# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1001545'
_audit_update_record             
;
2014-05-07 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H24 N2 O7 Zn'
_chemical_formula_weight         613.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   25.434(7)
_cell_length_b                   13.976(4)
_cell_length_c                   17.825(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.875(5)
_cell_angle_gamma                90.00
_cell_volume                     6242(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5865
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      27.51

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      1.306
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2528
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7533
_exptl_absorpt_correction_T_max  0.8123
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21030
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         28.34
_reflns_number_total             7721
_reflns_number_gt                5556
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0510P)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         7721
_refine_ls_number_parameters     381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.1068
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.002
_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 0.295871(9) 0.739652(15) 0.204165(12) 0.03316(8) Uani 1 1 d . . .
O3 O 0.22407(6) 0.78379(12) 0.21163(8) 0.0494(4) Uani 1 1 d . . .
N1 N 0.34858(6) 0.81340(12) 0.15119(9) 0.0384(4) Uani 1 1 d . . .
C19 C 0.19709(8) 0.79501(15) 0.14451(12) 0.0410(5) Uani 1 1 d . . .
N2 N 0.28824(7) 0.61088(11) 0.14698(9) 0.0372(4) Uani 1 1 d . . .
C14 C 0.26884(8) 0.43623(14) 0.07059(11) 0.0382(5) Uani 1 1 d . . .
C26 C -0.05970(10) 0.8264(3) 0.05905(13) 0.0628(7) Uani 1 1 d . . .
O4 O 0.21708(6) 0.78945(14) 0.08631(10) 0.0619(5) Uani 1 1 d . . .
O7 O 0.21443(8) 0.41209(11) -0.08211(9) 0.0656(5) Uani 1 1 d . . .
O1 O 0.32921(7) 0.68595(14) 0.30270(9) 0.0655(5) Uani 1 1 d . . .
C16 C 0.25864(9) 0.34196(14) 0.03242(11) 0.0397(5) Uani 1 1 d . . .
C11 C 0.29028(9) 0.60313(15) 0.07274(11) 0.0417(5) Uani 1 1 d . . .
H11 H 0.2982 0.6573 0.0465 0.050 Uiso 1 1 calc R . .
O2 O 0.34124(8) 0.83782(15) 0.32945(11) 0.0754(5) Uani 1 1 d . . .
C13 C 0.28113(9) 0.51789(14) 0.03337(11) 0.0427(5) Uani 1 1 d . . .
H13 H 0.2832 0.5155 -0.0182 0.051 Uiso 1 1 calc R . .
C20 C 0.13827(8) 0.81263(16) 0.13937(12) 0.0429(5) Uani 1 1 d . . .
C3 C 0.42462(9) 0.90696(15) 0.08077(12) 0.0424(5) Uani 1 1 d . . .
C5 C 0.33441(9) 0.86113(16) 0.08644(12) 0.0449(5) Uani 1 1 d . . .
H5 H 0.2985 0.8628 0.0645 0.054 Uiso 1 1 calc R . .
C4 C 0.37061(9) 0.90822(17) 0.05040(13) 0.0482(5) Uani 1 1 d . . .
H4 H 0.3588 0.9411 0.0053 0.058 Uiso 1 1 calc R . .
C17 C 0.23243(9) 0.33086(14) -0.04258(12) 0.0430(5) Uani 1 1 d . . .
C15 C 0.27581(10) 0.25928(14) 0.07389(12) 0.0440(5) Uani 1 1 d . . .
H15 H 0.2933 0.2653 0.1240 0.053 Uiso 1 1 calc R . .
O5 O 0.51452(8) 1.00964(15) 0.15668(9) 0.0779(6) Uani 1 1 d . . .
C12 C 0.26687(11) 0.44450(15) 0.14799(12) 0.0509(6) Uani 1 1 d . . .
H12 H 0.2583 0.3918 0.1753 0.061 Uiso 1 1 calc R . .
C6 C 0.46429(9) 0.95495(16) 0.04089(12) 0.0454(5) Uani 1 1 d . . .
C8 C 0.50897(10) 1.00415(17) 0.07911(12) 0.0504(6) Uani 1 1 d . . .
C29 C 0.34630(10) 0.7529(2) 0.34727(14) 0.0526(6) Uani 1 1 d . . .
C30 C 0.37638(9) 0.72346(19) 0.42475(12) 0.0490(6) Uani 1 1 d . . .
C22 C 0.10541(9) 0.81466(18) 0.06871(12) 0.0528(6) Uani 1 1 d . . .
H22 H 0.1202 0.8079 0.0248 0.063 Uiso 1 1 calc R . .
C10 C 0.27766(10) 0.53121(16) 0.18347(12) 0.0501(6) Uani 1 1 d . . .
H10 H 0.2776 0.5349 0.2356 0.060 Uiso 1 1 calc R . .
C7 C 0.45611(9) 0.95252(17) -0.03809(12) 0.0509(6) Uani 1 1 d . . .
H7 H 0.4263 0.9209 -0.0642 0.061 Uiso 1 1 calc R . .
O6 O -0.02518(7) 0.85132(18) 0.12621(9) 0.0895(7) Uani 1 1 d . . .
C23 C 0.05067(9) 0.8267(2) 0.06273(13) 0.0616(7) Uani 1 1 d . . .
H23 H 0.0290 0.8278 0.0151 0.074 Uiso 1 1 calc R . .
C28 C -0.06907(12) 0.7327(3) 0.04243(16) 0.0762(9) Uani 1 1 d . . .
H28 H -0.0539 0.6859 0.0765 0.091 Uiso 1 1 calc R . .
C25 C 0.02893(9) 0.8370(2) 0.12687(13) 0.0633(7) Uani 1 1 d . . .
C21 C 0.11556(9) 0.8238(2) 0.20310(13) 0.0651(8) Uani 1 1 d . . .
H21 H 0.1371 0.8224 0.2509 0.078 Uiso 1 1 calc R . .
C32 C 0.39870(11) 0.7935(2) 0.47460(15) 0.0627(7) Uani 1 1 d . . .
H32 H 0.3922 0.8578 0.4629 0.075 Uiso 1 1 calc R . .
C1 C 0.40061(9) 0.81287(19) 0.18128(14) 0.0597(7) Uani 1 1 d . . .
H1 H 0.4113 0.7803 0.2268 0.072 Uiso 1 1 calc R . .
C2 C 0.43894(10) 0.85778(19) 0.14854(14) 0.0610(7) Uani 1 1 d . . .
H2 H 0.4745 0.8552 0.1719 0.073 Uiso 1 1 calc R . .
C27 C -0.08334(11) 0.8966(2) 0.01226(15) 0.0717(8) Uani 1 1 d . . .
H27 H -0.0780 0.9607 0.0254 0.086 Uiso 1 1 calc R . .
C9 C 0.56376(14) 1.0469(3) 0.19777(15) 0.1024(13) Uani 1 1 d . . .
H9A H 0.5932 1.0133 0.1828 0.154 Uiso 1 1 calc R . .
H9B H 0.5646 1.0387 0.2514 0.154 Uiso 1 1 calc R . .
H9C H 0.5664 1.1138 0.1866 0.154 Uiso 1 1 calc R . .
C24 C 0.06142(10) 0.8371(3) 0.19777(13) 0.0820(10) Uani 1 1 d . . .
H24 H 0.0467 0.8460 0.2415 0.098 Uiso 1 1 calc R . .
C18 C 0.18765(14) 0.4027(2) -0.15733(14) 0.0821(10) Uani 1 1 d . . .
H18A H 0.2100 0.3693 -0.1868 0.123 Uiso 1 1 calc R . .
H18B H 0.1794 0.4651 -0.1788 0.123 Uiso 1 1 calc R . .
H18C H 0.1552 0.3675 -0.1579 0.123 Uiso 1 1 calc R . .
C31 C 0.38448(10) 0.6295(2) 0.44457(14) 0.0626(7) Uani 1 1 d . . .
H31 H 0.3681 0.5821 0.4120 0.075 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 1.9536(16) . ?
Zn1 O1 1.9638(17) . ?
Zn1 N1 2.0458(16) . ?
Zn1 N2 2.0610(16) . ?
O3 C19 1.283(2) . ?
N1 C5 1.328(3) . ?
N1 C1 1.340(3) . ?
C19 O4 1.233(3) . ?
C19 C20 1.503(3) . ?
N2 C11 1.338(2) . ?
N2 C10 1.340(3) . ?
C14 C13 1.383(3) . ?
C14 C12 1.394(3) . ?
C14 C16 1.485(3) . ?
C26 C28 1.355(4) . ?
C26 C27 1.359(4) . ?
C26 O6 1.402(3) . ?
O7 C17 1.373(2) . ?
O7 C18 1.402(3) . ?
O1 C29 1.256(3) . ?
C16 C17 1.396(3) . ?
C16 C15 1.401(3) . ?
C11 C13 1.382(3) . ?
O2 C29 1.229(3) . ?
C20 C21 1.369(3) . ?
C20 C22 1.387(3) . ?
C3 C2 1.383(3) . ?
C3 C4 1.387(3) . ?
C3 C6 1.490(3) . ?
C5 C4 1.377(3) . ?
C17 C15 1.379(3) 7 ?
C15 C17 1.379(3) 7 ?
O5 C8 1.368(3) . ?
O5 C9 1.436(3) . ?
C12 C10 1.373(3) . ?
C6 C7 1.388(3) . ?
C6 C8 1.401(3) . ?
C8 C7 1.383(3) 5_675 ?
C29 C30 1.516(3) . ?
C30 C31 1.367(4) . ?
C30 C32 1.377(3) . ?
C22 C23 1.388(3) . ?
C7 C8 1.383(3) 5_675 ?
O6 C25 1.389(3) . ?
C23 C25 1.360(3) . ?
C28 C32 1.389(4) 8_465 ?
C25 C24 1.386(3) . ?
C21 C24 1.376(3) . ?
C32 C28 1.389(4) 8_566 ?
C1 C2 1.371(3) . ?
C27 C31 1.385(3) 8_465 ?
C31 C27 1.385(3) 8_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zn1 O1 108.97(7) . . ?
O3 Zn1 N1 124.51(7) . . ?
O1 Zn1 N1 112.88(8) . . ?
O3 Zn1 N2 107.43(7) . . ?
O1 Zn1 N2 95.63(7) . . ?
N1 Zn1 N2 103.01(7) . . ?
C19 O3 Zn1 109.38(13) . . ?
C5 N1 C1 116.92(18) . . ?
C5 N1 Zn1 123.54(14) . . ?
C1 N1 Zn1 119.52(14) . . ?
O4 C19 O3 123.0(2) . . ?
O4 C19 C20 120.55(19) . . ?
O3 C19 C20 116.38(18) . . ?
C11 N2 C10 117.26(17) . . ?
C11 N2 Zn1 122.93(13) . . ?
C10 N2 Zn1 119.69(13) . . ?
C13 C14 C12 117.12(18) . . ?
C13 C14 C16 123.27(18) . . ?
C12 C14 C16 119.60(18) . . ?
C28 C26 C27 121.4(2) . . ?
C28 C26 O6 119.2(3) . . ?
C27 C26 O6 119.4(3) . . ?
C17 O7 C18 118.58(18) . . ?
C29 O1 Zn1 109.29(17) . . ?
C17 C16 C15 117.91(18) . . ?
C17 C16 C14 123.67(18) . . ?
C15 C16 C14 118.43(18) . . ?
N2 C11 C13 122.72(18) . . ?
C11 C13 C14 120.01(18) . . ?
C21 C20 C22 118.5(2) . . ?
C21 C20 C19 121.70(19) . . ?
C22 C20 C19 119.79(19) . . ?
C2 C3 C4 116.21(19) . . ?
C2 C3 C6 122.8(2) . . ?
C4 C3 C6 121.0(2) . . ?
N1 C5 C4 122.8(2) . . ?
C5 C4 C3 120.6(2) . . ?
O7 C17 C15 122.24(19) . 7 ?
O7 C17 C16 117.52(17) . . ?
C15 C17 C16 120.22(18) 7 . ?
C17 C15 C16 121.9(2) 7 . ?
C8 O5 C9 117.76(19) . . ?
C10 C12 C14 119.41(19) . . ?
C7 C6 C8 118.25(19) . . ?
C7 C6 C3 118.50(19) . . ?
C8 C6 C3 123.24(19) . . ?
O5 C8 C7 123.1(2) . 5_675 ?
O5 C8 C6 116.98(19) . . ?
C7 C8 C6 119.9(2) 5_675 . ?
O2 C29 O1 123.1(2) . . ?
O2 C29 C30 120.8(2) . . ?
O1 C29 C30 116.1(2) . . ?
C31 C30 C32 119.3(2) . . ?
C31 C30 C29 121.8(2) . . ?
C32 C30 C29 118.8(2) . . ?
C20 C22 C23 120.8(2) . . ?
N2 C10 C12 123.43(19) . . ?
C8 C7 C6 121.8(2) 5_675 . ?
C25 O6 C26 116.50(18) . . ?
C25 C23 C22 119.7(2) . . ?
C26 C28 C32 120.1(3) . 8_465 ?
C23 C25 C24 120.1(2) . . ?
C23 C25 O6 123.6(2) . . ?
C24 C25 O6 116.3(2) . . ?
C20 C21 C24 121.2(2) . . ?
C30 C32 C28 119.4(3) . 8_566 ?
N1 C1 C2 123.5(2) . . ?
C1 C2 C3 120.0(2) . . ?
C26 C27 C31 118.6(3) . 8_465 ?
C21 C24 C25 119.7(2) . . ?
C30 C31 C27 121.2(2) . 8_566 ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 1.000 0.085 0.250 178 36 ' '
2 1.000 -0.085 0.750 178 36 ' '
3 0.667 0.083 0.131 7 1 ' '
4 0.333 0.083 0.369 7 1 ' '
5 0.500 0.415 0.750 178 36 ' '
6 0.167 0.417 0.631 7 1 ' '
7 0.833 0.417 0.869 7 1 ' '
8 0.500 0.585 0.250 178 36 ' '
9 0.167 0.583 0.131 7 1 ' '
10 0.833 0.583 0.369 7 1 ' '
11 0.667 0.917 0.631 7 1 ' '
12 0.333 0.917 0.869 7 1 ' '
_platon_squeeze_details          
; 
;
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.055
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1001546'
_audit_update_record             
;
2014-05-07 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H24 Co N2 O7'
_chemical_formula_weight         607.46

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   25.3160(17)
_cell_length_b                   13.9919(10)
_cell_length_c                   17.8674(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.3550(10)
_cell_angle_gamma                90.00
_cell_volume                     6225.9(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6549
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      24.97

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      1.296
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2504
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8133
_exptl_absorpt_correction_T_max  0.8408
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27865
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         27.53
_reflns_number_total             7148
_reflns_number_gt                5668
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0610P)²+2.3845P] 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         7148
_refine_ls_number_parameters     381
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.1141
_refine_ls_wR_factor_gt          0.1082
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002

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 0.204849(9) 0.240157(17) 0.298585(13) 0.02991(9) Uani 1 1 d . . .
O1 O 0.16075(7) 0.33269(13) 0.17787(10) 0.0640(5) Uani 1 1 d . . .
O2 O 0.16826(6) 0.17967(12) 0.20325(8) 0.0549(4) Uani 1 1 d . . .
O3 O -0.22384(6) 0.21984(12) -0.22014(8) 0.0488(4) Uani 1 1 d . . .
O4 O -0.22077(6) 0.20501(14) -0.09703(9) 0.0573(4) Uani 1 1 d . . .
O5 O 0.28593(8) -0.08958(10) 0.58351(8) 0.0628(5) Uani 1 1 d . . .
O6 O -0.01583(7) 0.50409(16) 0.34316(9) 0.0745(6) Uani 1 1 d . . .
O10 O 0.02542(6) 0.1550(2) -0.12451(9) 0.0908(8) Uani 1 1 d . . .
N1 N 0.21518(6) 0.11343(11) 0.35744(8) 0.0354(3) Uani 1 1 d . . .
N2 N 0.15088(6) 0.31215(11) 0.35082(9) 0.0373(4) Uani 1 1 d . . .
C1 C -0.19799(8) 0.20436(15) -0.15272(12) 0.0402(4) Uani 1 1 d . . .
C2 C 0.21945(8) 0.01817(14) 0.46907(10) 0.0391(4) Uani 1 1 d . . .
H2 H 0.2159 0.0146 0.5199 0.047 Uiso 1 1 calc R . .
C3 C 0.23280(8) -0.06301(13) 0.43171(10) 0.0350(4) Uani 1 1 d . . .
C4 C 0.26781(8) -0.17024(14) 0.54399(11) 0.0406(4) Uani 1 1 d . . .
C5 C -0.13885(8) 0.18791(16) -0.14368(11) 0.0427(5) Uani 1 1 d . . .
C6 C 0.21154(8) 0.10383(14) 0.43080(10) 0.0382(4) Uani 1 1 d . . .
H6 H 0.2033 0.1575 0.4572 0.046 Uiso 1 1 calc R . .
C7 C 0.05895(9) 0.1776(3) -0.05543(13) 0.0637(8) Uani 1 1 d U . .
C8 C 0.24180(8) -0.15798(13) 0.46820(11) 0.0366(4) Uani 1 1 d . . .
C9 C 0.07493(8) 0.40551(15) 0.42092(12) 0.0405(4) Uani 1 1 d . . .
C10 C 0.12909(8) 0.41094(17) 0.44909(12) 0.0477(5) Uani 1 1 d . . .
H10 H 0.1413 0.4471 0.4924 0.057 Uiso 1 1 calc R . .
C11 C -0.00960(9) 0.50134(17) 0.42071(12) 0.0487(5) Uani 1 1 d . . .
C12 C 0.23600(9) -0.05283(14) 0.35529(11) 0.0458(5) Uani 1 1 d . . .
H12 H 0.2446 -0.1051 0.3276 0.055 Uiso 1 1 calc R . .
C13 C 0.22446(9) -0.23875(14) 0.42625(11) 0.0412(5) Uani 1 1 d . . .
H13 H 0.2070 -0.2315 0.3762 0.049 Uiso 1 1 calc R . .
C14 C 0.03546(8) 0.45417(16) 0.46004(12) 0.0439(5) Uani 1 1 d . . .
C15 C 0.16531(8) 0.36351(16) 0.41392(12) 0.0447(5) Uani 1 1 d . . .
H15 H 0.2016 0.3674 0.4351 0.054 Uiso 1 1 calc R . .
C16 C 0.15290(8) 0.24921(17) 0.15838(12) 0.0449(5) Uani 1 1 d . . .
C17 C 0.22650(10) 0.03454(15) 0.32086(11) 0.0467(5) Uani 1 1 d . . .
H17 H 0.2280 0.0393 0.2694 0.056 Uiso 1 1 calc R . .
C18 C 0.12266(8) 0.22335(17) 0.08077(11) 0.0438(5) Uani 1 1 d . . .
C19 C -0.10718(9) 0.18621(19) -0.07289(12) 0.0531(6) Uani 1 1 d . . .
H19 H -0.1231 0.1924 -0.0301 0.064 Uiso 1 1 calc R . .
C21 C 0.04452(8) 0.45415(17) 0.53858(12) 0.0486(5) Uani 1 1 d . . .
H21 H 0.0748 0.4235 0.5650 0.058 Uiso 1 1 calc R . .
C22 C -0.11497(9) 0.1777(2) -0.20647(13) 0.0668(8) Uani 1 1 d . . .
H22 H -0.1360 0.1783 -0.2548 0.080 Uiso 1 1 calc R . .
C23 C -0.05220(9) 0.1755(2) -0.06361(12) 0.0621(7) Uani 1 1 d . . .
H23 H -0.0312 0.1739 -0.0153 0.074 Uiso 1 1 calc R . .
C24 C -0.02922(9) 0.1671(2) -0.12736(13) 0.0640(7) Uani 1 1 d . . .
C25 C 0.05998(9) 0.3517(2) 0.35529(15) 0.0619(7) Uani 1 1 d . . .
H25 H 0.0239 0.3455 0.3336 0.074 Uiso 1 1 calc R . .
C26 C 0.09854(9) 0.30736(19) 0.32223(14) 0.0584(6) Uani 1 1 d . . .
H26 H 0.0876 0.2724 0.2779 0.070 Uiso 1 1 calc R . .
C27 C 0.11388(10) 0.1299(2) 0.05958(14) 0.0606(6) Uani 1 1 d . . .
H27 H 0.1296 0.0816 0.0919 0.073 Uiso 1 1 calc R . .
C28 C 0.31338(14) -0.09967(19) 0.65903(13) 0.0781(9) Uani 1 1 d . . .
H28A H 0.2913 -0.1342 0.6881 0.117 Uiso 1 1 calc R . .
H28B H 0.3214 -0.0376 0.6811 0.117 Uiso 1 1 calc R . .
H28C H 0.3462 -0.1341 0.6593 0.117 Uiso 1 1 calc R . .
C29 C 0.08178(11) 0.1060(2) -0.00968(15) 0.0733(8) Uani 1 1 d . . .
H29 H 0.0762 0.0425 -0.0241 0.088 Uiso 1 1 calc R . .
C30 C 0.10130(11) 0.2947(2) 0.03102(14) 0.0628(6) Uani 1 1 d . . .
H30 H 0.1083 0.3584 0.0438 0.075 Uiso 1 1 calc R . .
C31 C -0.06043(9) 0.1667(3) -0.19849(13) 0.0847(11) Uani 1 1 d . . .
H31 H -0.0446 0.1590 -0.2412 0.102 Uiso 1 1 calc R . .
C32 C 0.06948(12) 0.2714(3) -0.03766(16) 0.0754(9) Uani 1 1 d U . .
H32 H 0.0553 0.3192 -0.0716 0.090 Uiso 1 1 calc R . .
C33 C -0.06473(13) 0.5404(3) 0.30161(16) 0.0931(11) Uani 1 1 d . . .
H33A H -0.0944 0.5082 0.3174 0.140 Uiso 1 1 calc R . .
H33B H -0.0659 0.5297 0.2482 0.140 Uiso 1 1 calc R . .
H33C H -0.0670 0.6077 0.3110 0.140 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 O3 1.9752(14) 8_556 ?
Co1 O2 1.9771(15) . ?
Co1 N2 2.0521(15) . ?
Co1 N1 2.0542(15) . ?
O1 C16 1.225(3) . ?
O2 C16 1.276(3) . ?
O3 C1 1.282(2) . ?
O3 Co1 1.9752(14) 8_455 ?
O4 C1 1.236(2) . ?
O5 C4 1.366(2) . ?
O5 C28 1.409(3) . ?
O6 C11 1.367(3) . ?
O6 C33 1.418(3) . ?
O10 C24 1.386(3) . ?
O10 C7 1.402(3) . ?
N1 C6 1.337(2) . ?
N1 C17 1.340(2) . ?
N2 C26 1.333(3) . ?
N2 C15 1.332(3) . ?
C1 C5 1.495(3) . ?
C2 C6 1.377(3) . ?
C2 C3 1.390(3) . ?
C2 H2 0.9300 . ?
C3 C12 1.390(3) . ?
C3 C8 1.480(2) . ?
C4 C13 1.380(3) 7_546 ?
C4 C8 1.406(3) . ?
C5 C19 1.371(3) . ?
C5 C22 1.374(3) . ?
C6 H6 0.9300 . ?
C7 C29 1.354(4) . ?
C7 C32 1.365(5) . ?
C8 C13 1.383(3) . ?
C9 C10 1.375(3) . ?
C9 C25 1.388(3) . ?
C9 C14 1.484(3) . ?
C10 C15 1.372(3) . ?
C10 H10 0.9300 . ?
C11 C21 1.389(3) 5_566 ?
C11 C14 1.394(3) . ?
C12 C17 1.370(3) . ?
C12 H12 0.9300 . ?
C13 C4 1.380(3) 7_546 ?
C13 H13 0.9300 . ?
C14 C21 1.381(3) . ?
C15 H15 0.9300 . ?
C16 C18 1.503(3) . ?
C17 H17 0.9300 . ?
C18 C27 1.368(3) . ?
C18 C30 1.380(3) . ?
C19 C23 1.380(3) . ?
C19 H19 0.9300 . ?
C21 C11 1.389(3) 5_566 ?
C21 H21 0.9300 . ?
C22 C31 1.371(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.374(3) . ?
C23 H23 0.9300 . ?
C24 C31 1.370(3) . ?
C25 C26 1.376(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C29 1.394(3) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29 0.9300 . ?
C30 C32 1.381(4) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O2 106.04(7) 8_556 . ?
O3 Co1 N2 129.90(7) 8_556 . ?
O2 Co1 N2 110.79(7) . . ?
O3 Co1 N1 107.17(6) 8_556 . ?
O2 Co1 N1 93.92(6) . . ?
N2 Co1 N1 102.99(6) . . ?
C16 O2 Co1 104.93(14) . . ?
C1 O3 Co1 102.50(12) . 8_455 ?
C4 O5 C28 118.30(17) . . ?
C11 O6 C33 118.14(18) . . ?
C24 O10 C7 116.56(17) . . ?
C6 N1 C17 117.00(16) . . ?
C6 N1 Co1 124.31(13) . . ?
C17 N1 Co1 118.69(12) . . ?
C26 N2 C15 117.00(17) . . ?
C26 N2 Co1 119.88(14) . . ?
C15 N2 Co1 123.11(13) . . ?
O4 C1 O3 121.46(18) . . ?
O4 C1 C5 121.15(19) . . ?
O3 C1 C5 117.38(18) . . ?
C6 C2 C3 119.95(17) . . ?
C6 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C12 C3 C2 116.77(17) . . ?
C12 C3 C8 119.57(17) . . ?
C2 C3 C8 123.63(17) . . ?
O5 C4 C13 123.50(17) . 7_546 ?
O5 C4 C8 116.92(16) . . ?
C13 C4 C8 119.54(17) 7_546 . ?
C19 C5 C22 118.77(19) . . ?
C19 C5 C1 120.72(19) . . ?
C22 C5 C1 120.47(18) . . ?
N1 C6 C2 123.02(17) . . ?
N1 C6 H6 118.5 . . ?
C2 C6 H6 118.5 . . ?
C29 C7 C32 121.7(2) . . ?
C29 C7 O10 119.3(3) . . ?
C32 C7 O10 118.9(3) . . ?
C13 C8 C4 118.06(17) . . ?
C13 C8 C3 119.09(16) . . ?
C4 C8 C3 122.85(17) . . ?
C10 C9 C25 116.21(18) . . ?
C10 C9 C14 120.92(19) . . ?
C25 C9 C14 122.87(18) . . ?
C15 C10 C9 120.66(19) . . ?
C15 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
O6 C11 C21 123.37(19) . 5_566 ?
O6 C11 C14 117.33(18) . . ?
C21 C11 C14 119.3(2) 5_566 . ?
C17 C12 C3 119.74(18) . . ?
C17 C12 H12 120.1 . . ?
C3 C12 H12 120.1 . . ?
C4 C13 C8 122.40(18) 7_546 . ?
C4 C13 H13 118.8 7_546 . ?
C8 C13 H13 118.8 . . ?
C21 C14 C11 118.94(18) . . ?
C21 C14 C9 118.41(18) . . ?
C11 C14 C9 122.64(19) . . ?
N2 C15 C10 122.99(19) . . ?
N2 C15 H15 118.5 . . ?
C10 C15 H15 118.5 . . ?
O1 C16 O2 122.2(2) . . ?
O1 C16 C18 121.4(2) . . ?
O2 C16 C18 116.3(2) . . ?
N1 C17 C12 123.48(18) . . ?
N1 C17 H17 118.3 . . ?
C12 C17 H17 118.3 . . ?
C27 C18 C30 119.2(2) . . ?
C27 C18 C16 121.1(2) . . ?
C30 C18 C16 119.7(2) . . ?
C5 C19 C23 121.5(2) . . ?
C5 C19 H19 119.2 . . ?
C23 C19 H19 119.2 . . ?
C14 C21 C11 121.8(2) . 5_566 ?
C14 C21 H21 119.1 . . ?
C11 C21 H21 119.1 5_566 . ?
C31 C22 C5 120.6(2) . . ?
C31 C22 H22 119.7 . . ?
C5 C22 H22 119.7 . . ?
C24 C23 C19 118.5(2) . . ?
C24 C23 H23 120.7 . . ?
C19 C23 H23 120.7 . . ?
C31 C24 C23 120.6(2) . . ?
C31 C24 O10 116.0(2) . . ?
C23 C24 O10 123.27(19) . . ?
C26 C25 C9 120.0(2) . . ?
C26 C25 H25 120.0 . . ?
C9 C25 H25 120.0 . . ?
N2 C26 C25 123.1(2) . . ?
N2 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
C18 C27 C29 121.0(2) . . ?
C18 C27 H27 119.5 . . ?
C29 C27 H27 119.5 . . ?
O5 C28 H28A 109.5 . . ?
O5 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O5 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C7 C29 C27 118.4(3) . . ?
C7 C29 H29 120.8 . . ?
C27 C29 H29 120.8 . . ?
C32 C30 C18 120.0(3) . . ?
C32 C30 H30 120.0 . . ?
C18 C30 H30 120.0 . . ?
C24 C31 C22 119.9(2) . . ?
C24 C31 H31 120.1 . . ?
C22 C31 H31 120.1 . . ?
C7 C32 C30 119.5(3) . . ?
C7 C32 H32 120.3 . . ?
C30 C32 H32 120.3 . . ?
O6 C33 H33A 109.5 . . ?
O6 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O6 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Co1 O2 C16 -76.99(15) 8_556 . . . ?
N2 Co1 O2 C16 68.39(15) . . . . ?
N1 Co1 O2 C16 173.88(14) . . . . ?
O3 Co1 N1 C6 108.80(16) 8_556 . . . ?
O2 Co1 N1 C6 -143.08(16) . . . . ?
N2 Co1 N1 C6 -30.70(17) . . . . ?
O3 Co1 N1 C17 -70.98(17) 8_556 . . . ?
O2 Co1 N1 C17 37.14(17) . . . . ?
N2 Co1 N1 C17 149.52(16) . . . . ?
O3 Co1 N2 C26 139.45(18) 8_556 . . . ?
O2 Co1 N2 C26 4.8(2) . . . . ?
N1 Co1 N2 C26 -94.55(19) . . . . ?
O3 Co1 N2 C15 -41.68(19) 8_556 . . . ?
O2 Co1 N2 C15 -176.31(16) . . . . ?
N1 Co1 N2 C15 84.32(17) . . . . ?
Co1 O3 C1 O4 8.3(2) 8_455 . . . ?
Co1 O3 C1 C5 -170.14(15) 8_455 . . . ?
C6 C2 C3 C12 -1.7(3) . . . . ?
C6 C2 C3 C8 -179.73(19) . . . . ?
C28 O5 C4 C13 -0.8(4) . . . 7_546 ?
C28 O5 C4 C8 -178.4(2) . . . . ?
O4 C1 C5 C19 -9.0(3) . . . . ?
O3 C1 C5 C19 169.4(2) . . . . ?
O4 C1 C5 C22 173.4(2) . . . . ?
O3 C1 C5 C22 -8.1(3) . . . . ?
C17 N1 C6 C2 0.8(3) . . . . ?
Co1 N1 C6 C2 -179.01(15) . . . . ?
C3 C2 C6 N1 1.2(3) . . . . ?
C24 O10 C7 C29 105.5(3) . . . . ?
C24 O10 C7 C32 -77.2(4) . . . . ?
O5 C4 C8 C13 178.2(2) . . . . ?
C13 C4 C8 C13 0.5(4) 7_546 . . . ?
O5 C4 C8 C3 -1.3(3) . . . . ?
C13 C4 C8 C3 -178.93(19) 7_546 . . . ?
C12 C3 C8 C13 -35.4(3) . . . . ?
C2 C3 C8 C13 142.6(2) . . . . ?
C12 C3 C8 C4 144.0(2) . . . . ?
C2 C3 C8 C4 -38.0(3) . . . . ?
C25 C9 C10 C15 -1.2(3) . . . . ?
C14 C9 C10 C15 178.1(2) . . . . ?
C33 O6 C11 C21 -10.7(4) . . . 5_566 ?
C33 O6 C11 C14 171.8(3) . . . . ?
C2 C3 C12 C17 0.4(3) . . . . ?
C8 C3 C12 C17 178.5(2) . . . . ?
C4 C8 C13 C4 -0.5(4) . . . 7_546 ?
C3 C8 C13 C4 178.9(2) . . . 7_546 ?
O6 C11 C14 C21 176.7(2) . . . . ?
C21 C11 C14 C21 -0.9(4) 5_566 . . . ?
O6 C11 C14 C9 -1.9(4) . . . . ?
C21 C11 C14 C9 -179.5(2) 5_566 . . . ?
C10 C9 C14 C21 -38.7(3) . . . . ?
C25 C9 C14 C21 140.6(3) . . . . ?
C10 C9 C14 C11 140.0(2) . . . . ?
C25 C9 C14 C11 -40.8(3) . . . . ?
C26 N2 C15 C10 -0.5(3) . . . . ?
Co1 N2 C15 C10 -179.43(17) . . . . ?
C9 C10 C15 N2 1.5(4) . . . . ?
Co1 O2 C16 O1 -1.3(3) . . . . ?
Co1 O2 C16 C18 -179.09(14) . . . . ?
C6 N1 C17 C12 -2.2(3) . . . . ?
Co1 N1 C17 C12 177.64(19) . . . . ?
C3 C12 C17 N1 1.6(4) . . . . ?
O1 C16 C18 C27 -179.7(2) . . . . ?
O2 C16 C18 C27 -1.9(3) . . . . ?
O1 C16 C18 C30 -2.6(3) . . . . ?
O2 C16 C18 C30 175.2(2) . . . . ?
C22 C5 C19 C23 0.6(4) . . . . ?
C1 C5 C19 C23 -177.0(3) . . . . ?
C11 C14 C21 C11 0.9(4) . . . 5_566 ?
C9 C14 C21 C11 179.6(2) . . . 5_566 ?
C19 C5 C22 C31 -0.4(5) . . . . ?
C1 C5 C22 C31 177.2(3) . . . . ?
C5 C19 C23 C24 0.5(4) . . . . ?
C19 C23 C24 C31 -1.8(5) . . . . ?
C19 C23 C24 O10 -179.3(3) . . . . ?
C7 O10 C24 C31 165.3(3) . . . . ?
C7 O10 C24 C23 -17.1(5) . . . . ?
C10 C9 C25 C26 0.1(4) . . . . ?
C14 C9 C25 C26 -179.2(2) . . . . ?
C15 N2 C26 C25 -0.7(4) . . . . ?
Co1 N2 C26 C25 178.3(2) . . . . ?
C9 C25 C26 N2 0.9(4) . . . . ?
C30 C18 C27 C29 -3.0(4) . . . . ?
C16 C18 C27 C29 174.2(2) . . . . ?
C32 C7 C29 C27 4.4(4) . . . . ?
O10 C7 C29 C27 -178.4(2) . . . . ?
C18 C27 C29 C7 -0.6(4) . . . . ?
C27 C18 C30 C32 2.9(4) . . . . ?
C16 C18 C30 C32 -174.3(2) . . . . ?
C23 C24 C31 C22 2.0(5) . . . . ?
O10 C24 C31 C22 179.7(3) . . . . ?
C5 C22 C31 C24 -0.8(5) . . . . ?
C29 C7 C32 C30 -4.4(4) . . . . ?
O10 C7 C32 C30 178.4(2) . . . . ?
C18 C30 C32 C7 0.7(4) . . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 1.000 0.083 0.250 191 37 ' '
2 1.000 -0.083 0.750 191 37 ' '
3 0.658 0.074 0.122 12 0 ' '
4 0.342 0.074 0.378 12 0 ' '
5 0.485 0.180 0.214 7 0 ' '
6 0.520 0.180 0.297 6 0 ' '
7 0.500 0.417 0.750 191 37 ' '
8 0.985 0.319 0.714 7 0 ' '
9 0.020 0.319 0.797 6 0 ' '
10 0.158 0.426 0.622 12 0 ' '
11 0.842 0.426 0.878 12 0 ' '
12 0.500 0.583 0.250 191 37 ' '
13 0.158 0.574 0.122 12 0 ' '
14 0.842 0.574 0.378 12 0 ' '
15 0.985 0.680 0.214 7 0 ' '
16 0.020 0.680 0.297 6 0 ' '
17 0.485 0.819 0.714 7 0 ' '
18 0.520 0.819 0.797 6 0 ' '
19 0.658 0.926 0.622 12 0 ' '
20 0.342 0.926 0.878 12 0 ' '
_platon_squeeze_details          
; 
;
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.050
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1001547'
_audit_update_record             
;
2014-05-07 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H24 Cd N2 O7'
_chemical_formula_weight         660.93

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.317(3)
_cell_length_b                   12.722(4)
_cell_length_c                   15.451(4)
_cell_angle_alpha                108.632(4)
_cell_angle_beta                 97.755(4)
_cell_angle_gamma                91.789(4)
_cell_volume                     1714.2(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3444
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      23.21

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      1.281
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             668
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8324
_exptl_absorpt_correction_T_max  0.8648
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13367
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_sigmaI/netI    0.1320
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         26.37
_reflns_number_total             6897
_reflns_number_gt                5091
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.1250P)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         6897
_refine_ls_number_parameters     381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_ref         0.2269
_refine_ls_wR_factor_gt          0.2166
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.002
_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 1.14157(5) 0.52590(3) 0.39962(3) 0.0336(2) Uani 1 1 d . . .
O5 O 1.4626(7) 0.6682(8) -0.0317(4) 0.100(3) Uani 1 1 d . . .
O1 O 1.3062(6) 0.6157(5) 0.3372(4) 0.0543(13) Uani 1 1 d . . .
O2 O 1.1526(6) 0.4832(5) 0.2380(4) 0.0527(13) Uani 1 1 d . . .
O3 O 1.2461(5) 0.5944(4) -0.4535(4) 0.0488(12) Uani 1 1 d . . .
O4 O 1.0325(5) 0.6000(4) -0.4029(4) 0.0467(12) Uani 1 1 d . . .
O7 O 0.3241(5) 0.9943(4) 0.3888(4) 0.0533(13) Uani 1 1 d . . .
O6 O 0.8945(7) 1.0021(6) 0.3278(7) 0.105(3) Uani 1 1 d . . .
N1 N 1.2821(6) 0.3726(4) 0.3882(4) 0.0401(13) Uani 1 1 d . . .
N2 N 0.9705(6) 0.6533(5) 0.3830(5) 0.0478(15) Uani 1 1 d . . .
C3 C 0.7886(7) 0.8196(5) 0.3684(6) 0.0453(17) Uani 1 1 d . . .
C2 C 0.8406(12) 0.7495(8) 0.2915(7) 0.091(4) Uani 1 1 d . . .
H2 H 0.8151 0.7578 0.2338 0.109 Uiso 1 1 calc R . .
C4 C 0.8297(13) 0.8013(9) 0.4462(7) 0.087(4) Uani 1 1 d . . .
H4 H 0.7993 0.8460 0.5000 0.105 Uiso 1 1 calc R . .
C1 C 0.9295(11) 0.6683(7) 0.3007(7) 0.078(3) Uani 1 1 d . . .
H1 H 0.9625 0.6221 0.2486 0.093 Uiso 1 1 calc R . .
C32 C 1.1673(7) 0.6034(5) -0.3906(5) 0.0343(14) Uani 1 1 d . . .
C7 C 0.5540(7) 0.9064(5) 0.3773(5) 0.0415(15) Uani 1 1 d . . .
H7 H 0.5159 0.8448 0.3891 0.050 Uiso 1 1 calc R . .
C19 C 1.2516(8) 0.5591(6) 0.2562(5) 0.0426(16) Uani 1 1 d . . .
C8 C 0.4679(7) 0.9933(5) 0.3770(5) 0.0391(15) Uani 1 1 d . . .
C6 C 0.6959(7) 0.9102(5) 0.3602(6) 0.0447(17) Uani 1 1 d . . .
C16 C 0.4637(8) 1.2767(6) 0.4503(6) 0.0481(19) Uani 1 1 d . . .
H16 H 0.5342 1.2776 0.4993 0.058 Uiso 1 1 calc R . .
C21 C 1.4210(10) 0.6637(9) 0.1939(6) 0.072(3) Uani 1 1 d . . .
H21 H 1.4655 0.7003 0.2543 0.086 Uiso 1 1 calc R . .
C9 C 0.5260(8) 1.0873(6) 0.3626(6) 0.0461(17) Uani 1 1 d . . .
C14 C 0.4398(7) 1.1862(5) 0.3707(6) 0.0447(17) Uani 1 1 d . . .
C28 C 1.3938(8) 0.6107(7) -0.2780(6) 0.0511(18) Uani 1 1 d . . .
H28 H 1.4466 0.5931 -0.3270 0.061 Uiso 1 1 calc R . .
C25 C 1.2432(11) 0.5290(8) 0.0879(6) 0.069(3) Uani 1 1 d . . .
H25 H 1.1678 0.4743 0.0754 0.083 Uiso 1 1 calc R . .
C29 C 1.2454(7) 0.6231(6) -0.2950(5) 0.0385(15) Uani 1 1 d . . .
C20 C 1.3072(8) 0.5851(7) 0.1773(5) 0.0470(17) Uani 1 1 d . . .
C17 C 1.2588(8) 0.2842(6) 0.3108(6) 0.0496(18) Uani 1 1 d . . .
H17 H 1.1898 0.2863 0.2620 0.059 Uiso 1 1 calc R . .
C18 C 1.3804(8) 0.3665(6) 0.4561(6) 0.0462(17) Uani 1 1 d . . .
H18 H 1.3948 0.4260 0.5111 0.055 Uiso 1 1 calc R . .
C15 C 0.3334(8) 1.1907(6) 0.3009(6) 0.0520(19) Uani 1 1 d . . .
H15 H 0.3120 1.1301 0.2470 0.062 Uiso 1 1 calc R . .
C22 C 1.4697(11) 0.6887(10) 0.1228(6) 0.079(3) Uani 1 1 d . . .
H22 H 1.5479 0.7413 0.1351 0.095 Uiso 1 1 calc R . .
C27 C 1.4642(9) 0.6241(8) -0.1901(6) 0.059(2) Uani 1 1 d . . .
H27 H 1.5631 0.6151 -0.1801 0.071 Uiso 1 1 calc R . .
C24 C 1.2946(12) 0.5565(10) 0.0157(7) 0.086(3) Uani 1 1 d . . .
H24 H 1.2528 0.5189 -0.0451 0.103 Uiso 1 1 calc R . .
C31 C 1.2379(10) 0.6691(10) -0.1334(6) 0.076(3) Uani 1 1 d . . .
H31 H 1.1859 0.6910 -0.0841 0.091 Uiso 1 1 calc R . .
C30 C 1.1724(8) 0.6547(7) -0.2201(5) 0.055(2) Uani 1 1 d . . .
H30 H 1.0744 0.6665 -0.2297 0.066 Uiso 1 1 calc R . .
C10 C 0.6667(8) 1.0913(6) 0.3456(8) 0.066(3) Uani 1 1 d . . .
H10 H 0.7060 1.1544 0.3365 0.079 Uiso 1 1 calc R . .
C12 C 0.9494(12) 1.0834(10) 0.2969(12) 0.119(6) Uani 1 1 d . . .
H12A H 0.8772 1.0967 0.2519 0.178 Uiso 1 1 calc R . .
H12B H 1.0341 1.0591 0.2692 0.178 Uiso 1 1 calc R . .
H12C H 0.9752 1.1508 0.3480 0.178 Uiso 1 1 calc R . .
C23 C 1.4041(9) 0.6368(9) 0.0329(6) 0.069(3) Uani 1 1 d . . .
C11 C 0.7514(8) 1.0020(6) 0.3418(7) 0.062(2) Uani 1 1 d . . .
C26 C 1.3866(9) 0.6506(9) -0.1183(6) 0.065(2) Uani 1 1 d . . .
C13 C 0.2563(9) 0.8985(8) 0.3942(8) 0.075(3) Uani 1 1 d . . .
H13A H 0.2580 0.8384 0.3379 0.112 Uiso 1 1 calc R . .
H13B H 0.1574 0.9108 0.4032 0.112 Uiso 1 1 calc R . .
H13C H 0.3066 0.8802 0.4453 0.112 Uiso 1 1 calc R . .
C5 C 0.9166(14) 0.7175(10) 0.4502(8) 0.097(4) Uani 1 1 d . . .
H5 H 0.9382 0.7065 0.5071 0.117 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 2.224(5) 1_556 ?
Cd1 O4 2.260(5) 2_765 ?
Cd1 N1 2.356(5) . ?
Cd1 N2 2.356(5) . ?
Cd1 O1 2.362(5) . ?
Cd1 O2 2.398(5) . ?
O5 C23 1.357(10) . ?
O5 C26 1.373(10) . ?
O1 C19 1.255(9) . ?
O2 C19 1.251(9) . ?
O3 C32 1.273(8) . ?
O3 Cd1 2.224(5) 1_554 ?
O4 C32 1.242(8) . ?
O4 Cd1 2.260(5) 2_765 ?
O7 C8 1.376(8) . ?
O7 C13 1.386(9) . ?
O6 C11 1.379(9) . ?
O6 C12 1.381(12) . ?
N1 C18 1.320(9) . ?
N1 C17 1.341(10) . ?
N2 C5 1.273(11) . ?
N2 C1 1.352(11) . ?
C3 C4 1.307(12) . ?
C3 C2 1.395(13) . ?
C3 C6 1.488(8) . ?
C2 C1 1.375(10) . ?
C2 H2 0.9300 . ?
C4 C5 1.371(11) . ?
C4 H4 0.9300 . ?
C1 H1 0.9300 . ?
C32 C29 1.495(10) . ?
C7 C6 1.386(10) . ?
C7 C8 1.387(8) . ?
C7 H7 0.9300 . ?
C19 C20 1.509(9) . ?
C8 C9 1.391(10) . ?
C6 C11 1.388(10) . ?
C16 C14 1.376(11) . ?
C16 C18 1.387(9) 1_465 ?
C16 H16 0.9300 . ?
C21 C22 1.365(12) . ?
C21 C20 1.374(11) . ?
C21 H21 0.9300 . ?
C9 C10 1.374(11) . ?
C9 C14 1.494(8) . ?
C14 C15 1.379(10) . ?
C28 C27 1.380(11) . ?
C28 C29 1.396(9) . ?
C28 H28 0.9300 . ?
C25 C20 1.377(11) . ?
C25 C24 1.407(12) . ?
C25 H25 0.9300 . ?
C29 C30 1.378(10) . ?
C17 C15 1.373(9) 1_645 ?
C17 H17 0.9300 . ?
C18 C16 1.387(9) 1_645 ?
C18 H18 0.9300 . ?
C15 C17 1.373(9) 1_465 ?
C15 H15 0.9300 . ?
C22 C23 1.378(12) . ?
C22 H22 0.9300 . ?
C27 C26 1.365(12) . ?
C27 H27 0.9300 . ?
C24 C23 1.357(13) . ?
C24 H24 0.9300 . ?
C31 C30 1.347(11) . ?
C31 C26 1.413(12) . ?
C31 H31 0.9300 . ?
C30 H30 0.9300 . ?
C10 C11 1.394(9) . ?
C10 H10 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C5 H5 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 O4 102.98(19) 1_556 2_765 ?
O3 Cd1 N1 86.9(2) 1_556 . ?
O4 Cd1 N1 80.78(18) 2_765 . ?
O3 Cd1 N2 104.5(2) 1_556 . ?
O4 Cd1 N2 92.42(19) 2_765 . ?
N1 Cd1 N2 167.9(2) . . ?
O3 Cd1 O1 97.44(19) 1_556 . ?
O4 Cd1 O1 158.4(2) 2_765 . ?
N1 Cd1 O1 93.4(2) . . ?
N2 Cd1 O1 89.3(2) . . ?
O3 Cd1 O2 150.5(2) 1_556 . ?
O4 Cd1 O2 103.4(2) 2_765 . ?
N1 Cd1 O2 84.7(2) . . ?
N2 Cd1 O2 87.2(2) . . ?
O1 Cd1 O2 55.09(19) . . ?
C23 O5 C26 121.5(7) . . ?
C19 O1 Cd1 91.7(4) . . ?
C19 O2 Cd1 90.1(5) . . ?
C32 O3 Cd1 118.5(4) . 1_554 ?
C32 O4 Cd1 132.7(4) . 2_765 ?
C8 O7 C13 118.1(5) . . ?
C11 O6 C12 118.8(7) . . ?
C18 N1 C17 117.2(6) . . ?
C18 N1 Cd1 123.4(5) . . ?
C17 N1 Cd1 119.4(4) . . ?
C5 N2 C1 114.9(6) . . ?
C5 N2 Cd1 123.6(6) . . ?
C1 N2 Cd1 121.4(5) . . ?
C4 C3 C2 115.5(7) . . ?
C4 C3 C6 123.6(8) . . ?
C2 C3 C6 120.9(7) . . ?
C1 C2 C3 120.2(9) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C3 C4 C5 121.3(9) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
N2 C1 C2 122.2(9) . . ?
N2 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
O4 C32 O3 124.8(7) . . ?
O4 C32 C29 118.6(6) . . ?
O3 C32 C29 116.6(5) . . ?
C6 C7 C8 120.8(6) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
O2 C19 O1 123.0(7) . . ?
O2 C19 C20 118.7(7) . . ?
O1 C19 C20 118.3(6) . . ?
O7 C8 C7 124.8(6) . . ?
O7 C8 C9 115.5(5) . . ?
C7 C8 C9 119.7(6) . . ?
C7 C6 C11 119.2(6) . . ?
C7 C6 C3 119.3(6) . . ?
C11 C6 C3 121.4(6) . . ?
C14 C16 C18 118.7(7) . 1_465 ?
C14 C16 H16 120.7 . . ?
C18 C16 H16 120.7 1_465 . ?
C22 C21 C20 120.8(8) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C10 C9 C8 119.6(6) . . ?
C10 C9 C14 119.7(6) . . ?
C8 C9 C14 120.6(6) . . ?
C16 C14 C15 117.4(6) . . ?
C16 C14 C9 120.1(6) . . ?
C15 C14 C9 122.4(7) . . ?
C27 C28 C29 121.7(7) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C20 C25 C24 118.5(8) . . ?
C20 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C30 C29 C28 117.5(7) . . ?
C30 C29 C32 120.7(6) . . ?
C28 C29 C32 121.8(6) . . ?
C21 C20 C25 119.7(7) . . ?
C21 C20 C19 120.7(7) . . ?
C25 C20 C19 119.6(7) . . ?
N1 C17 C15 122.3(7) . 1_645 ?
N1 C17 H17 118.8 . . ?
C15 C17 H17 118.8 1_645 . ?
N1 C18 C16 124.0(7) . 1_645 ?
N1 C18 H18 118.0 . . ?
C16 C18 H18 118.0 1_645 . ?
C17 C15 C14 120.4(7) 1_465 . ?
C17 C15 H15 119.8 1_465 . ?
C14 C15 H15 119.8 . . ?
C21 C22 C23 120.6(9) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C26 C27 C28 119.0(7) . . ?
C26 C27 H27 120.5 . . ?
C28 C27 H27 120.5 . . ?
C23 C24 C25 121.3(9) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
C30 C31 C26 119.2(8) . . ?
C30 C31 H31 120.4 . . ?
C26 C31 H31 120.4 . . ?
C31 C30 C29 122.3(7) . . ?
C31 C30 H30 118.8 . . ?
C29 C30 H30 118.8 . . ?
C9 C10 C11 120.8(7) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
O6 C12 H12A 109.5 . . ?
O6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C24 C23 O5 125.8(9) . . ?
C24 C23 C22 118.9(8) . . ?
O5 C23 C22 115.2(8) . . ?
O6 C11 C6 116.4(6) . . ?
O6 C11 C10 123.6(7) . . ?
C6 C11 C10 119.8(7) . . ?
C27 C26 O5 116.8(7) . . ?
C27 C26 C31 120.2(7) . . ?
O5 C26 C31 122.7(8) . . ?
O7 C13 H13A 109.5 . . ?
O7 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O7 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C5 C4 125.8(9) . . ?
N2 C5 H5 117.1 . . ?
C4 C5 H5 117.1 . . ?

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
O3 Cd1 O1 C19 170.5(4) 1_556 . . . ?
O4 Cd1 O1 C19 9.7(7) 2_765 . . . ?
N1 Cd1 O1 C19 83.2(4) . . . . ?
N2 Cd1 O1 C19 -85.0(4) . . . . ?
O2 Cd1 O1 C19 2.0(4) . . . . ?
O3 Cd1 O2 C19 -25.9(6) 1_556 . . . ?
O4 Cd1 O2 C19 -179.2(4) 2_765 . . . ?
N1 Cd1 O2 C19 -100.0(4) . . . . ?
N2 Cd1 O2 C19 89.0(4) . . . . ?
O1 Cd1 O2 C19 -2.1(4) . . . . ?
O3 Cd1 N1 C18 -4.5(5) 1_556 . . . ?
O4 Cd1 N1 C18 -108.2(6) 2_765 . . . ?
N2 Cd1 N1 C18 -164.6(9) . . . . ?
O1 Cd1 N1 C18 92.8(6) . . . . ?
O2 Cd1 N1 C18 147.2(6) . . . . ?
O3 Cd1 N1 C17 172.7(6) 1_556 . . . ?
O4 Cd1 N1 C17 69.1(6) 2_765 . . . ?
N2 Cd1 N1 C17 12.7(13) . . . . ?
O1 Cd1 N1 C17 -90.0(6) . . . . ?
O2 Cd1 N1 C17 -35.5(6) . . . . ?
O3 Cd1 N2 C5 -23.4(9) 1_556 . . . ?
O4 Cd1 N2 C5 80.6(9) 2_765 . . . ?
N1 Cd1 N2 C5 136.0(12) . . . . ?
O1 Cd1 N2 C5 -120.9(9) . . . . ?
O2 Cd1 N2 C5 -176.0(9) . . . . ?
O3 Cd1 N2 C1 152.1(7) 1_556 . . . ?
O4 Cd1 N2 C1 -103.8(7) 2_765 . . . ?
N1 Cd1 N2 C1 -48.4(13) . . . . ?
O1 Cd1 N2 C1 54.6(7) . . . . ?
O2 Cd1 N2 C1 -0.5(7) . . . . ?
C4 C3 C2 C1 -0.4(16) . . . . ?
C6 C3 C2 C1 178.2(9) . . . . ?
C2 C3 C4 C5 -0.7(18) . . . . ?
C6 C3 C4 C5 -179.2(10) . . . . ?
C5 N2 C1 C2 2.3(16) . . . . ?
Cd1 N2 C1 C2 -173.7(9) . . . . ?
C3 C2 C1 N2 -0.4(17) . . . . ?
Cd1 O4 C32 O3 111.0(7) 2_765 . . . ?
Cd1 O4 C32 C29 -71.0(8) 2_765 . . . ?
Cd1 O3 C32 O4 -16.3(8) 1_554 . . . ?
Cd1 O3 C32 C29 165.7(4) 1_554 . . . ?
Cd1 O2 C19 O1 3.8(7) . . . . ?
Cd1 O2 C19 C20 -175.5(6) . . . . ?
Cd1 O1 C19 O2 -3.8(7) . . . . ?
Cd1 O1 C19 C20 175.5(6) . . . . ?
C13 O7 C8 C7 -5.3(12) . . . . ?
C13 O7 C8 C9 173.7(8) . . . . ?
C6 C7 C8 O7 176.7(7) . . . . ?
C6 C7 C8 C9 -2.2(11) . . . . ?
C8 C7 C6 C11 -0.6(12) . . . . ?
C8 C7 C6 C3 175.2(7) . . . . ?
C4 C3 C6 C7 -65.6(13) . . . . ?
C2 C3 C6 C7 116.0(10) . . . . ?
C4 C3 C6 C11 110.1(12) . . . . ?
C2 C3 C6 C11 -68.3(12) . . . . ?
O7 C8 C9 C10 -176.8(8) . . . . ?
C7 C8 C9 C10 2.2(12) . . . . ?
O7 C8 C9 C14 6.6(10) . . . . ?
C7 C8 C9 C14 -174.3(7) . . . . ?
C18 C16 C14 C15 -0.1(11) 1_465 . . . ?
C18 C16 C14 C9 -179.1(7) 1_465 . . . ?
C10 C9 C14 C16 -77.1(11) . . . . ?
C8 C9 C14 C16 99.4(9) . . . . ?
C10 C9 C14 C15 103.9(10) . . . . ?
C8 C9 C14 C15 -79.6(10) . . . . ?
C27 C28 C29 C30 3.2(12) . . . . ?
C27 C28 C29 C32 -177.0(7) . . . . ?
O4 C32 C29 C30 -10.4(10) . . . . ?
O3 C32 C29 C30 167.7(7) . . . . ?
O4 C32 C29 C28 169.7(7) . . . . ?
O3 C32 C29 C28 -12.1(10) . . . . ?
C22 C21 C20 C25 1.4(16) . . . . ?
C22 C21 C20 C19 -178.8(9) . . . . ?
C24 C25 C20 C21 -1.7(15) . . . . ?
C24 C25 C20 C19 178.5(9) . . . . ?
O2 C19 C20 C21 -176.5(8) . . . . ?
O1 C19 C20 C21 4.2(12) . . . . ?
O2 C19 C20 C25 3.3(11) . . . . ?
O1 C19 C20 C25 -176.0(8) . . . . ?
C18 N1 C17 C15 -0.3(11) . . . 1_645 ?
Cd1 N1 C17 C15 -177.7(6) . . . 1_645 ?
C17 N1 C18 C16 2.6(11) . . . 1_645 ?
Cd1 N1 C18 C16 179.9(6) . . . 1_645 ?
C16 C14 C15 C17 2.2(12) . . . 1_465 ?
C9 C14 C15 C17 -178.8(8) . . . 1_465 ?
C20 C21 C22 C23 1.0(18) . . . . ?
C29 C28 C27 C26 -0.4(14) . . . . ?
C20 C25 C24 C23 -0.4(18) . . . . ?
C26 C31 C30 C29 -0.4(16) . . . . ?
C28 C29 C30 C31 -2.7(13) . . . . ?
C32 C29 C30 C31 177.5(8) . . . . ?
C8 C9 C10 C11 0.6(15) . . . . ?
C14 C9 C10 C11 177.2(9) . . . . ?
C25 C24 C23 O5 178.9(10) . . . . ?
C25 C24 C23 C22 2.8(18) . . . . ?
C26 O5 C23 C24 23.4(18) . . . . ?
C26 O5 C23 C22 -160.4(11) . . . . ?
C21 C22 C23 C24 -3.1(18) . . . . ?
C21 C22 C23 O5 -179.6(11) . . . . ?
C12 O6 C11 C6 171.2(11) . . . . ?
C12 O6 C11 C10 -14.0(18) . . . . ?
C7 C6 C11 O6 178.4(9) . . . . ?
C3 C6 C11 O6 2.6(14) . . . . ?
C7 C6 C11 C10 3.4(14) . . . . ?
C3 C6 C11 C10 -172.3(9) . . . . ?
C9 C10 C11 O6 -178.0(10) . . . . ?
C9 C10 C11 C6 -3.4(16) . . . . ?
C28 C27 C26 O5 -177.0(8) . . . . ?
C28 C27 C26 C31 -2.9(15) . . . . ?
C23 O5 C26 C27 -144.1(10) . . . . ?
C23 O5 C26 C31 41.9(16) . . . . ?
C30 C31 C26 C27 3.3(16) . . . . ?
C30 C31 C26 O5 177.1(9) . . . . ?
C1 N2 C5 C4 -3.6(19) . . . . ?
Cd1 N2 C5 C4 172.3(11) . . . . ?
C3 C4 C5 N2 3(2) . . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.013 0.000 0.000 473 97 ' '
_platon_squeeze_details          
; 
;
_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         2.130
_refine_diff_density_min         -2.467
_refine_diff_density_rms         0.174
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1001548'
_audit_update_record             
;
2014-05-07 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H31 N3 Ni O9'
_chemical_formula_weight         696.34

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'

_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                   11.5007(11)
_cell_length_b                   11.7623(11)
_cell_length_c                   13.8198(13)
_cell_angle_alpha                70.8350(10)
_cell_angle_beta                 65.6940(10)
_cell_angle_gamma                76.9930(10)
_cell_volume                     1600.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5437
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      27.45

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      1.445
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             724
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8147
_exptl_absorpt_correction_T_max  0.8455
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12668
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         26.37
_reflns_number_total             6421
_reflns_number_gt                5306
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.1110P)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         6421
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1642
_refine_ls_wR_factor_gt          0.1559
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.002
_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 0.33845(3) 0.36300(3) 0.45094(3) 0.01503(14) Uani 1 1 d . . .
O1 O 0.36694(19) 0.19241(18) 0.40268(17) 0.0222(4) Uani 1 1 d . . .
O2 O 0.24997(18) 0.35949(18) 0.35047(17) 0.0210(4) Uani 1 1 d . . .
O3 O 0.20083(17) 0.28403(17) -0.39661(16) 0.0188(4) Uani 1 1 d . . .
O4 O 0.39428(18) 0.30363(19) -0.41441(16) 0.0224(4) Uani 1 1 d . . .
O9 O 0.1804(2) 0.90262(18) 0.59724(19) 0.0262(5) Uani 1 1 d . . .
O5 O 0.1529(2) 0.0476(2) 0.10091(18) 0.0299(5) Uani 1 1 d . . .
O8 O 0.81059(19) 0.4360(2) -0.04121(18) 0.0312(5) Uani 1 1 d . . .
N2 N 0.2643(2) 0.5341(2) 0.4671(2) 0.0183(5) Uani 1 1 d . . .
N1 N 0.5091(2) 0.4100(2) 0.33041(19) 0.0171(5) Uani 1 1 d . . .
C11 C 0.2514(3) 0.2114(3) -0.2347(2) 0.0201(6) Uani 1 1 d . . .
C14 C 0.2846(2) 0.2688(2) -0.3546(2) 0.0180(6) Uani 1 1 d . . .
C19 C 0.1374(2) 0.7645(2) 0.4864(2) 0.0169(6) Uani 1 1 d . . .
C1 C 0.2939(3) 0.2497(3) 0.3508(2) 0.0187(6) Uani 1 1 d . . .
C12 C 0.1310(3) 0.1723(3) -0.1705(2) 0.0222(6) Uani 1 1 d . . .
H12 H 0.0724 0.1799 -0.2033 0.027 Uiso 1 1 calc R . .
C2 C 0.2568(3) 0.1923(3) 0.2872(2) 0.0218(6) Uani 1 1 d . . .
C25 C 0.6159(3) 0.3413(3) 0.3395(2) 0.0205(6) Uani 1 1 d . . .
H25 H 0.6083 0.2758 0.4011 0.025 Uiso 1 1 calc R . .
C21 C -0.0243(2) 0.9323(2) 0.4468(2) 0.0177(6) Uani 1 1 d . . .
H21 H -0.0414 0.8865 0.4115 0.021 Uiso 1 1 calc R . .
C30 C 0.9696(3) 0.5143(3) 0.1034(2) 0.0213(6) Uani 1 1 d . . .
H30 H 0.9490 0.5250 0.1726 0.026 Uiso 1 1 calc R . .
C9 C 0.3056(3) 0.1469(3) -0.0723(3) 0.0260(7) Uani 1 1 d . . .
H9 H 0.3638 0.1390 -0.0390 0.031 Uiso 1 1 calc R . .
C20 C 0.0678(3) 0.8861(2) 0.4942(2) 0.0173(6) Uani 1 1 d . . .
C18 C 0.2699(3) 0.7410(2) 0.4545(2) 0.0184(6) Uani 1 1 d . . .
H18 H 0.3189 0.8024 0.4386 0.022 Uiso 1 1 calc R . .
C22 C 0.0914(3) 0.9542(3) 0.5490(2) 0.0187(6) Uani 1 1 d . . .
C29 C 0.8774(3) 0.4816(3) 0.0801(2) 0.0200(6) Uani 1 1 d . . .
C24 C 0.5215(3) 0.5042(3) 0.2408(2) 0.0193(6) Uani 1 1 d . . .
H24 H 0.4482 0.5536 0.2342 0.023 Uiso 1 1 calc R . .
C10 C 0.3391(3) 0.1982(3) -0.1854(2) 0.0240(6) Uani 1 1 d . . .
H10 H 0.4203 0.2237 -0.2280 0.029 Uiso 1 1 calc R . .
C15 C 0.3293(2) 0.6261(3) 0.4465(2) 0.0184(6) Uani 1 1 d . . .
H15 H 0.4180 0.6123 0.4258 0.022 Uiso 1 1 calc R . .
C16 C 0.1352(3) 0.5566(3) 0.5005(3) 0.0263(7) Uani 1 1 d . . .
H16 H 0.0879 0.4931 0.5185 0.032 Uiso 1 1 calc R . .
C27 C 0.6383(3) 0.5303(3) 0.1585(2) 0.0198(6) Uani 1 1 d . . .
H27 H 0.6431 0.5957 0.0972 0.024 Uiso 1 1 calc R . .
C4 C 0.3036(3) 0.0758(3) 0.2788(2) 0.0240(6) Uani 1 1 d . . .
H4 H 0.3577 0.0297 0.3154 0.029 Uiso 1 1 calc R . .
C26 C 0.7370(3) 0.3633(3) 0.2612(2) 0.0206(6) Uani 1 1 d . . .
H26 H 0.8092 0.3149 0.2715 0.025 Uiso 1 1 calc R . .
C8 C 0.1862(3) 0.1080(3) -0.0104(2) 0.0241(6) Uani 1 1 d . . .
C28 C 0.7494(3) 0.4583(3) 0.1674(2) 0.0200(6) Uani 1 1 d . . .
C13 C 0.0972(3) 0.1221(3) -0.0581(3) 0.0251(6) Uani 1 1 d . . .
H13 H 0.0156 0.0981 -0.0150 0.030 Uiso 1 1 calc R . .
C5 C 0.2701(3) 0.0266(3) 0.2154(3) 0.0273(7) Uani 1 1 d . . .
H5 H 0.3017 -0.0518 0.2094 0.033 Uiso 1 1 calc R . .
C7 C 0.1897(3) 0.0966(3) 0.1621(2) 0.0250(6) Uani 1 1 d . . .
C3 C 0.1723(3) 0.2594(3) 0.2343(3) 0.0301(7) Uani 1 1 d . . .
H3 H 0.1377 0.3368 0.2422 0.036 Uiso 1 1 calc R . .
C17 C 0.0705(3) 0.6677(3) 0.5091(3) 0.0253(7) Uani 1 1 d . . .
H17 H -0.0183 0.6788 0.5302 0.030 Uiso 1 1 calc R . .
C32 C 0.8421(3) 0.4007(3) -0.1398(3) 0.0297(7) Uani 1 1 d . . .
H32A H 0.8696 0.4683 -0.2027 0.044 Uiso 1 1 calc R . .
H32B H 0.7679 0.3745 -0.1382 0.044 Uiso 1 1 calc R . .
H32C H 0.9100 0.3355 -0.1445 0.044 Uiso 1 1 calc R . .
C31 C 0.9074(3) 0.4685(3) -0.0250(2) 0.0217(6) Uani 1 1 d . . .
C23 C 0.2004(3) 0.9696(3) 0.6573(3) 0.0321(8) Uani 1 1 d . . .
H23A H 0.2289 1.0461 0.6089 0.048 Uiso 1 1 calc R . .
H23B H 0.2643 0.9249 0.6872 0.048 Uiso 1 1 calc R . .
H23C H 0.1214 0.9828 0.7161 0.048 Uiso 1 1 calc R . .
C6 C 0.1398(3) 0.2124(3) 0.1708(3) 0.0320(7) Uani 1 1 d . . .
H6 H 0.0853 0.2581 0.1344 0.038 Uiso 1 1 calc R . .
O6 O 0.5738(2) 0.2341(2) -0.1062(2) 0.0362(6) Uani 1 1 d . . .
N6 N 0.5890(3) 0.2254(2) 0.0550(2) 0.0305(6) Uani 1 1 d . . .
C35 C 0.6102(3) 0.1841(3) -0.0297(3) 0.0345(8) Uani 1 1 d . . .
H35 H 0.6579 0.1091 -0.0309 0.041 Uiso 1 1 calc R . .
C33 C 0.5164(3) 0.3435(3) 0.0620(3) 0.0370(8) Uani 1 1 d . . .
H33A H 0.5740 0.4013 0.0443 0.055 Uiso 1 1 calc R . .
H33B H 0.4546 0.3374 0.1355 0.055 Uiso 1 1 calc R . .
H33C H 0.4729 0.3692 0.0110 0.055 Uiso 1 1 calc R . .
O1W O 0.5152(6) 0.0521(5) 0.5503(6) 0.150(2) Uani 1 1 d . . .
C34 C 0.6430(4) 0.1621(3) 0.1401(3) 0.0392(8) Uani 1 1 d . . .
H34A H 0.6902 0.0871 0.1259 0.059 Uiso 1 1 calc R . .
H34B H 0.5748 0.1459 0.2109 0.059 Uiso 1 1 calc R . .
H34C H 0.6994 0.2116 0.1395 0.059 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 N1 2.031(2) . ?
Ni1 O2 2.0457(19) . ?
Ni1 N2 2.048(2) . ?
Ni1 O4 2.072(2) 1_556 ?
Ni1 O3 2.107(2) 1_556 ?
Ni1 O1 2.232(2) . ?
Ni1 C14 2.412(3) 1_556 ?
O1 C1 1.264(3) . ?
O2 C1 1.275(3) . ?
O3 C14 1.269(3) . ?
O3 Ni1 2.107(2) 1_554 ?
O4 C14 1.263(3) . ?
O4 Ni1 2.072(2) 1_554 ?
O9 C22 1.370(3) . ?
O9 C23 1.424(3) . ?
O5 C8 1.392(4) . ?
O5 C7 1.396(3) . ?
O8 C31 1.375(3) . ?
O8 C32 1.434(4) . ?
N2 C15 1.340(4) . ?
N2 C16 1.352(3) . ?
N1 C25 1.338(3) . ?
N1 C24 1.343(4) . ?
C11 C12 1.387(4) . ?
C11 C10 1.390(4) . ?
C11 C14 1.486(4) . ?
C14 Ni1 2.412(3) 1_554 ?
C19 C18 1.389(4) . ?
C19 C17 1.396(4) . ?
C19 C20 1.487(4) . ?
C1 C2 1.496(4) . ?
C12 C13 1.385(4) . ?
C12 H12 0.9300 . ?
C2 C4 1.379(4) . ?
C2 C3 1.401(4) . ?
C25 C26 1.385(4) . ?
C25 H25 0.9300 . ?
C21 C20 1.388(4) . ?
C21 C22 1.390(4) 2_576 ?
C21 H21 0.9300 . ?
C30 C29 1.387(4) . ?
C30 C31 1.392(4) 2_765 ?
C30 H30 0.9300 . ?
C9 C8 1.373(4) . ?
C9 C10 1.395(4) . ?
C9 H9 0.9300 . ?
C20 C22 1.398(4) . ?
C18 C15 1.388(4) . ?
C18 H18 0.9300 . ?
C22 C21 1.390(4) 2_576 ?
C29 C31 1.402(4) . ?
C29 C28 1.483(4) . ?
C24 C27 1.376(4) . ?
C24 H24 0.9300 . ?
C10 H10 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.366(4) . ?
C16 H16 0.9300 . ?
C27 C28 1.393(4) . ?
C27 H27 0.9300 . ?
C4 C5 1.401(4) . ?
C4 H4 0.9300 . ?
C26 C28 1.385(4) . ?
C26 H26 0.9300 . ?
C8 C13 1.385(4) . ?
C13 H13 0.9300 . ?
C5 C7 1.377(4) . ?
C5 H5 0.9300 . ?
C7 C6 1.378(5) . ?
C3 C6 1.377(4) . ?
C3 H3 0.9300 . ?
C17 H17 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C31 C30 1.392(4) 2_765 ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C6 H6 0.9300 . ?
O6 C35 1.219(4) . ?
N6 C35 1.323(4) . ?
N6 C33 1.461(4) . ?
N6 C34 1.464(4) . ?
C35 H35 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

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 Ni1 O2 96.99(9) . . ?
N1 Ni1 N2 96.12(9) . . ?
O2 Ni1 N2 96.93(8) . . ?
N1 Ni1 O4 99.19(8) . 1_556 ?
O2 Ni1 O4 157.24(9) . 1_556 ?
N2 Ni1 O4 97.15(9) . 1_556 ?
N1 Ni1 O3 161.57(8) . 1_556 ?
O2 Ni1 O3 98.43(8) . 1_556 ?
N2 Ni1 O3 91.98(9) . 1_556 ?
O4 Ni1 O3 63.29(7) 1_556 1_556 ?
N1 Ni1 O1 89.86(8) . . ?
O2 Ni1 O1 61.94(7) . . ?
N2 Ni1 O1 158.66(8) . . ?
O4 Ni1 O1 102.10(8) 1_556 . ?
O3 Ni1 O1 88.53(8) 1_556 . ?
N1 Ni1 C14 130.53(9) . 1_556 ?
O2 Ni1 C14 128.90(9) . 1_556 ?
N2 Ni1 C14 95.52(9) . 1_556 ?
O4 Ni1 C14 31.58(8) 1_556 1_556 ?
O3 Ni1 C14 31.72(8) 1_556 1_556 ?
O1 Ni1 C14 96.07(8) . 1_556 ?
C1 O1 Ni1 84.68(16) . . ?
C1 O2 Ni1 92.69(16) . . ?
C14 O3 Ni1 87.52(16) . 1_554 ?
C14 O4 Ni1 89.25(16) . 1_554 ?
C22 O9 C23 116.8(2) . . ?
C8 O5 C7 115.6(2) . . ?
C31 O8 C32 118.0(2) . . ?
C15 N2 C16 116.8(2) . . ?
C15 N2 Ni1 127.41(18) . . ?
C16 N2 Ni1 115.80(18) . . ?
C25 N1 C24 117.8(2) . . ?
C25 N1 Ni1 117.93(19) . . ?
C24 N1 Ni1 124.20(17) . . ?
C12 C11 C10 119.4(3) . . ?
C12 C11 C14 119.9(2) . . ?
C10 C11 C14 120.7(3) . . ?
O4 C14 O3 119.9(3) . . ?
O4 C14 C11 120.7(2) . . ?
O3 C14 C11 119.4(2) . . ?
O4 C14 Ni1 59.18(15) . 1_554 ?
O3 C14 Ni1 60.76(15) . 1_554 ?
C11 C14 Ni1 179.7(2) . 1_554 ?
C18 C19 C17 116.6(2) . . ?
C18 C19 C20 123.0(2) . . ?
C17 C19 C20 120.4(2) . . ?
O1 C1 O2 120.7(2) . . ?
O1 C1 C2 121.6(2) . . ?
O2 C1 C2 117.7(2) . . ?
C13 C12 C11 120.6(3) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C4 C2 C3 119.2(3) . . ?
C4 C2 C1 122.0(3) . . ?
C3 C2 C1 118.8(3) . . ?
N1 C25 C26 122.9(3) . . ?
N1 C25 H25 118.5 . . ?
C26 C25 H25 118.5 . . ?
C20 C21 C22 121.1(3) . 2_576 ?
C20 C21 H21 119.4 . . ?
C22 C21 H21 119.4 2_576 . ?
C29 C30 C31 121.1(3) . 2_765 ?
C29 C30 H30 119.4 . . ?
C31 C30 H30 119.4 2_765 . ?
C8 C9 C10 119.6(3) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C21 C20 C22 119.2(2) . . ?
C21 C20 C19 118.8(2) . . ?
C22 C20 C19 121.9(2) . . ?
C15 C18 C19 120.2(3) . . ?
C15 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
O9 C22 C21 123.6(2) . 2_576 ?
O9 C22 C20 116.7(2) . . ?
C21 C22 C20 119.6(2) 2_576 . ?
C30 C29 C31 119.5(3) . . ?
C30 C29 C28 119.6(3) . . ?
C31 C29 C28 120.9(3) . . ?
N1 C24 C27 122.6(2) . . ?
N1 C24 H24 118.7 . . ?
C27 C24 H24 118.7 . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
N2 C15 C18 122.9(2) . . ?
N2 C15 H15 118.6 . . ?
C18 C15 H15 118.6 . . ?
N2 C16 C17 123.5(3) . . ?
N2 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C24 C27 C28 119.6(3) . . ?
C24 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C2 C4 C5 120.4(3) . . ?
C2 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C25 C26 C28 119.2(2) . . ?
C25 C26 H26 120.4 . . ?
C28 C26 H26 120.4 . . ?
C9 C8 C13 120.9(3) . . ?
C9 C8 O5 121.3(3) . . ?
C13 C8 O5 117.7(3) . . ?
C26 C28 C27 117.8(3) . . ?
C26 C28 C29 120.5(2) . . ?
C27 C28 C29 121.7(3) . . ?
C8 C13 C12 119.3(3) . . ?
C8 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C7 C5 C4 118.8(3) . . ?
C7 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C7 C6 122.0(3) . . ?
C5 C7 O5 119.3(3) . . ?
C6 C7 O5 118.6(3) . . ?
C6 C3 C2 120.9(3) . . ?
C6 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C16 C17 C19 120.1(3) . . ?
C16 C17 H17 120.0 . . ?
C19 C17 H17 120.0 . . ?
O8 C32 H32A 109.5 . . ?
O8 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O8 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O8 C31 C30 124.9(3) . 2_765 ?
O8 C31 C29 115.7(3) . . ?
C30 C31 C29 119.4(3) 2_765 . ?
O9 C23 H23A 109.5 . . ?
O9 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O9 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C3 C6 C7 118.8(3) . . ?
C3 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C35 N6 C33 119.8(3) . . ?
C35 N6 C34 123.0(3) . . ?
C33 N6 C34 117.0(3) . . ?
O6 C35 N6 126.8(3) . . ?
O6 C35 H35 116.6 . . ?
N6 C35 H35 116.6 . . ?
N6 C33 H33A 109.5 . . ?
N6 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N6 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N6 C34 H34A 109.5 . . ?
N6 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N6 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 O1 C1 -98.77(17) . . . . ?
O2 Ni1 O1 C1 -0.77(16) . . . . ?
N2 Ni1 O1 C1 7.9(3) . . . . ?
O4 Ni1 O1 C1 161.86(16) 1_556 . . . ?
O3 Ni1 O1 C1 99.59(16) 1_556 . . . ?
C14 Ni1 O1 C1 130.44(17) 1_556 . . . ?
N1 Ni1 O2 C1 86.86(17) . . . . ?
N2 Ni1 O2 C1 -176.07(17) . . . . ?
O4 Ni1 O2 C1 -48.2(3) 1_556 . . . ?
O3 Ni1 O2 C1 -83.02(17) 1_556 . . . ?
O1 Ni1 O2 C1 0.76(16) . . . . ?
C14 Ni1 O2 C1 -73.20(19) 1_556 . . . ?
N1 Ni1 N2 C15 -27.8(2) . . . . ?
O2 Ni1 N2 C15 -125.6(2) . . . . ?
O4 Ni1 N2 C15 72.3(2) 1_556 . . . ?
O3 Ni1 N2 C15 135.6(2) 1_556 . . . ?
O1 Ni1 N2 C15 -133.3(2) . . . . ?
C14 Ni1 N2 C15 104.0(2) 1_556 . . . ?
N1 Ni1 N2 C16 150.9(2) . . . . ?
O2 Ni1 N2 C16 53.0(2) . . . . ?
O4 Ni1 N2 C16 -109.0(2) 1_556 . . . ?
O3 Ni1 N2 C16 -45.7(2) 1_556 . . . ?
O1 Ni1 N2 C16 45.3(4) . . . . ?
C14 Ni1 N2 C16 -77.3(2) 1_556 . . . ?
O2 Ni1 N1 C25 -127.1(2) . . . . ?
N2 Ni1 N1 C25 135.1(2) . . . . ?
O4 Ni1 N1 C25 36.8(2) 1_556 . . . ?
O3 Ni1 N1 C25 19.5(4) 1_556 . . . ?
O1 Ni1 N1 C25 -65.4(2) . . . . ?
C14 Ni1 N1 C25 32.5(3) 1_556 . . . ?
O2 Ni1 N1 C24 51.3(2) . . . . ?
N2 Ni1 N1 C24 -46.5(2) . . . . ?
O4 Ni1 N1 C24 -144.8(2) 1_556 . . . ?
O3 Ni1 N1 C24 -162.1(2) 1_556 . . . ?
O1 Ni1 N1 C24 113.0(2) . . . . ?
C14 Ni1 N1 C24 -149.1(2) 1_556 . . . ?
Ni1 O4 C14 O3 -0.5(3) 1_554 . . . ?
Ni1 O4 C14 C11 -179.7(2) 1_554 . . . ?
Ni1 O3 C14 O4 0.5(3) 1_554 . . . ?
Ni1 O3 C14 C11 179.7(2) 1_554 . . . ?
C12 C11 C14 O4 -179.2(3) . . . . ?
C10 C11 C14 O4 1.9(4) . . . . ?
C12 C11 C14 O3 1.6(4) . . . . ?
C10 C11 C14 O3 -177.2(3) . . . . ?
C12 C11 C14 Ni1 115(38) . . . 1_554 ?
C10 C11 C14 Ni1 -63(38) . . . 1_554 ?
Ni1 O1 C1 O2 1.3(3) . . . . ?
Ni1 O1 C1 C2 -179.2(3) . . . . ?
Ni1 O2 C1 O1 -1.4(3) . . . . ?
Ni1 O2 C1 C2 179.1(2) . . . . ?
C10 C11 C12 C13 0.9(4) . . . . ?
C14 C11 C12 C13 -178.0(3) . . . . ?
O1 C1 C2 C4 -2.3(4) . . . . ?
O2 C1 C2 C4 177.2(3) . . . . ?
O1 C1 C2 C3 178.0(3) . . . . ?
O2 C1 C2 C3 -2.5(4) . . . . ?
C24 N1 C25 C26 0.1(4) . . . . ?
Ni1 N1 C25 C26 178.6(2) . . . . ?
C22 C21 C20 C22 1.3(5) 2_576 . . . ?
C22 C21 C20 C19 -179.5(3) 2_576 . . . ?
C18 C19 C20 C21 132.4(3) . . . . ?
C17 C19 C20 C21 -46.1(4) . . . . ?
C18 C19 C20 C22 -48.5(4) . . . . ?
C17 C19 C20 C22 133.0(3) . . . . ?
C17 C19 C18 C15 0.1(4) . . . . ?
C20 C19 C18 C15 -178.5(3) . . . . ?
C23 O9 C22 C21 2.0(4) . . . 2_576 ?
C23 O9 C22 C20 -177.3(3) . . . . ?
C21 C20 C22 O9 178.0(3) . . . . ?
C19 C20 C22 O9 -1.1(4) . . . . ?
C21 C20 C22 C21 -1.3(5) . . . 2_576 ?
C19 C20 C22 C21 179.6(3) . . . 2_576 ?
C31 C30 C29 C31 -1.6(5) 2_765 . . . ?
C31 C30 C29 C28 177.0(3) 2_765 . . . ?
C25 N1 C24 C27 1.2(4) . . . . ?
Ni1 N1 C24 C27 -177.2(2) . . . . ?
C12 C11 C10 C9 -0.4(4) . . . . ?
C14 C11 C10 C9 178.4(3) . . . . ?
C8 C9 C10 C11 0.9(5) . . . . ?
C16 N2 C15 C18 -2.2(4) . . . . ?
Ni1 N2 C15 C18 176.5(2) . . . . ?
C19 C18 C15 N2 0.8(4) . . . . ?
C15 N2 C16 C17 2.9(5) . . . . ?
Ni1 N2 C16 C17 -175.9(3) . . . . ?
N1 C24 C27 C28 -0.8(4) . . . . ?
C3 C2 C4 C5 1.9(5) . . . . ?
C1 C2 C4 C5 -177.8(3) . . . . ?
N1 C25 C26 C28 -1.9(4) . . . . ?
C10 C9 C8 C13 -1.8(5) . . . . ?
C10 C9 C8 O5 174.8(3) . . . . ?
C7 O5 C8 C9 43.8(4) . . . . ?
C7 O5 C8 C13 -139.4(3) . . . . ?
C25 C26 C28 C27 2.3(4) . . . . ?
C25 C26 C28 C29 -177.8(3) . . . . ?
C24 C27 C28 C26 -1.0(4) . . . . ?
C24 C27 C28 C29 179.1(3) . . . . ?
C30 C29 C28 C26 -63.9(4) . . . . ?
C31 C29 C28 C26 114.7(3) . . . . ?
C30 C29 C28 C27 116.0(3) . . . . ?
C31 C29 C28 C27 -65.4(4) . . . . ?
C9 C8 C13 C12 2.3(5) . . . . ?
O5 C8 C13 C12 -174.5(3) . . . . ?
C11 C12 C13 C8 -1.8(5) . . . . ?
C2 C4 C5 C7 -0.1(5) . . . . ?
C4 C5 C7 C6 -1.0(5) . . . . ?
C4 C5 C7 O5 -178.4(3) . . . . ?
C8 O5 C7 C5 -120.4(3) . . . . ?
C8 O5 C7 C6 62.2(4) . . . . ?
C4 C2 C3 C6 -2.6(5) . . . . ?
C1 C2 C3 C6 177.1(3) . . . . ?
N2 C16 C17 C19 -2.2(5) . . . . ?
C18 C19 C17 C16 0.6(4) . . . . ?
C20 C19 C17 C16 179.2(3) . . . . ?
C32 O8 C31 C30 9.1(4) . . . 2_765 ?
C32 O8 C31 C29 -169.3(3) . . . . ?
C30 C29 C31 O8 -180.0(3) . . . . ?
C28 C29 C31 O8 1.4(4) . . . . ?
C30 C29 C31 C30 1.5(5) . . . 2_765 ?
C28 C29 C31 C30 -177.0(3) . . . 2_765 ?
C2 C3 C6 C7 1.5(5) . . . . ?
C5 C7 C6 C3 0.3(5) . . . . ?
O5 C7 C6 C3 177.7(3) . . . . ?
C33 N6 C35 O6 -0.9(6) . . . . ?
C34 N6 C35 O6 -176.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.955
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.107
