1.280(8) . ?
O6 Co3 2.224(6) 1_554 ?
O7 H1 0.8435 . ?
O8 H1W 0.8200 . ?
O8 H2W 0.8503 . ?
O9 H3W 0.8200 . ?
O9 H4W 0.7608 . ?
O10 H5W 0.8200 . ?
O10 H6W 0.7353 . ?
O11 C16 1.279(8) . ?
O12 C16 1.227(8) . ?
O13 C20 1.249(8) . ?
O14 C20 1.269(8) . ?
O14 Co4 2.026(5) 2_656 ?
O15 C28 1.252(8) . ?
O15 Co3 2.153(5) 1_546 ?
O16 C28 1.258(8) . ?
O16 Co1 2.028(5) 2_566 ?
C1 C2 1.495(10) . ?
C2 C8 1.379(11) . ?
C2 C3 1.382(10) . ?
C3 C4 1.407(10) . ?
C3 H3 0.9300 . ?
C4 C6 1.375(11) . ?
C4 C5 1.487(11) . ?
C6 C7 1.401(11) . ?
C6 C9 1.483(10) . ?
C7 C8 1.396(10) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9300 . ?
C9 C10 1.333(12) . ?
C9 C15 1.436(11) . ?
C10 C11 1.390(11) . ?
C10 H10A 0.9300 . ?
C11 C12 1.370(10) . ?
C11 H11 0.9300 . ?
C12 C14 1.399(11) . ?
C12 C13 1.480(10) . ?
C14 C15 1.359(10) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.492(9) . ?
C17 C18 1.386(9) . ?
C17 C23 1.390(9) . ?
C18 C19 1.397(9) . ?
C18 H18 0.9300 . ?
C19 C21 1.419(9) . ?
C19 C20 1.490(9) . ?
C21 C22 1.388(10) . ?
C21 C24 1.506(9) . ?
C22 C23 1.405(9) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.370(10) . ?
C24 C30 1.414(10) . ?
C25 C26 1.382(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.411(10) . ?
C26 H26 0.9300 . ?
C27 C29 1.383(10) . ?
C27 C28 1.518(9) . ?
C29 C30 1.373(10) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.362(14) . ?
C31 H31 0.9300 . ?
C32 C33 1.369(16) . ?
C32 H32 0.9300 . ?
C33 C34 1.336(17) . ?
C33 H33 0.9300 . ?
C34 C35 1.387(16) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.355(12) . ?
C36 H36 0.9300 . ?
C37 C38 1.385(13) . ?
C37 H37 0.9300 . ?
C38 C39 1.349(13) . ?
C38 H38 0.9300 . ?
C39 C40 1.394(12) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
O17 H8W 0.9550 . ?
O17 H7W 0.9537 . ?
O17 H8W 0.9550 . ?

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
O16 Co1 O9 89.0(2) 2_566 . ?
O16 Co1 O7 92.1(2) 2_566 . ?
O9 Co1 O7 178.0(2) . . ?
O16 Co1 O2 175.85(19) 2_566 . ?
O9 Co1 O2 94.32(19) . . ?
O7 Co1 O2 84.65(19) . . ?
O16 Co1 O11 91.2(2) 2_566 . ?
O9 Co1 O11 93.92(19) . . ?
O7 Co1 O11 84.44(19) . . ?
O2 Co1 O11 91.04(19) . . ?
O16 Co1 O8 94.2(2) 2_566 . ?
O9 Co1 O8 86.3(2) . . ?
O7 Co1 O8 95.2(2) . . ?
O2 Co1 O8 83.6(2) . . ?
O11 Co1 O8 174.64(19) . . ?
O16 Co1 H2W 115.7 2_566 . ?
O9 Co1 H2W 88.3 . . ?
O7 Co1 H2W 92.7 . . ?
O2 Co1 H2W 62.1 . . ?
O11 Co1 H2W 153.1 . . ?
O8 Co1 H2W 21.6 . . ?
O5 Co2 O7 91.9(2) 1_556 . ?
O5 Co2 O1 176.1(2) 1_556 . ?
O7 Co2 O1 84.2(2) . . ?
O5 Co2 N1 91.1(2) 1_556 . ?
O7 Co2 N1 176.7(2) . . ?
O1 Co2 N1 92.8(2) . . ?
O5 Co2 O11 88.3(2) 1_556 . ?
O7 Co2 O11 84.26(18) . . ?
O1 Co2 O11 91.8(2) . . ?
N1 Co2 O11 97.1(2) . . ?
O5 Co2 O10 92.0(2) 1_556 . ?
O7 Co2 O10 90.2(2) . . ?
O1 Co2 O10 87.5(2) . . ?
N1 Co2 O10 88.4(2) . . ?
O11 Co2 O10 174.5(2) . . ?
O7 Co3 O7 179.998(1) 2_575 . ?
O7 Co3 O15 93.59(19) 2_575 1_564 ?
O7 Co3 O15 86.41(19) . 1_564 ?
O7 Co3 O15 86.41(19) 2_575 2_566 ?
O7 Co3 O15 93.59(19) . 2_566 ?
O15 Co3 O15 179.999(1) 1_564 2_566 ?
O7 Co3 O6 94.14(19) 2_575 2_574 ?
O7 Co3 O6 85.86(19) . 2_574 ?
O15 Co3 O6 86.0(2) 1_564 2_574 ?
O15 Co3 O6 94.0(2) 2_566 2_574 ?
O7 Co3 O6 85.86(19) 2_575 1_556 ?
O7 Co3 O6 94.14(19) . 1_556 ?
O15 Co3 O6 94.0(2) 1_564 1_556 ?
O15 Co3 O6 86.0(2) 2_566 1_556 ?
O6 Co3 O6 180.0(3) 2_574 1_556 ?
O4 Co4 O3 163.3(2) 2_665 1_546 ?
O4 Co4 O14 88.3(3) 2_665 2_656 ?
O3 Co4 O14 90.5(3) 1_546 2_656 ?
O4 Co4 O13 88.7(2) 2_665 . ?
O3 Co4 O13 87.8(3) 1_546 . ?
O14 Co4 O13 163.5(2) 2_656 . ?
O4 Co4 N2 102.1(3) 2_665 . ?
O3 Co4 N2 94.5(2) 1_546 . ?
O14 Co4 N2 99.9(2) 2_656 . ?
O13 Co4 N2 96.6(2) . . ?
O4 Co4 Co4 85.47(17) 2_665 2_656 ?
O3 Co4 Co4 77.91(17) 1_546 2_656 ?
O14 Co4 Co4 80.64(16) 2_656 2_656 ?
O13 Co4 Co4 82.96(15) . 2_656 ?
N2 Co4 Co4 172.5(2) . 2_656 ?
C31 N1 C35 117.6(8) . . ?
C31 N1 Co2 122.0(6) . . ?
C35 N1 Co2 120.3(6) . . ?
C40 N2 C36 116.8(7) . . ?
C40 N2 Co4 121.7(6) . . ?
C36 N2 Co4 121.5(6) . . ?
C1 O1 Co2 129.0(5) . . ?
C1 O2 Co1 126.4(5) . . ?
C5 O3 Co4 129.6(5) . 1_564 ?
C5 O4 Co4 121.6(6) . 2_665 ?
C13 O5 Co2 132.1(5) . 1_554 ?
C13 O6 Co3 122.1(5) . 1_554 ?
Co3 O7 Co1 126.9(3) . . ?
Co3 O7 Co2 123.6(2) . . ?
Co1 O7 Co2 95.87(18) . . ?
Co3 O7 H1 100.3 . . ?
Co1 O7 H1 100.7 . . ?
Co2 O7 H1 106.1 . . ?
Co1 O8 H1W 109.4 . . ?
Co1 O8 H2W 48.0 . . ?
H1W O8 H2W 110.0 . . ?
Co1 O9 H3W 109.5 . . ?
Co1 O9 H4W 123.4 . . ?
H3W O9 H4W 106.5 . . ?
Co2 O10 H5W 109.6 . . ?
Co2 O10 H6W 86.4 . . ?
H5W O10 H6W 55.4 . . ?
C16 O11 Co2 130.3(5) . . ?
C16 O11 Co1 133.7(5) . . ?
Co2 O11 Co1 92.50(17) . . ?
C20 O13 Co4 124.2(5) . . ?
C20 O14 Co4 127.1(5) . 2_656 ?
C28 O15 Co3 131.9(4) . 1_546 ?
C28 O16 Co1 136.6(5) . 2_566 ?
O1 C1 O2 125.8(7) . . ?
O1 C1 C2 117.3(7) . . ?
O2 C1 C2 116.9(7) . . ?
C8 C2 C3 117.5(7) . . ?
C8 C2 C1 122.5(7) . . ?
C3 C2 C1 120.0(7) . . ?
C2 C3 C4 122.8(7) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C6 C4 C3 118.9(7) . . ?
C6 C4 C5 124.4(7) . . ?
C3 C4 C5 116.7(7) . . ?
O4 C5 O3 125.0(8) . . ?
O4 C5 C4 119.0(8) . . ?
O3 C5 C4 115.9(7) . . ?
C4 C6 C7 119.0(7) . . ?
C4 C6 C9 123.8(7) . . ?
C7 C6 C9 117.0(8) . . ?
C8 C7 C6 120.7(8) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C2 C8 C7 121.0(8) . . ?
C2 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
C10 C9 C15 116.6(7) . . ?
C10 C9 C6 121.7(8) . . ?
C15 C9 C6 121.6(7) . . ?
C9 C10 C11 122.7(8) . . ?
C9 C10 H10A 118.7 . . ?
C11 C10 H10A 118.7 . . ?
C12 C11 C10 121.2(8) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C14 117.4(7) . . ?
C11 C12 C13 120.4(7) . . ?
C14 C12 C13 122.2(7) . . ?
O5 C13 O6 123.0(7) . . ?
O5 C13 C12 117.1(6) . . ?
O6 C13 C12 119.9(7) . . ?
C15 C14 C12 121.0(8) . . ?
C15 C14 H14 119.5 . . ?
C12 C14 H14 119.5 . . ?
C14 C15 C9 121.0(8) . . ?
C14 C15 H15 119.5 . . ?
C9 C15 H15 119.5 . . ?
O12 C16 O11 124.5(7) . . ?
O12 C16 C17 118.6(6) . . ?
O11 C16 C17 116.8(6) . . ?
C18 C17 C23 118.6(6) . . ?
C18 C17 C16 119.8(6) . . ?
C23 C17 C16 121.6(6) . . ?
C17 C18 C19 122.8(7) . . ?
C17 C18 H18 118.6 . . ?
C19 C18 H18 118.6 . . ?
C18 C19 C21 118.5(6) . . ?
C18 C19 C20 117.6(6) . . ?
C21 C19 C20 123.8(6) . . ?
O13 C20 O14 125.1(7) . . ?
O13 C20 C19 119.1(7) . . ?
O14 C20 C19 115.8(6) . . ?
C22 C21 C19 118.6(6) . . ?
C22 C21 C24 116.9(6) . . ?
C19 C21 C24 124.2(6) . . ?
C21 C22 C23 121.7(7) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C17 C23 C22 119.8(7) . . ?
C17 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C25 C24 C30 118.8(7) . . ?
C25 C24 C21 122.1(7) . . ?
C30 C24 C21 118.7(7) . . ?
C24 C25 C26 120.9(7) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C27 120.1(7) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C29 C27 C26 119.0(6) . . ?
C29 C27 C28 120.3(7) . . ?
C26 C27 C28 120.7(7) . . ?
O15 C28 O16 126.8(7) . . ?
O15 C28 C27 119.5(6) . . ?
O16 C28 C27 113.7(7) . . ?
C30 C29 C27 120.4(7) . . ?
C30 C29 H29 119.8 . . ?
C27 C29 H29 119.8 . . ?
C29 C30 C24 120.7(7) . . ?
C29 C30 H30 119.6 . . ?
C24 C30 H30 119.6 . . ?
N1 C31 C32 122.9(10) . . ?
N1 C31 H31 118.5 . . ?
C32 C31 H31 118.5 . . ?
C31 C32 C33 119.4(11) . . ?
C31 C32 H32 120.3 . . ?
C33 C32 H32 120.3 . . ?
C34 C33 C32 118.5(11) . . ?
C34 C33 H33 120.8 . . ?
C32 C33 H33 120.8 . . ?
C33 C34 C35 120.7(12) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
N1 C35 C34 120.9(10) . . ?
N1 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
N2 C36 C37 123.7(9) . . ?
N2 C36 H36 118.1 . . ?
C37 C36 H36 118.1 . . ?
C36 C37 C38 118.4(9) . . ?
C36 C37 H37 120.8 . . ?
C38 C37 H37 120.8 . . ?
C39 C38 C37 119.3(9) . . ?
C39 C38 H38 120.4 . . ?
C37 C38 H38 120.4 . . ?
C38 C39 C40 117.7(9) . . ?
C38 C39 H39 121.2 . . ?
C40 C39 H39 121.2 . . ?
N2 C40 C39 123.9(8) . . ?
N2 C40 H40 118.1 . . ?
C39 C40 H40 118.1 . . ?
H8W O17 H7W 140.6 . . ?
H8W O17 H8W 0.0 . . ?
H7W O17 H8W 140.6 . . ?

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
O5 Co2 N1 C31 33.5(7) 1_556 . . . ?
O7 Co2 N1 C31 -169(4) . . . . ?
O1 Co2 N1 C31 -147.1(7) . . . . ?
O11 Co2 N1 C31 -54.9(7) . . . . ?
O10 Co2 N1 C31 125.5(7) . . . . ?
O5 Co2 N1 C35 -143.8(8) 1_556 . . . ?
O7 Co2 N1 C35 14(4) . . . . ?
O1 Co2 N1 C35 35.5(8) . . . . ?
O11 Co2 N1 C35 127.7(7) . . . . ?
O10 Co2 N1 C35 -51.9(8) . . . . ?
O4 Co4 N2 C40 -90.1(7) 2_665 . . . ?
O3 Co4 N2 C40 91.5(8) 1_546 . . . ?
O14 Co4 N2 C40 0.2(8) 2_656 . . . ?
O13 Co4 N2 C40 179.8(7) . . . . ?
Co4 Co4 N2 C40 93.6(16) 2_656 . . . ?
O4 Co4 N2 C36 89.4(8) 2_665 . . . ?
O3 Co4 N2 C36 -89.0(8) 1_546 . . . ?
O14 Co4 N2 C36 179.7(8) 2_656 . . . ?
O13 Co4 N2 C36 -0.7(8) . . . . ?
Co4 Co4 N2 C36 -86.9(16) 2_656 . . . ?
O5 Co2 O1 C1 -43(3) 1_556 . . . ?
O7 Co2 O1 C1 -34.6(6) . . . . ?
N1 Co2 O1 C1 146.6(7) . . . . ?
O11 Co2 O1 C1 49.4(7) . . . . ?
O10 Co2 O1 C1 -125.1(7) . . . . ?
O16 Co1 O2 C1 71(3) 2_566 . . . ?
O9 Co1 O2 C1 -145.0(6) . . . . ?
O7 Co1 O2 C1 33.3(6) . . . . ?
O11 Co1 O2 C1 -51.0(6) . . . . ?
O8 Co1 O2 C1 129.2(6) . . . . ?
O7 Co3 O7 Co1 25(6) 2_575 . . . ?
O15 Co3 O7 Co1 -151.1(3) 1_564 . . . ?
O15 Co3 O7 Co1 28.9(3) 2_566 . . . ?
O6 Co3 O7 Co1 -64.9(3) 2_574 . . . ?
O6 Co3 O7 Co1 115.1(3) 1_556 . . . ?
O7 Co3 O7 Co2 -106(6) 2_575 . . . ?
O15 Co3 O7 Co2 78.2(3) 1_564 . . . ?
O15 Co3 O7 Co2 -101.8(3) 2_566 . . . ?
O6 Co3 O7 Co2 164.4(3) 2_574 . . . ?
O6 Co3 O7 Co2 -15.6(3) 1_556 . . . ?
O16 Co1 O7 Co3 -36.5(3) 2_566 . . . ?
O9 Co1 O7 Co3 -161(5) . . . . ?
O2 Co1 O7 Co3 140.9(3) . . . . ?
O11 Co1 O7 Co3 -127.5(3) . . . . ?
O8 Co1 O7 Co3 57.9(3) . . . . ?
O16 Co1 O7 Co2 104.1(2) 2_566 . . . ?
O9 Co1 O7 Co2 -20(6) . . . . ?
O2 Co1 O7 Co2 -78.5(2) . . . . ?
O11 Co1 O7 Co2 13.08(18) . . . . ?
O8 Co1 O7 Co2 -161.5(2) . . . . ?
O5 Co2 O7 Co3 41.2(3) 1_556 . . . ?
O1 Co2 O7 Co3 -138.2(3) . . . . ?
N1 Co2 O7 Co3 -116(4) . . . . ?
O11 Co2 O7 Co3 129.3(3) . . . . ?
O10 Co2 O7 Co3 -50.8(3) . . . . ?
O5 Co2 O7 Co1 -101.3(2) 1_556 . . . ?
O1 Co2 O7 Co1 79.3(2) . . . . ?
N1 Co2 O7 Co1 101(4) . . . . ?
O11 Co2 O7 Co1 -13.15(19) . . . . ?
O10 Co2 O7 Co1 166.7(2) . . . . ?
O5 Co2 O11 C16 -94.6(6) 1_556 . . . ?
O7 Co2 O11 C16 173.4(6) . . . . ?
O1 Co2 O11 C16 89.4(6) . . . . ?
N1 Co2 O11 C16 -3.7(6) . . . . ?
O10 Co2 O11 C16 172(2) . . . . ?
O5 Co2 O11 Co1 104.7(2) 1_556 . . . ?
O7 Co2 O11 Co1 12.64(18) . . . . ?
O1 Co2 O11 Co1 -71.3(2) . . . . ?
N1 Co2 O11 Co1 -164.4(2) . . . . ?
O10 Co2 O11 Co1 11(2) . . . . ?
O16 Co1 O11 C16 95.7(6) 2_566 . . . ?
O9 Co1 O11 C16 6.5(6) . . . . ?
O7 Co1 O11 C16 -172.4(6) . . . . ?
O2 Co1 O11 C16 -87.9(6) . . . . ?
O8 Co1 O11 C16 -86(2) . . . . ?
O16 Co1 O11 Co2 -104.7(2) 2_566 . . . ?
O9 Co1 O11 Co2 166.16(18) . . . . ?
O7 Co1 O11 Co2 -12.76(18) . . . . ?
O2 Co1 O11 Co2 71.76(19) . . . . ?
O8 Co1 O11 Co2 74(2) . . . . ?
O4 Co4 O13 C20 88.3(6) 2_665 . . . ?
O3 Co4 O13 C20 -75.3(6) 1_546 . . . ?
O14 Co4 O13 C20 8.8(13) 2_656 . . . ?
N2 Co4 O13 C20 -169.7(6) . . . . ?
Co4 Co4 O13 C20 2.7(6) 2_656 . . . ?
Co2 O1 C1 O2 -17.4(11) . . . . ?
Co2 O1 C1 C2 161.1(5) . . . . ?
Co1 O2 C1 O1 18.2(11) . . . . ?
Co1 O2 C1 C2 -160.3(5) . . . . ?
O1 C1 C2 C8 172.3(8) . . . . ?
O2 C1 C2 C8 -9.0(12) . . . . ?
O1 C1 C2 C3 -10.3(11) . . . . ?
O2 C1 C2 C3 168.3(7) . . . . ?
C8 C2 C3 C4 -0.2(12) . . . . ?
C1 C2 C3 C4 -177.7(7) . . . . ?
C2 C3 C4 C6 0.2(12) . . . . ?
C2 C3 C4 C5 -179.0(7) . . . . ?
Co4 O4 C5 O3 -7.8(11) 2_665 . . . ?
Co4 O4 C5 C4 170.1(5) 2_665 . . . ?
Co4 O3 C5 O4 6.1(13) 1_564 . . . ?
Co4 O3 C5 C4 -171.9(5) 1_564 . . . ?
C6 C4 C5 O4 -17.2(12) . . . . ?
C3 C4 C5 O4 161.9(7) . . . . ?
C6 C4 C5 O3 160.9(8) . . . . ?
C3 C4 C5 O3 -20.0(10) . . . . ?
C3 C4 C6 C7 -0.2(13) . . . . ?
C5 C4 C6 C7 178.9(8) . . . . ?
C3 C4 C6 C9 -176.9(7) . . . . ?
C5 C4 C6 C9 2.2(13) . . . . ?
C4 C6 C7 C8 0.2(14) . . . . ?
C9 C6 C7 C8 177.2(8) . . . . ?
C3 C2 C8 C7 0.3(14) . . . . ?
C1 C2 C8 C7 177.6(8) . . . . ?
C6 C7 C8 C2 -0.3(15) . . . . ?
C4 C6 C9 C10 98.4(12) . . . . ?
C7 C6 C9 C10 -78.4(12) . . . . ?
C4 C6 C9 C15 -86.5(12) . . . . ?
C7 C6 C9 C15 96.7(11) . . . . ?
C15 C9 C10 C11 4.1(16) . . . . ?
C6 C9 C10 C11 179.3(10) . . . . ?
C9 C10 C11 C12 -2.5(18) . . . . ?
C10 C11 C12 C14 -0.6(16) . . . . ?
C10 C11 C12 C13 -177.8(9) . . . . ?
Co2 O5 C13 O6 -5.9(12) 1_554 . . . ?
Co2 O5 C13 C12 172.0(5) 1_554 . . . ?
Co3 O6 C13 O5 56.0(10) 1_554 . . . ?
Co3 O6 C13 C12 -121.9(7) 1_554 . . . ?
C11 C12 C13 O5 0.8(12) . . . . ?
C14 C12 C13 O5 -176.2(8) . . . . ?
C11 C12 C13 O6 178.8(9) . . . . ?
C14 C12 C13 O6 1.8(13) . . . . ?
C11 C12 C14 C15 1.8(15) . . . . ?
C13 C12 C14 C15 178.9(9) . . . . ?
C12 C14 C15 C9 0.0(16) . . . . ?
C10 C9 C15 C14 -2.8(15) . . . . ?
C6 C9 C15 C14 -178.1(9) . . . . ?
Co2 O11 C16 O12 -82.0(10) . . . . ?
Co1 O11 C16 O12 70.8(10) . . . . ?
Co2 O11 C16 C17 100.4(7) . . . . ?
Co1 O11 C16 C17 -106.8(7) . . . . ?
O12 C16 C17 C18 18.6(11) . . . . ?
O11 C16 C17 C18 -163.7(7) . . . . ?
O12 C16 C17 C23 -157.9(8) . . . . ?
O11 C16 C17 C23 19.9(11) . . . . ?
C23 C17 C18 C19 -1.8(12) . . . . ?
C16 C17 C18 C19 -178.4(7) . . . . ?
C17 C18 C19 C21 3.6(12) . . . . ?
C17 C18 C19 C20 -171.7(7) . . . . ?
Co4 O13 C20 O14 -2.5(12) . . . . ?
Co4 O13 C20 C19 -179.9(5) . . . . ?
Co4 O14 C20 O13 -0.2(12) 2_656 . . . ?
Co4 O14 C20 C19 177.3(5) 2_656 . . . ?
C18 C19 C20 O13 149.4(8) . . . . ?
C21 C19 C20 O13 -25.6(12) . . . . ?
C18 C19 C20 O14 -28.2(11) . . . . ?
C21 C19 C20 O14 156.8(8) . . . . ?
C18 C19 C21 C22 -2.6(12) . . . . ?
C20 C19 C21 C22 172.4(8) . . . . ?
C18 C19 C21 C24 171.8(8) . . . . ?
C20 C19 C21 C24 -13.2(13) . . . . ?
C19 C21 C22 C23 0.0(13) . . . . ?
C24 C21 C22 C23 -174.9(8) . . . . ?
C18 C17 C23 C22 -0.9(12) . . . . ?
C16 C17 C23 C22 175.5(8) . . . . ?
C21 C22 C23 C17 1.9(13) . . . . ?
C22 C21 C24 C25 125.8(8) . . . . ?
C19 C21 C24 C25 -48.7(12) . . . . ?
C22 C21 C24 C30 -46.6(11) . . . . ?
C19 C21 C24 C30 138.9(8) . . . . ?
C30 C24 C25 C26 1.7(12) . . . . ?
C21 C24 C25 C26 -170.7(7) . . . . ?
C24 C25 C26 C27 -0.2(12) . . . . ?
C25 C26 C27 C29 -2.0(12) . . . . ?
C25 C26 C27 C28 175.7(7) . . . . ?
Co3 O15 C28 O16 24.8(12) 1_546 . . . ?
Co3 O15 C28 C27 -156.5(5) 1_546 . . . ?
Co1 O16 C28 O15 -8.6(13) 2_566 . . . ?
Co1 O16 C28 C27 172.6(5) 2_566 . . . ?
C29 C27 C28 O15 -169.5(7) . . . . ?
C26 C27 C28 O15 12.7(11) . . . . ?
C29 C27 C28 O16 9.4(10) . . . . ?
C26 C27 C28 O16 -168.3(7) . . . . ?
C26 C27 C29 C30 2.7(12) . . . . ?
C28 C27 C29 C30 -175.0(7) . . . . ?
C27 C29 C30 C24 -1.2(13) . . . . ?
C25 C24 C30 C29 -1.1(12) . . . . ?
C21 C24 C30 C29 171.6(7) . . . . ?
C35 N1 C31 C32 1.2(16) . . . . ?
Co2 N1 C31 C32 -176.3(9) . . . . ?
N1 C31 C32 C33 0(2) . . . . ?
C31 C32 C33 C34 -1(2) . . . . ?
C32 C33 C34 C35 0(2) . . . . ?
C31 N1 C35 C34 -1.7(16) . . . . ?
Co2 N1 C35 C34 175.8(10) . . . . ?
C33 C34 C35 N1 1(2) . . . . ?
C40 N2 C36 C37 -1.1(17) . . . . ?
Co4 N2 C36 C37 179.4(10) . . . . ?
N2 C36 C37 C38 3.6(19) . . . . ?
C36 C37 C38 C39 -5.7(19) . . . . ?
C37 C38 C39 C40 5.4(18) . . . . ?
C36 N2 C40 C39 0.9(16) . . . . ?
Co4 N2 C40 C39 -179.6(8) . . . . ?
C38 C39 C40 N2 -3.1(18) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H6W O6 0.74 2.44 3.150(8) 161.7 1_556
O10 H5W O15 0.82 1.99 2.800(8) 168.5 1_564
O9 H4W O2 0.76 2.08 2.778(7) 152.3 2_565
O9 H3W O12 0.82 1.81 2.629(7) 173.8 2_565
O8 H2W O2 0.85 2.02 2.869(7) 179.6 .
O8 H1W O6 0.82 1.95 2.743(8) 163.1 2_574

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.124
####################################################################### 
# 
# 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_244-12pb1
_database_code_depnum_ccdc_archive 'CCDC 1430233'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H18 O14 Pb3'
_chemical_formula_weight         1224.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   13.48481(14)
_cell_length_b                   12.16380(14)
_cell_length_c                   17.6457(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1954(10)
_cell_angle_gamma                90.00
_cell_volume                     2882.46(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2224
_exptl_absorpt_coefficient_mu    34.188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0634
_exptl_absorpt_correction_T_max  0.1169
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APE-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11000
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.96
_diffrn_reflns_theta_max         69.71
_reflns_number_total             5347
_reflns_number_gt                4330
_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)+(0.0170P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5347
_refine_ls_number_parameters     432
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0520
_refine_ls_wR_factor_gt          0.0493
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_restrained_S_all      0.965
_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
Pb1 Pb -0.569952(19) 0.65117(2) 0.467857(15) 0.01459(7) Uani 1 1 d . . .
Pb2 Pb 0.513504(19) 0.87570(2) 0.621408(16) 0.01621(7) Uani 1 1 d . . .
Pb3 Pb 0.421143(19) 0.96400(2) 0.891273(15) 0.01559(7) Uani 1 1 d . . .
O1 O -0.4373(3) 0.7530(4) 0.3945(3) 0.0241(12) Uani 1 1 d . . .
O2 O -0.4071(3) 0.7051(4) 0.5148(3) 0.0239(12) Uani 1 1 d . . .
O3 O 0.1282(4) 0.6592(4) 0.6055(3) 0.0270(12) Uani 1 1 d . . .
O4 O 0.0302(4) 0.6036(4) 0.5087(3) 0.0252(12) Uani 1 1 d . . .
O5 O 0.4150(3) 0.8622(4) 0.5007(3) 0.0184(11) Uani 1 1 d . . .
O6 O 0.3698(3) 1.0295(4) 0.4580(3) 0.0217(11) Uani 1 1 d . . .
O7 O 0.3497(4) 0.9230(5) 0.6496(3) 0.0316(14) Uani 1 1 d . . .
O8 O 0.3877(3) 1.0259(4) 0.7537(3) 0.0217(12) Uani 1 1 d . . .
O9 O 0.0888(3) 1.1692(4) 0.8866(3) 0.0209(11) Uani 1 1 d . . .
O10 O 0.0301(4) 1.0150(4) 0.9295(3) 0.0208(11) Uani 1 1 d . . .
O11 O -0.4179(4) 1.0009(5) 0.8621(3) 0.0328(14) Uani 1 1 d . . .
O12 O -0.4496(4) 0.8538(5) 0.7877(3) 0.0345(14) Uani 1 1 d . . .
O13 O 0.5360(4) 1.0674(4) 0.6703(3) 0.0302(13) Uani 1 1 d . . .
H1W H 0.5638 1.0394 0.6335 0.036 Uiso 1 1 d R . .
H2W H 0.4910 1.0829 0.7016 0.036 Uiso 1 1 d R . .
O14 O 0.2533(6) 0.9998(6) 0.0102(4) 0.0524(18) Uani 1 1 d D . .
C1 C -0.3780(5) 0.7423(6) 0.4533(4) 0.0185(16) Uani 1 1 d . . .
C2 C -0.2711(5) 0.7719(6) 0.4512(4) 0.0182(16) Uani 1 1 d . . .
C3 C -0.2309(5) 0.7923(6) 0.3836(4) 0.0218(17) Uani 1 1 d . . .
H3 H -0.2716 0.7914 0.3381 0.026 Uiso 1 1 calc R . .
C4 C -0.1301(5) 0.8140(6) 0.3829(4) 0.0225(17) Uani 1 1 d . . .
H4 H -0.1041 0.8289 0.3369 0.027 Uiso 1 1 calc R . .
C5 C -0.0671(5) 0.8139(6) 0.4498(4) 0.0190(16) Uani 1 1 d . . .
C6 C -0.1087(5) 0.7957(6) 0.5176(4) 0.0219(17) Uani 1 1 d . . .
H6 H -0.0685 0.7979 0.5633 0.026 Uiso 1 1 calc R . .
C7 C -0.2095(5) 0.7742(7) 0.5183(4) 0.0236(17) Uani 1 1 d . . .
H7 H -0.2360 0.7612 0.5643 0.028 Uiso 1 1 calc R . .
C8 C 0.0428(5) 0.8359(6) 0.4508(4) 0.0171(15) Uani 1 1 d . . .
C9 C 0.1128(5) 0.7754(6) 0.4973(4) 0.0134(14) Uani 1 1 d . . .
C10 C 0.0894(5) 0.6746(6) 0.5397(4) 0.0146(15) Uani 1 1 d . . .
C11 C 0.2117(5) 0.8082(6) 0.5044(4) 0.0147(15) Uani 1 1 d . . .
H11 H 0.2574 0.7701 0.5372 0.018 Uiso 1 1 calc R . .
C12 C 0.2437(5) 0.8962(6) 0.4636(4) 0.0150(15) Uani 1 1 d . . .
C13 C 0.3496(5) 0.9328(6) 0.4743(4) 0.0165(15) Uani 1 1 d . . .
C14 C 0.1755(5) 0.9524(6) 0.4140(4) 0.0231(17) Uani 1 1 d . . .
H14 H 0.1968 1.0092 0.3841 0.028 Uiso 1 1 calc R . .
C15 C 0.0753(5) 0.9234(7) 0.4091(4) 0.0271(19) Uani 1 1 d . . .
H15 H 0.0295 0.9632 0.3775 0.033 Uiso 1 1 calc R . .
C16 C 0.3292(5) 0.9704(6) 0.7105(4) 0.0153(15) Uani 1 1 d . . .
C17 C 0.2235(5) 0.9562(6) 0.7311(4) 0.0148(14) Uani 1 1 d . . .
C18 C 0.1888(5) 1.0234(6) 0.7873(3) 0.0148(15) Uani 1 1 d . . .
H18 H 0.2301 1.0765 0.8114 0.018 Uiso 1 1 calc R . .
C19 C 0.0915(5) 1.0097(6) 0.8067(3) 0.0119(14) Uani 1 1 d . . .
C20 C 0.0660(5) 1.0700(6) 0.8765(4) 0.0143(14) Uani 1 1 d . . .
C21 C 0.0260(5) 0.9349(6) 0.7676(4) 0.0147(15) Uani 1 1 d . . .
C22 C 0.0655(5) 0.8676(6) 0.7150(4) 0.0208(16) Uani 1 1 d . . .
H22 H 0.0249 0.8141 0.6908 0.025 Uiso 1 1 calc R . .
C23 C 0.1622(5) 0.8762(6) 0.6970(4) 0.0233(17) Uani 1 1 d . . .
H23 H 0.1862 0.8282 0.6619 0.028 Uiso 1 1 calc R . .
C24 C -0.0815(5) 0.9307(6) 0.7796(4) 0.0169(15) Uani 1 1 d . . .
C25 C -0.1343(5) 0.8315(6) 0.7754(4) 0.0220(17) Uani 1 1 d . . .
H25 H -0.1017 0.7664 0.7657 0.026 Uiso 1 1 calc R . .
C26 C -0.2351(5) 0.8297(6) 0.7856(4) 0.0255(18) Uani 1 1 d . . .
H26 H -0.2698 0.7635 0.7828 0.031 Uiso 1 1 calc R . .
C27 C -0.2841(5) 0.9265(7) 0.8000(4) 0.0200(16) Uani 1 1 d . . .
C28 C -0.3919(5) 0.9257(7) 0.8177(4) 0.0251(18) Uani 1 1 d . . .
C29 C -0.2328(5) 1.0262(6) 0.8015(4) 0.0238(17) Uani 1 1 d . . .
H29 H -0.2656 1.0916 0.8103 0.029 Uiso 1 1 calc R . .
C30 C -0.1335(5) 1.0268(6) 0.7900(4) 0.0211(16) Uani 1 1 d . . .
H30 H -0.1002 1.0937 0.7891 0.025 Uiso 1 1 calc R . .
H3W H 0.213(5) 0.947(6) 0.020(5) 0.06(4) Uiso 1 1 d D . .
H4W H 0.307(3) 1.007(7) 0.040(4) 0.04(3) Uiso 1 1 d 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
Pb1 O2 2.369(5) . ?
Pb1 O10 2.477(5) 2_446 ?
Pb1 O10 2.555(5) 4_575 ?
Pb1 O1 2.614(5) . ?
Pb1 O9 2.613(5) 2_446 ?
Pb1 O5 2.643(5) 1_455 ?
Pb2 O7 2.379(5) . ?
Pb2 O5 2.412(5) . ?
Pb2 O6 2.484(5) 3_676 ?
Pb2 O13 2.495(5) . ?
Pb2 H1W 2.1076 . ?
Pb3 O11 2.319(5) 1_655 ?
Pb3 O3 2.468(5) 2_556 ?
Pb3 O4 2.493(5) 2_556 ?
Pb3 O8 2.543(5) . ?
Pb3 O4 2.566(5) 4_676 ?
Pb3 C10 2.845(7) 2_556 ?
O1 C1 1.259(8) . ?
O2 C1 1.270(8) . ?
O3 C10 1.243(8) . ?
O3 Pb3 2.468(5) 2_546 ?
O4 C10 1.266(8) . ?
O4 Pb3 2.493(5) 2_546 ?
O4 Pb3 2.566(5) 4_575 ?
O5 C13 1.288(8) . ?
O5 Pb1 2.643(5) 1_655 ?
O6 C13 1.246(8) . ?
O6 Pb2 2.484(5) 3_676 ?
O7 C16 1.271(8) . ?
O8 C16 1.245(8) . ?
O9 C20 1.254(8) . ?
O9 Pb1 2.613(5) 2_456 ?
O10 C20 1.279(8) . ?
O10 Pb1 2.477(5) 2_456 ?
O10 Pb1 2.555(5) 4_676 ?
O11 C28 1.275(9) . ?
O11 Pb3 2.319(5) 1_455 ?
O12 C28 1.255(9) . ?
O13 H1W 0.8502 . ?
O13 H2W 0.8765 . ?
O14 H3W 0.865(10) . ?
O14 H4W 0.863(10) . ?
C1 C2 1.490(9) . ?
C2 C3 1.377(10) . ?
C2 C7 1.384(9) . ?
C3 C4 1.386(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(10) . ?
C5 C8 1.504(9) . ?
C6 C7 1.384(9) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C15 1.387(10) . ?
C8 C9 1.403(9) . ?
C9 C11 1.387(9) . ?
C9 C10 1.485(9) . ?
C10 Pb3 2.845(7) 2_546 ?
C11 C12 1.380(9) . ?
C11 H11 0.9300 . ?
C12 C14 1.391(9) . ?
C12 C13 1.492(9) . ?
C14 C15 1.391(9) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.512(9) . ?
C17 C23 1.380(10) . ?
C17 C18 1.398(9) . ?
C18 C19 1.397(9) . ?
C18 H18 0.9300 . ?
C19 C21 1.404(9) . ?
C19 C20 1.501(8) . ?
C21 C22 1.380(9) . ?
C21 C24 1.485(9) . ?
C22 C23 1.374(9) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C30 1.384(10) . ?
C24 C25 1.399(10) . ?
C25 C26 1.387(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.385(11) . ?
C26 H26 0.9300 . ?
C27 C29 1.394(10) . ?
C27 C28 1.514(9) . ?
C29 C30 1.373(9) . ?
C29 H29 0.9300 . ?
C30 H30 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
O2 Pb1 O10 78.24(17) . 2_446 ?
O2 Pb1 O10 79.45(17) . 4_575 ?
O10 Pb1 O10 65.16(17) 2_446 4_575 ?
O2 Pb1 O1 52.24(16) . . ?
O10 Pb1 O1 124.47(15) 2_446 . ?
O10 Pb1 O1 80.91(16) 4_575 . ?
O2 Pb1 O9 78.60(16) . 2_446 ?
O10 Pb1 O9 51.04(15) 2_446 2_446 ?
O10 Pb1 O9 115.29(15) 4_575 2_446 ?
O1 Pb1 O9 125.39(15) . 2_446 ?
O2 Pb1 O5 75.01(16) . 1_455 ?
O10 Pb1 O5 120.33(15) 2_446 1_455 ?
O10 Pb1 O5 151.53(15) 4_575 1_455 ?
O1 Pb1 O5 73.62(15) . 1_455 ?
O9 Pb1 O5 71.77(15) 2_446 1_455 ?
O7 Pb2 O5 75.77(17) . . ?
O7 Pb2 O6 130.81(18) . 3_676 ?
O5 Pb2 O6 81.92(16) . 3_676 ?
O7 Pb2 O13 77.74(18) . . ?
O5 Pb2 O13 114.16(17) . . ?
O6 Pb2 O13 72.41(16) 3_676 . ?
O7 Pb2 H1W 92.7 . . ?
O5 Pb2 H1W 107.5 . . ?
O6 Pb2 H1W 53.4 3_676 . ?
O13 Pb2 H1W 19.0 . . ?
O11 Pb3 O3 94.5(2) 1_655 2_556 ?
O11 Pb3 O4 80.44(18) 1_655 2_556 ?
O3 Pb3 O4 51.88(15) 2_556 2_556 ?
O11 Pb3 O8 79.58(16) 1_655 . ?
O3 Pb3 O8 73.30(16) 2_556 . ?
O4 Pb3 O8 119.13(17) 2_556 . ?
O11 Pb3 O4 76.21(18) 1_655 4_676 ?
O3 Pb3 O4 115.19(16) 2_556 4_676 ?
O4 Pb3 O4 63.36(19) 2_556 4_676 ?
O8 Pb3 O4 154.83(16) . 4_676 ?
O11 Pb3 C10 90.3(2) 1_655 2_556 ?
O3 Pb3 C10 25.84(16) 2_556 2_556 ?
O4 Pb3 C10 26.39(16) 2_556 2_556 ?
O8 Pb3 C10 97.52(18) . 2_556 ?
O4 Pb3 C10 89.41(18) 4_676 2_556 ?
C1 O1 Pb1 87.4(4) . . ?
C1 O2 Pb1 98.5(4) . . ?
C10 O3 Pb3 94.3(4) . 2_546 ?
C10 O4 Pb3 92.5(4) . 2_546 ?
C10 O4 Pb3 149.4(5) . 4_575 ?
Pb3 O4 Pb3 116.64(19) 2_546 4_575 ?
C13 O5 Pb2 125.3(4) . . ?
C13 O5 Pb1 129.2(4) . 1_655 ?
Pb2 O5 Pb1 102.29(16) . 1_655 ?
C13 O6 Pb2 137.0(4) . 3_676 ?
C16 O7 Pb2 124.3(4) . . ?
C16 O8 Pb3 118.1(5) . . ?
C20 O9 Pb1 90.8(4) . 2_456 ?
C20 O10 Pb1 96.5(4) . 2_456 ?
C20 O10 Pb1 148.3(4) . 4_676 ?
Pb1 O10 Pb1 114.84(17) 2_456 4_676 ?
C28 O11 Pb3 108.2(5) . 1_455 ?
Pb2 O13 H1W 53.8 . . ?
Pb2 O13 H2W 110.4 . . ?
H1W O13 H2W 160.9 . . ?
H3W O14 H4W 117(2) . . ?
O1 C1 O2 121.3(6) . . ?
O1 C1 C2 119.8(7) . . ?
O2 C1 C2 118.9(6) . . ?
C3 C2 C7 119.0(6) . . ?
C3 C2 C1 121.6(6) . . ?
C7 C2 C1 119.3(6) . . ?
C2 C3 C4 120.3(7) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 121.2(7) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 118.0(6) . . ?
C4 C5 C8 122.4(6) . . ?
C6 C5 C8 119.6(6) . . ?
C7 C6 C5 120.9(7) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C2 120.6(7) . . ?
C6 C7 H7 119.7 . . ?
C2 C7 H7 119.7 . . ?
C15 C8 C9 119.1(6) . . ?
C15 C8 C5 119.3(6) . . ?
C9 C8 C5 121.5(6) . . ?
C11 C9 C8 119.4(6) . . ?
C11 C9 C10 116.1(6) . . ?
C8 C9 C10 124.5(6) . . ?
O3 C10 O4 119.8(7) . . ?
O3 C10 C9 120.2(6) . . ?
O4 C10 C9 120.0(6) . . ?
O3 C10 Pb3 59.9(4) . 2_546 ?
O4 C10 Pb3 61.1(4) . 2_546 ?
C9 C10 Pb3 168.5(5) . 2_546 ?
C12 C11 C9 121.3(6) . . ?
C12 C11 H11 119.3 . . ?
C9 C11 H11 119.3 . . ?
C11 C12 C14 119.2(6) . . ?
C11 C12 C13 120.4(6) . . ?
C14 C12 C13 120.3(6) . . ?
O6 C13 O5 123.8(6) . . ?
O6 C13 C12 118.6(7) . . ?
O5 C13 C12 117.6(6) . . ?
C12 C14 C15 119.9(7) . . ?
C12 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C8 C15 C14 120.9(7) . . ?
C8 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
O8 C16 O7 126.0(6) . . ?
O8 C16 C17 118.3(6) . . ?
O7 C16 C17 115.7(6) . . ?
C23 C17 C18 119.7(6) . . ?
C23 C17 C16 121.1(6) . . ?
C18 C17 C16 119.1(6) . . ?
C19 C18 C17 119.1(6) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C21 121.3(6) . . ?
C18 C19 C20 115.7(6) . . ?
C21 C19 C20 122.7(6) . . ?
O9 C20 O10 120.3(6) . . ?
O9 C20 C19 121.0(6) . . ?
O10 C20 C19 118.4(6) . . ?
C22 C21 C19 116.8(6) . . ?
C22 C21 C24 121.1(6) . . ?
C19 C21 C24 122.0(6) . . ?
C23 C22 C21 122.8(7) . . ?
C23 C22 H22 118.6 . . ?
C21 C22 H22 118.6 . . ?
C22 C23 C17 119.8(7) . . ?
C22 C23 H23 120.1 . . ?
C17 C23 H23 120.1 . . ?
C30 C24 C25 118.3(6) . . ?
C30 C24 C21 120.1(7) . . ?
C25 C24 C21 121.4(7) . . ?
C26 C25 C24 120.4(7) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C27 C26 C25 120.0(7) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C29 119.9(7) . . ?
C26 C27 C28 120.9(7) . . ?
C29 C27 C28 119.1(7) . . ?
O12 C28 O11 124.4(7) . . ?
O12 C28 C27 119.2(7) . . ?
O11 C28 C27 116.4(7) . . ?
C30 C29 C27 119.4(7) . . ?
C30 C29 H29 120.3 . . ?
C27 C29 H29 120.3 . . ?
C29 C30 C24 121.8(7) . . ?
C29 C30 H30 119.1 . . ?
C24 C30 H30 119.1 . . ?

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 Pb1 O1 C1 4.2(4) . . . . ?
O10 Pb1 O1 C1 -28.2(5) 2_446 . . . ?
O10 Pb1 O1 C1 -79.4(4) 4_575 . . . ?
O9 Pb1 O1 C1 35.2(5) 2_446 . . . ?
O5 Pb1 O1 C1 87.7(4) 1_455 . . . ?
O10 Pb1 O2 C1 149.0(5) 2_446 . . . ?
O10 Pb1 O2 C1 82.4(4) 4_575 . . . ?
O1 Pb1 O2 C1 -4.2(4) . . . . ?
O9 Pb1 O2 C1 -158.9(5) 2_446 . . . ?
O5 Pb1 O2 C1 -84.9(4) 1_455 . . . ?
O7 Pb2 O5 C13 44.7(5) . . . . ?
O6 Pb2 O5 C13 -91.1(5) 3_676 . . . ?
O13 Pb2 O5 C13 -24.6(5) . . . . ?
O7 Pb2 O5 Pb1 -116.6(2) . . . 1_655 ?
O6 Pb2 O5 Pb1 107.59(17) 3_676 . . 1_655 ?
O13 Pb2 O5 Pb1 174.12(14) . . . 1_655 ?
O5 Pb2 O7 C16 -164.5(7) . . . . ?
O6 Pb2 O7 C16 -98.8(6) 3_676 . . . ?
O13 Pb2 O7 C16 -45.3(6) . . . . ?
O11 Pb3 O8 C16 134.6(5) 1_655 . . . ?
O3 Pb3 O8 C16 -127.4(5) 2_556 . . . ?
O4 Pb3 O8 C16 -152.6(5) 2_556 . . . ?
O4 Pb3 O8 C16 118.6(5) 4_676 . . . ?
C10 Pb3 O8 C16 -136.5(5) 2_556 . . . ?
Pb1 O1 C1 O2 -7.3(7) . . . . ?
Pb1 O1 C1 C2 171.7(6) . . . . ?
Pb1 O2 C1 O1 8.2(8) . . . . ?
Pb1 O2 C1 C2 -170.9(5) . . . . ?
O1 C1 C2 C3 -11.7(11) . . . . ?
O2 C1 C2 C3 167.3(7) . . . . ?
O1 C1 C2 C7 171.3(7) . . . . ?
O2 C1 C2 C7 -9.7(11) . . . . ?
C7 C2 C3 C4 0.4(12) . . . . ?
C1 C2 C3 C4 -176.6(7) . . . . ?
C2 C3 C4 C5 1.2(12) . . . . ?
C3 C4 C5 C6 -2.5(11) . . . . ?
C3 C4 C5 C8 179.3(7) . . . . ?
C4 C5 C6 C7 2.3(12) . . . . ?
C8 C5 C6 C7 -179.4(7) . . . . ?
C5 C6 C7 C2 -0.8(12) . . . . ?
C3 C2 C7 C6 -0.6(12) . . . . ?
C1 C2 C7 C6 176.5(7) . . . . ?
C4 C5 C8 C15 45.7(11) . . . . ?
C6 C5 C8 C15 -132.4(8) . . . . ?
C4 C5 C8 C9 -139.1(8) . . . . ?
C6 C5 C8 C9 42.7(10) . . . . ?
C15 C8 C9 C11 4.0(11) . . . . ?
C5 C8 C9 C11 -171.2(6) . . . . ?
C15 C8 C9 C10 -174.7(7) . . . . ?
C5 C8 C9 C10 10.2(11) . . . . ?
Pb3 O3 C10 O4 12.7(7) 2_546 . . . ?
Pb3 O3 C10 C9 -166.7(5) 2_546 . . . ?
Pb3 O4 C10 O3 -12.6(7) 2_546 . . . ?
Pb3 O4 C10 O3 -175.3(6) 4_575 . . . ?
Pb3 O4 C10 C9 166.8(5) 2_546 . . . ?
Pb3 O4 C10 C9 4.1(13) 4_575 . . . ?
Pb3 O4 C10 Pb3 -162.7(10) 4_575 . . 2_546 ?
C11 C9 C10 O3 41.4(9) . . . . ?
C8 C9 C10 O3 -139.9(7) . . . . ?
C11 C9 C10 O4 -138.0(7) . . . . ?
C8 C9 C10 O4 40.7(10) . . . . ?
C11 C9 C10 Pb3 -46(3) . . . 2_546 ?
C8 C9 C10 Pb3 133(2) . . . 2_546 ?
C8 C9 C11 C12 -3.2(10) . . . . ?
C10 C9 C11 C12 175.6(6) . . . . ?
C9 C11 C12 C14 -0.6(10) . . . . ?
C9 C11 C12 C13 177.6(6) . . . . ?
Pb2 O6 C13 O5 53.0(11) 3_676 . . . ?
Pb2 O6 C13 C12 -127.5(6) 3_676 . . . ?
Pb2 O5 C13 O6 64.1(8) . . . . ?
Pb1 O5 C13 O6 -139.7(6) 1_655 . . . ?
Pb2 O5 C13 C12 -115.3(6) . . . . ?
Pb1 O5 C13 C12 40.8(8) 1_655 . . . ?
C11 C12 C13 O6 -156.5(7) . . . . ?
C14 C12 C13 O6 21.6(10) . . . . ?
C11 C12 C13 O5 22.9(10) . . . . ?
C14 C12 C13 O5 -158.9(7) . . . . ?
C11 C12 C14 C15 3.5(11) . . . . ?
C13 C12 C14 C15 -174.6(7) . . . . ?
C9 C8 C15 C14 -1.0(12) . . . . ?
C5 C8 C15 C14 174.2(7) . . . . ?
C12 C14 C15 C8 -2.7(12) . . . . ?
Pb3 O8 C16 O7 -120.5(7) . . . . ?
Pb3 O8 C16 C17 59.2(8) . . . . ?
Pb2 O7 C16 O8 21.4(11) . . . . ?
Pb2 O7 C16 C17 -158.3(5) . . . . ?
O8 C16 C17 C23 -164.5(7) . . . . ?
O7 C16 C17 C23 15.3(10) . . . . ?
O8 C16 C17 C18 13.6(10) . . . . ?
O7 C16 C17 C18 -166.6(7) . . . . ?
C23 C17 C18 C19 -1.4(10) . . . . ?
C16 C17 C18 C19 -179.5(6) . . . . ?
C17 C18 C19 C21 -4.2(10) . . . . ?
C17 C18 C19 C20 169.3(6) . . . . ?
Pb1 O9 C20 O10 11.7(7) 2_456 . . . ?
Pb1 O9 C20 C19 -160.7(6) 2_456 . . . ?
Pb1 O10 C20 O9 -12.5(7) 2_456 . . . ?
Pb1 O10 C20 O9 159.0(5) 4_676 . . . ?
Pb1 O10 C20 C19 160.2(5) 2_456 . . . ?
Pb1 O10 C20 C19 -28.3(12) 4_676 . . . ?
C18 C19 C20 O9 47.0(9) . . . . ?
C21 C19 C20 O9 -139.6(7) . . . . ?
C18 C19 C20 O10 -125.6(7) . . . . ?
C21 C19 C20 O10 47.8(9) . . . . ?
C18 C19 C21 C22 6.8(10) . . . . ?
C20 C19 C21 C22 -166.2(6) . . . . ?
C18 C19 C21 C24 -171.0(6) . . . . ?
C20 C19 C21 C24 16.0(10) . . . . ?
C19 C21 C22 C23 -4.2(11) . . . . ?
C24 C21 C22 C23 173.6(7) . . . . ?
C21 C22 C23 C17 -1.2(12) . . . . ?
C18 C17 C23 C22 4.1(11) . . . . ?
C16 C17 C23 C22 -177.8(7) . . . . ?
C22 C21 C24 C30 -139.4(7) . . . . ?
C19 C21 C24 C30 38.3(10) . . . . ?
C22 C21 C24 C25 36.0(10) . . . . ?
C19 C21 C24 C25 -146.3(7) . . . . ?
C30 C24 C25 C26 -3.5(11) . . . . ?
C21 C24 C25 C26 -178.9(6) . . . . ?
C24 C25 C26 C27 0.0(11) . . . . ?
C25 C26 C27 C29 2.3(11) . . . . ?
C25 C26 C27 C28 -175.0(7) . . . . ?
Pb3 O11 C28 O12 8.8(10) 1_455 . . . ?
Pb3 O11 C28 C27 -172.3(5) 1_455 . . . ?
C26 C27 C28 O12 -32.2(11) . . . . ?
C29 C27 C28 O12 150.5(8) . . . . ?
C26 C27 C28 O11 148.8(7) . . . . ?
C29 C27 C28 O11 -28.5(10) . . . . ?
C26 C27 C29 C30 -1.1(11) . . . . ?
C28 C27 C29 C30 176.2(7) . . . . ?
C27 C29 C30 C24 -2.5(11) . . . . ?
C25 C24 C30 C29 4.7(11) . . . . ?
C21 C24 C30 C29 -179.8(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O14 H4W O11 0.863(10) 2.18(3) 3.016(9) 163(7) 3_576
O14 H3W O2 0.865(10) 2.46(2) 3.307(9) 166(8) 4_675
O13 H2W O8 0.88 1.87 2.636(6) 144.9 .
O13 H1W O6 0.85 2.09 2.941(7) 179.2 3_676

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        69.71
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.197
