# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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 1584238'
_audit_update_record             
;
2017-11-06 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H12 N2 O3'
_chemical_formula_weight         340.33

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'

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

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

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

_cell_length_a                   28.212(6)
_cell_length_b                   7.6096(17)
_cell_length_c                   14.583(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.955(4)
_cell_angle_gamma                90
_cell_volume                     2994.5(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    803
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      26.12

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_F_000             1408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.103
_shelx_estimated_absorpt_T_min   0.950
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8068
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 Sheldrick, G.M. SADABS: Program for absorption correction
 using area detector data. University of Göttingen, Germany, 1996.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10293
_diffrn_reflns_av_unetI/netI     0.1228
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.509
_diffrn_reflns_theta_max         26.408
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3061
_reflns_number_gt                1219
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BRUKER Smart'
_computing_cell_refinement       'BRUKER Smart'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0327P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00112(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3061
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1015
_refine_ls_wR_factor_gt          0.0742
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_restrained_S_all      0.846
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.04349(6) 0.1829(3) 0.83673(13) 0.0444(6) Uani 1 1 d . . . . .
O2 O 0.10702(7) 0.5146(3) 1.17548(14) 0.0527(6) Uani 1 1 d . . . . .
O3 O -0.18797(8) 0.0151(3) 0.90889(16) 0.0583(7) Uani 1 1 d . . . . .
N1 N -0.04749(8) 0.1161(3) 0.87163(17) 0.0325(6) Uani 1 1 d . . . . .
N2 N -0.09545(8) 0.1244(3) 0.96936(16) 0.0359(6) Uani 1 1 d . . . . .
C1 C 0.05934(10) 0.2542(3) 0.91555(19) 0.0335(7) Uani 1 1 d . . . . .
C2 C 0.10988(9) 0.3286(4) 0.94916(19) 0.0334(7) Uani 1 1 d . . . . .
C3 C 0.14113(10) 0.3137(4) 0.8914(2) 0.0442(8) Uani 1 1 d . . . . .
H3 H 0.1297 0.2627 0.8310 0.053 Uiso 1 1 calc R U . . .
C4 C 0.18901(11) 0.3746(4) 0.9238(2) 0.0536(9) Uani 1 1 d . . . . .
H4 H 0.2102 0.3621 0.8859 0.064 Uiso 1 1 calc R U . . .
C5 C 0.20582(11) 0.4548(4) 1.0130(2) 0.0554(9) Uani 1 1 d . . . . .
H5 H 0.2383 0.4955 1.0347 0.067 Uiso 1 1 calc R U . . .
C6 C 0.17463(11) 0.4741(4) 1.0692(2) 0.0470(8) Uani 1 1 d . . . . .
H6 H 0.1859 0.5299 1.1284 0.056 Uiso 1 1 calc R U . . .
C7 C 0.12648(10) 0.4109(4) 1.03831(19) 0.0344(7) Uani 1 1 d . . . . .
C8 C 0.09374(10) 0.4306(4) 1.10071(19) 0.0355(7) Uani 1 1 d . . . . .
C9 C 0.04413(10) 0.3475(3) 1.06972(19) 0.0313(7) Uani 1 1 d . . . . .
C10 C 0.01335(10) 0.3558(4) 1.12940(19) 0.0392(8) Uani 1 1 d . . . . .
H10 H 0.0249 0.4118 1.1884 0.047 Uiso 1 1 calc R U . . .
C11 C -0.03357(10) 0.2837(4) 1.10343(19) 0.0398(8) Uani 1 1 d . . . . .
H11 H -0.0533 0.2884 1.1444 0.048 Uiso 1 1 calc R U . . .
C12 C -0.05028(10) 0.2040(4) 1.01445(19) 0.0331(7) Uani 1 1 d . . . . .
C13 C -0.01989(10) 0.1975(3) 0.95327(18) 0.0306(7) Uani 1 1 d . . . . .
C14 C 0.02787(10) 0.2664(3) 0.97949(18) 0.0306(7) Uani 1 1 d . . . . .
C15 C -0.09250(10) 0.0744(3) 0.8838(2) 0.0333(7) Uani 1 1 d . . . . .
C16 C -0.13130(10) -0.0189(3) 0.81404(19) 0.0323(7) Uani 1 1 d . . . . .
C17 C -0.17764(10) -0.0454(4) 0.8294(2) 0.0400(8) Uani 1 1 d . . . . .
C18 C -0.21347(11) -0.1404(4) 0.7638(2) 0.0517(9) Uani 1 1 d . . . . .
H18 H -0.2441 -0.1575 0.7743 0.062 Uiso 1 1 calc R U . . .
C19 C -0.20505(11) -0.2100(4) 0.6837(2) 0.0502(9) Uani 1 1 d . . . . .
H19 H -0.2296 -0.2753 0.6408 0.060 Uiso 1 1 calc R U . . .
C20 C -0.15969(11) -0.1831(4) 0.6664(2) 0.0474(8) Uani 1 1 d . . . . .
H20 H -0.1539 -0.2286 0.6115 0.057 Uiso 1 1 calc R U . . .
C21 C -0.12370(10) -0.0891(4) 0.7308(2) 0.0407(8) Uani 1 1 d . . . . .
H21 H -0.0934 -0.0714 0.7190 0.049 Uiso 1 1 calc R U . . .
H1N H -0.0385(10) 0.110(3) 0.8171(19) 0.062(10) Uiso 1 1 d . . . . .
H2O H -0.1607(14) 0.073(5) 0.950(3) 0.130(18) Uiso 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
O1 C1 1.231(3) . ?
O2 C8 1.224(3) . ?
O3 C17 1.356(3) . ?
N1 C13 1.366(3) . ?
N1 C15 1.370(3) . ?
N2 C15 1.330(3) . ?
N2 C12 1.391(3) . ?
C1 C14 1.466(3) . ?
C1 C2 1.479(3) . ?
C2 C3 1.391(3) . ?
C2 C7 1.395(3) . ?
C3 C4 1.375(3) . ?
C4 C5 1.389(4) . ?
C5 C6 1.375(4) . ?
C6 C7 1.387(3) . ?
C7 C8 1.481(3) . ?
C8 C9 1.481(3) . ?
C9 C10 1.399(3) . ?
C9 C14 1.404(3) . ?
C10 C11 1.380(3) . ?
C11 C12 1.384(3) . ?
C12 C13 1.407(3) . ?
C13 C14 1.391(3) . ?
C15 C16 1.445(3) . ?
C16 C21 1.398(3) . ?
C16 C17 1.404(3) . ?
C17 C18 1.376(4) . ?
C18 C19 1.366(4) . ?
C19 C20 1.389(3) . ?
C20 C21 1.367(3) . ?

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
C13 N1 C15 107.8(2) . . ?
C15 N2 C12 105.6(2) . . ?
O1 C1 C14 119.9(3) . . ?
O1 C1 C2 122.1(3) . . ?
C14 C1 C2 118.0(2) . . ?
C3 C2 C7 120.1(3) . . ?
C3 C2 C1 119.2(3) . . ?
C7 C2 C1 120.7(3) . . ?
C4 C3 C2 119.8(3) . . ?
C3 C4 C5 120.2(3) . . ?
C6 C5 C4 120.2(3) . . ?
C5 C6 C7 120.4(3) . . ?
C6 C7 C2 119.3(3) . . ?
C6 C7 C8 119.5(3) . . ?
C2 C7 C8 121.2(3) . . ?
O2 C8 C7 121.1(3) . . ?
O2 C8 C9 120.7(3) . . ?
C7 C8 C9 118.2(2) . . ?
C10 C9 C14 120.7(3) . . ?
C10 C9 C8 119.6(3) . . ?
C14 C9 C8 119.7(2) . . ?
C11 C10 C9 122.1(3) . . ?
C10 C11 C12 117.9(3) . . ?
C11 C12 N2 130.4(2) . . ?
C11 C12 C13 120.4(3) . . ?
N2 C12 C13 109.2(2) . . ?
N1 C13 C14 132.1(2) . . ?
N1 C13 C12 105.7(3) . . ?
C14 C13 C12 122.2(3) . . ?
C13 C14 C9 116.7(2) . . ?
C13 C14 C1 121.3(2) . . ?
C9 C14 C1 122.1(3) . . ?
N2 C15 N1 111.7(3) . . ?
N2 C15 C16 124.0(2) . . ?
N1 C15 C16 124.3(2) . . ?
C21 C16 C17 118.0(3) . . ?
C21 C16 C15 121.5(2) . . ?
C17 C16 C15 120.5(2) . . ?
O3 C17 C18 118.4(3) . . ?
O3 C17 C16 122.0(3) . . ?
C18 C17 C16 119.6(3) . . ?
C19 C18 C17 121.5(3) . . ?
C18 C19 C20 119.8(3) . . ?
C21 C20 C19 119.4(3) . . ?
C20 C21 C16 121.7(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
N1 H1N O1 0.90(3) 2.28(3) 3.115(3) 154(2) 2_556
N1 H1N O1 0.90(3) 2.31(3) 2.805(3) 114(2) .
O3 H2O N2 0.93(4) 1.82(4) 2.634(3) 144(3) .

_refine_diff_density_max         0.188
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.045

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

data_7
_database_code_depnum_ccdc_archive 'CCDC 1584244'
_audit_update_record             
;
2017-11-06 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H52 Cd2 N8 O10'
_chemical_formula_weight         1341.95

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'

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

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

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

_cell_length_a                   14.031(3)
_cell_length_b                   14.194(3)
_cell_length_c                   16.346(3)
_cell_angle_alpha                105.581(3)
_cell_angle_beta                 100.380(3)
_cell_angle_gamma                110.189(3)
_cell_volume                     2806.0(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    848
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      20.42

_exptl_crystal_description       Prism
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.829
_shelx_estimated_absorpt_T_min   0.692
_shelx_estimated_absorpt_T_max   0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6883
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 Sheldrick, G.M. SADABS: Program for absorption correction
 using area detector data. University of Göttingen, Germany, 1996.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15842
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.622
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             10184
_reflns_number_gt                6781
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0640P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10184
_refine_ls_number_parameters     814
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1337
_refine_ls_wR_factor_gt          0.1139
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.39682(3) 0.07603(3) 0.63724(3) 0.02160(13) Uani 1 1 d . . . . .
Cd2 Cd 0.52067(3) 0.25565(3) 0.85718(3) 0.02206(13) Uani 1 1 d . . . . .
O1 O 0.4344(3) 0.0756(3) 0.7814(2) 0.0275(9) Uani 1 1 d . . . . .
O2 O 0.2381(3) 0.0678(3) 0.5377(3) 0.0286(10) Uani 1 1 d . . . . .
O3 O -0.1223(3) -0.2552(3) 0.3023(3) 0.0486(13) Uani 1 1 d . . . . .
O4 O 0.4277(3) 0.2414(3) 0.7236(2) 0.0249(9) Uani 1 1 d . . . . .
O5 O 0.6688(3) 0.2481(3) 0.9461(3) 0.0323(10) Uani 1 1 d . . . . .
O6 O 1.0873(3) 0.3685(4) 0.9912(3) 0.0519(13) Uani 1 1 d . . . . .
N1 N 0.2735(3) -0.0797(3) 0.6194(3) 0.0211(10) Uani 1 1 d . . . . .
N2 N 0.2087(4) -0.2480(4) 0.6269(3) 0.0278(12) Uani 1 1 d . . . . .
N3 N 0.5665(4) 0.0660(4) 0.6435(3) 0.0311(12) Uani 1 1 d . . . . .
N4 N 0.4767(4) 0.1534(4) 0.5427(3) 0.0280(12) Uani 1 1 d . . . . .
N5 N 0.6546(4) 0.3420(3) 0.8092(3) 0.0235(11) Uani 1 1 d . . . . .
N6 N 0.7428(4) 0.4395(4) 0.7352(3) 0.0288(12) Uani 1 1 d . . . . .
N7 N 0.5775(3) 0.4107(4) 0.9857(3) 0.0249(11) Uani 1 1 d . . . . .
N8 N 0.4017(3) 0.2308(4) 0.9404(3) 0.0254(11) Uani 1 1 d . . . . .
C1 C 0.4377(5) -0.0089(4) 0.8000(4) 0.0266(14) Uani 1 1 d . . . . .
C2 C 0.5093(5) 0.0060(5) 0.8795(4) 0.0415(17) Uani 1 1 d . . . . .
H2 H 0.5472 0.0752 0.9215 0.050 Uiso 1 1 calc R U . . .
C3 C 0.5256(6) -0.0769(5) 0.8978(5) 0.050(2) Uani 1 1 d . . . . .
H3 H 0.5750 -0.0631 0.9506 0.060 Uiso 1 1 calc R U . . .
C4 C 0.4686(5) -0.1812(5) 0.8374(5) 0.0478(19) Uani 1 1 d . . . . .
H4 H 0.4810 -0.2378 0.8478 0.057 Uiso 1 1 calc R U . . .
C5 C 0.3929(5) -0.1990(5) 0.7613(4) 0.0351(16) Uani 1 1 d . . . . .
H5 H 0.3525 -0.2693 0.7218 0.042 Uiso 1 1 calc R U . . .
C6 C 0.3746(4) -0.1168(4) 0.7413(4) 0.0270(14) Uani 1 1 d . . . . .
C7 C 0.2861(4) -0.1477(4) 0.6613(4) 0.0254(13) Uani 1 1 d . . . . .
C8 C 0.1787(4) -0.1414(4) 0.5523(4) 0.0225(13) Uani 1 1 d . . . . .
C9 C 0.1410(4) -0.2461(4) 0.5558(4) 0.0252(13) Uani 1 1 d . . . . .
C10 C 0.0470(5) -0.3280(5) 0.4942(4) 0.0359(16) Uani 1 1 d . . . . .
H10 H 0.0232 -0.3972 0.4957 0.043 Uiso 1 1 calc R U . . .
C11 C -0.0094(5) -0.3042(5) 0.4317(4) 0.0360(16) Uani 1 1 d . . . . .
H11 H -0.0716 -0.3587 0.3897 0.043 Uiso 1 1 calc R U . . .
C12 C 0.0237(4) -0.2003(4) 0.4289(4) 0.0256(13) Uani 1 1 d . . . . .
C13 C 0.1194(4) -0.1167(4) 0.4892(4) 0.0230(13) Uani 1 1 d . . . . .
C14 C 0.1521(4) -0.0074(4) 0.4872(4) 0.0208(12) Uani 1 1 d . . . . .
C15 C 0.0802(4) 0.0140(4) 0.4231(4) 0.0215(12) Uani 1 1 d . . . . .
C16 C 0.1071(4) 0.1175(5) 0.4233(4) 0.0265(14) Uani 1 1 d . . . . .
H16 H 0.1707 0.1731 0.4625 0.032 Uiso 1 1 calc R U . . .
C17 C 0.0388(5) 0.1384(5) 0.3646(4) 0.0345(15) Uani 1 1 d . . . . .
H17 H 0.0566 0.2076 0.3641 0.041 Uiso 1 1 calc R U . . .
C18 C -0.0554(5) 0.0554(5) 0.3075(4) 0.0369(16) Uani 1 1 d . . . . .
H18 H -0.1018 0.0697 0.2695 0.044 Uiso 1 1 calc R U . . .
C19 C -0.0821(5) -0.0475(5) 0.3055(4) 0.0365(16) Uani 1 1 d . . . . .
H19 H -0.1455 -0.1025 0.2655 0.044 Uiso 1 1 calc R U . . .
C20 C -0.0158(4) -0.0700(4) 0.3625(4) 0.0247(13) Uani 1 1 d . . . . .
C21 C -0.0444(4) -0.1822(5) 0.3599(4) 0.0327(15) Uani 1 1 d . . . . .
C22 C 0.6088(5) 0.0224(5) 0.6937(5) 0.0409(17) Uani 1 1 d . . . . .
H22 H 0.5626 -0.0308 0.7084 0.049 Uiso 1 1 calc R U . . .
C23 C 0.7170(5) 0.0508(6) 0.7257(5) 0.0427(17) Uani 1 1 d . . . . .
H23 H 0.7431 0.0185 0.7613 0.051 Uiso 1 1 calc R U . . .
C24 C 0.7838(5) 0.1286(6) 0.7025(5) 0.0439(18) Uani 1 1 d . . . . .
H24 H 0.8571 0.1513 0.7234 0.053 Uiso 1 1 calc R U . . .
C25 C 0.7423(5) 0.1731(5) 0.6485(4) 0.0388(17) Uani 1 1 d . . . . .
H25 H 0.7872 0.2251 0.6318 0.047 Uiso 1 1 calc R U . . .
C26 C 0.6325(5) 0.1397(5) 0.6189(4) 0.0293(14) Uani 1 1 d . . . . .
C27 C 0.5825(5) 0.1814(5) 0.5582(4) 0.0293(14) Uani 1 1 d . . . . .
C28 C 0.6391(5) 0.2471(5) 0.5191(5) 0.0412(17) Uani 1 1 d . . . . .
H28 H 0.7119 0.2661 0.5304 0.049 Uiso 1 1 calc R U . . .
C29 C 0.5897(6) 0.2846(6) 0.4642(5) 0.0461(18) Uani 1 1 d . . . . .
H29 H 0.6280 0.3286 0.4377 0.055 Uiso 1 1 calc R U . . .
C30 C 0.4828(5) 0.2564(5) 0.4489(5) 0.0422(17) Uani 1 1 d . . . . .
H30 H 0.4473 0.2817 0.4125 0.051 Uiso 1 1 calc R U . . .
C31 C 0.4291(5) 0.1901(5) 0.4882(4) 0.0311(15) Uani 1 1 d . . . . .
H31 H 0.3561 0.1697 0.4764 0.037 Uiso 1 1 calc R U . . .
C32 C 0.4460(4) 0.3217(4) 0.6920(4) 0.0211(12) Uani 1 1 d . . . . .
C33 C 0.3598(5) 0.3329(5) 0.6456(4) 0.0293(14) Uani 1 1 d . . . . .
H33 H 0.2913 0.2837 0.6369 0.035 Uiso 1 1 calc R U . . .
C34 C 0.3723(5) 0.4145(5) 0.6120(4) 0.0402(17) Uani 1 1 d . . . . .
H34 H 0.3132 0.4210 0.5822 0.048 Uiso 1 1 calc R U . . .
C35 C 0.4737(5) 0.4861(5) 0.6234(5) 0.050(2) Uani 1 1 d . . . . .
H35 H 0.4832 0.5414 0.6011 0.060 Uiso 1 1 calc R U . . .
C36 C 0.5603(5) 0.4762(5) 0.6672(4) 0.0383(16) Uani 1 1 d . . . . .
H36 H 0.6279 0.5244 0.6726 0.046 Uiso 1 1 calc R U . . .
C37 C 0.5514(5) 0.3962(4) 0.7045(4) 0.0261(14) Uani 1 1 d . . . . .
C38 C 0.6486(4) 0.3911(4) 0.7487(4) 0.0234(13) Uani 1 1 d . . . . .
C39 C 0.7600(4) 0.3601(4) 0.8371(4) 0.0239(13) Uani 1 1 d . . . . .
C40 C 0.8132(5) 0.4197(5) 0.7895(4) 0.0280(14) Uani 1 1 d . . . . .
C41 C 0.9225(5) 0.4481(5) 0.8009(4) 0.0342(15) Uani 1 1 d . . . . .
H41 H 0.9569 0.4846 0.7679 0.041 Uiso 1 1 calc R U . . .
C42 C 0.9766(5) 0.4203(5) 0.8620(4) 0.0348(16) Uani 1 1 d . . . . .
H42 H 1.0488 0.4382 0.8700 0.042 Uiso 1 1 calc R U . . .
C43 C 0.9270(4) 0.3660(5) 0.9129(4) 0.0287(14) Uani 1 1 d . . . . .
C44 C 0.8165(4) 0.3332(4) 0.9009(4) 0.0240(13) Uani 1 1 d . . . . .
C45 C 0.7655(5) 0.2783(4) 0.9555(4) 0.0253(13) Uani 1 1 d . . . . .
C46 C 0.8303(5) 0.2579(4) 1.0244(4) 0.0283(14) Uani 1 1 d . . . . .
C47 C 0.7826(5) 0.2078(5) 1.0773(4) 0.0344(15) Uani 1 1 d . . . . .
H47 H 0.7094 0.1843 1.0671 0.041 Uiso 1 1 calc R U . . .
C48 C 0.8429(5) 0.1922(5) 1.1454(5) 0.0436(18) Uani 1 1 d . . . . .
H48 H 0.8107 0.1586 1.1810 0.052 Uiso 1 1 calc R U . . .
C49 C 0.9526(6) 0.2279(6) 1.1597(5) 0.0492(19) Uani 1 1 d . . . . .
H49 H 0.9938 0.2187 1.2057 0.059 Uiso 1 1 calc R U . . .
C50 C 1.0001(5) 0.2760(5) 1.1069(4) 0.0392(17) Uani 1 1 d . . . . .
H50 H 1.0732 0.2987 1.1168 0.047 Uiso 1 1 calc R U . . .
C51 C 0.9399(5) 0.2912(5) 1.0386(4) 0.0304(14) Uani 1 1 d . . . . .
C52 C 0.9923(5) 0.3441(5) 0.9817(4) 0.0344(15) Uani 1 1 d . . . . .
C53 C 0.6714(5) 0.4947(5) 1.0081(4) 0.0318(15) Uani 1 1 d . . . . .
H53 H 0.7081 0.4982 0.9662 0.038 Uiso 1 1 calc R U . . .
C54 C 0.7157(5) 0.5757(5) 1.0900(4) 0.0335(15) Uani 1 1 d . . . . .
H54 H 0.7813 0.6326 1.1036 0.040 Uiso 1 1 calc R U . . .
C55 C 0.6608(5) 0.5708(5) 1.1512(4) 0.0392(17) Uani 1 1 d . . . . .
H55 H 0.6880 0.6255 1.2068 0.047 Uiso 1 1 calc R U . . .
C56 C 0.5648(5) 0.4841(5) 1.1299(4) 0.0355(16) Uani 1 1 d . . . . .
H56 H 0.5275 0.4788 1.1713 0.043 Uiso 1 1 calc R U . . .
C57 C 0.5250(4) 0.4053(4) 1.0462(4) 0.0225(13) Uani 1 1 d . . . . .
C58 C 0.4215(4) 0.3094(5) 1.0169(4) 0.0250(13) Uani 1 1 d . . . . .
C59 C 0.3500(5) 0.3000(5) 1.0662(4) 0.0358(16) Uani 1 1 d . . . . .
H59 H 0.3653 0.3543 1.1199 0.043 Uiso 1 1 calc R U . . .
C60 C 0.2553(5) 0.2083(6) 1.0338(5) 0.0475(19) Uani 1 1 d . . . . .
H60 H 0.2057 0.2014 1.0651 0.057 Uiso 1 1 calc R U . . .
C61 C 0.2350(5) 0.1287(5) 0.9564(5) 0.0426(18) Uani 1 1 d . . . . .
H61 H 0.1723 0.0663 0.9348 0.051 Uiso 1 1 calc R U . . .
C62 C 0.3091(5) 0.1419(5) 0.9102(4) 0.0357(16) Uani 1 1 d . . . . .
H62 H 0.2947 0.0879 0.8565 0.043 Uiso 1 1 calc R U . . .
O1S O 0.8194(5) 0.5907(5) 0.6618(5) 0.0748(18) Uani 1 1 d . . . . .
H1S H 0.7795 0.5418 0.6734 0.112 Uiso 1 1 calc R U . . .
C1S C 0.8547(11) 0.5482(8) 0.5932(7) 0.129(5) Uani 1 1 d . . . . .
H1S1 H 0.8835 0.6014 0.5679 0.193 Uiso 1 1 calc R U . . .
H1S2 H 0.7961 0.4866 0.5481 0.193 Uiso 1 1 calc R U . . .
H1S3 H 0.9089 0.5270 0.6158 0.193 Uiso 1 1 calc R U . . .
O2S O 0.9709(4) 0.9740(5) 0.9086(5) 0.0818(19) Uani 1 1 d . . . . .
H2S H 0.9188 0.9160 0.8868 0.123 Uiso 1 1 calc R U . . .
C2S C 0.9443(7) 1.0517(7) 0.8862(7) 0.094(3) Uani 1 1 d . . . . .
H2S1 H 0.8779 1.0467 0.8967 0.140 Uiso 1 1 calc R U . . .
H2S2 H 0.9376 1.0401 0.8245 0.140 Uiso 1 1 calc R U . . .
H2S3 H 0.9991 1.1218 0.9222 0.140 Uiso 1 1 calc R U . . .
O3S O 0.8174(7) 0.7772(9) 0.7781(8) 0.057(3) Uani 0.55 1 d D . P A 1
H3S H 0.8142 0.7187 0.7492 0.086 Uiso 0.55 1 calc R U P A 1
C3S C 0.727(2) 0.786(3) 0.7446(15) 0.070(8) Uani 0.55 1 d D U P A 1
H3S1 H 0.7362 0.8189 0.7006 0.105 Uiso 0.55 1 calc R U P A 1
H3S2 H 0.7115 0.8296 0.7916 0.105 Uiso 0.55 1 calc R U P A 1
H3S3 H 0.6694 0.7159 0.7175 0.105 Uiso 0.55 1 calc R U P A 1
O3SA O 0.7230(10) 0.7125(10) 0.6425(8) 0.063(3) Uani 0.45 1 d D . P B 2
H3SA H 0.7462 0.6662 0.6338 0.094 Uiso 0.45 1 calc R U P B 2
C3SA C 0.751(3) 0.767(4) 0.7320(15) 0.080(12) Uani 0.45 1 d D U P B 2
H3S4 H 0.8259 0.8101 0.7546 0.119 Uiso 0.45 1 calc R U P B 2
H3S5 H 0.7318 0.7160 0.7616 0.119 Uiso 0.45 1 calc R U P B 2
H3S6 H 0.7132 0.8119 0.7427 0.119 Uiso 0.45 1 calc R U P B 2
O4S O 1.1760(10) 0.5527(7) 0.6473(6) 0.072(3) Uani 0.65 1 d D . P C 1
H4S H 1.1849 0.6126 0.6465 0.108 Uiso 0.65 1 calc R U P C 1
C4S C 1.1890(8) 0.5549(6) 0.7371(5) 0.072(3) Uani 0.65 1 d D . P C 1
H4S1 H 1.2619 0.5708 0.7650 0.108 Uiso 0.65 1 calc R U P C 1
H4S2 H 1.1436 0.4861 0.7365 0.108 Uiso 0.65 1 calc R U P C 1
H4S3 H 1.1702 0.6093 0.7699 0.108 Uiso 0.65 1 calc R U P C 1
O4SA O 1.1202(12) 0.5679(14) 0.6800(15) 0.064(6) Uani 0.35 1 d D . P D 2
H4SA H 1.1384 0.6322 0.6892 0.095 Uiso 0.35 1 calc R U P D 2
C4SA C 1.1890(8) 0.5549(6) 0.7371(5) 0.072(3) Uani 0.35 1 d . . P D 2
H4S4 H 1.2526 0.6205 0.7650 0.108 Uiso 0.35 1 calc R U P D 2
H4S5 H 1.2063 0.4981 0.7064 0.108 Uiso 0.35 1 calc R U P D 2
H4S6 H 1.1584 0.5367 0.7818 0.108 Uiso 0.35 1 calc R U P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.190(4) . ?
Cd1 O4 2.233(4) . ?
Cd1 O1 2.323(4) . ?
Cd1 N4 2.353(5) . ?
Cd1 N3 2.419(5) . ?
Cd1 O2 2.457(4) . ?
Cd2 O4 2.250(4) . ?
Cd2 N5 2.260(4) . ?
Cd2 O1 2.271(4) . ?
Cd2 N8 2.330(4) . ?
Cd2 N7 2.365(5) . ?
Cd2 O5 2.365(4) . ?
O1 C1 1.327(6) . ?
O2 C14 1.247(6) . ?
O3 C21 1.216(7) . ?
O4 C32 1.341(6) . ?
O5 C45 1.240(6) . ?
O6 C52 1.224(7) . ?
N1 C7 1.364(7) . ?
N1 C8 1.376(7) . ?
N2 C7 1.343(7) . ?
N2 C9 1.374(7) . ?
N3 C22 1.327(8) . ?
N3 C26 1.343(7) . ?
N4 C31 1.336(7) . ?
N4 C27 1.354(7) . ?
N5 C38 1.361(7) . ?
N5 C39 1.376(7) . ?
N6 C38 1.352(7) . ?
N6 C40 1.361(7) . ?
N7 C57 1.339(6) . ?
N7 C53 1.342(7) . ?
N8 C58 1.341(7) . ?
N8 C62 1.352(7) . ?
C1 C2 1.406(8) . ?
C1 C6 1.421(8) . ?
C2 C3 1.370(9) . ?
C3 C4 1.385(9) . ?
C4 C5 1.382(9) . ?
C5 C6 1.384(8) . ?
C6 C7 1.476(8) . ?
C8 C13 1.402(8) . ?
C8 C9 1.417(7) . ?
C9 C10 1.393(8) . ?
C10 C11 1.364(9) . ?
C11 C12 1.401(8) . ?
C12 C13 1.406(7) . ?
C12 C21 1.480(8) . ?
C13 C14 1.470(7) . ?
C14 C15 1.486(8) . ?
C15 C16 1.384(7) . ?
C15 C20 1.412(7) . ?
C16 C17 1.395(8) . ?
C17 C18 1.376(8) . ?
C18 C19 1.366(8) . ?
C19 C20 1.374(8) . ?
C20 C21 1.488(8) . ?
C22 C23 1.386(9) . ?
C23 C24 1.372(9) . ?
C24 C25 1.374(9) . ?
C25 C26 1.391(8) . ?
C26 C27 1.477(9) . ?
C27 C28 1.378(8) . ?
C28 C29 1.362(9) . ?
C29 C30 1.366(9) . ?
C30 C31 1.369(8) . ?
C32 C33 1.389(8) . ?
C32 C37 1.429(8) . ?
C33 C34 1.382(8) . ?
C34 C35 1.377(9) . ?
C35 C36 1.367(9) . ?
C36 C37 1.406(8) . ?
C37 C38 1.459(8) . ?
C39 C44 1.409(8) . ?
C39 C40 1.416(8) . ?
C40 C41 1.407(8) . ?
C41 C42 1.369(9) . ?
C42 C43 1.397(8) . ?
C43 C44 1.415(8) . ?
C43 C52 1.489(8) . ?
C44 C45 1.461(8) . ?
C45 C46 1.472(8) . ?
C46 C47 1.382(8) . ?
C46 C51 1.398(8) . ?
C47 C48 1.387(9) . ?
C48 C49 1.397(9) . ?
C49 C50 1.365(9) . ?
C50 C51 1.388(8) . ?
C51 C52 1.486(8) . ?
C53 C54 1.371(8) . ?
C54 C55 1.371(8) . ?
C55 C56 1.381(8) . ?
C56 C57 1.380(8) . ?
C57 C58 1.492(7) . ?
C58 C59 1.389(8) . ?
C59 C60 1.386(8) . ?
C60 C61 1.356(9) . ?
C61 C62 1.382(8) . ?
O1S C1S 1.383(10) . ?
O2S C2S 1.393(10) . ?
O3S C3S 1.347(17) . ?
O3SA C3SA 1.367(19) . ?
O4S C4S 1.437(11) . ?
O4SA C4SA 1.315(14) . ?

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 O4 129.80(15) . . ?
N1 Cd1 O1 78.95(15) . . ?
O4 Cd1 O1 75.33(13) . . ?
N1 Cd1 N4 135.24(16) . . ?
O4 Cd1 N4 87.80(15) . . ?
O1 Cd1 N4 141.61(15) . . ?
N1 Cd1 N3 110.99(16) . . ?
O4 Cd1 N3 108.24(15) . . ?
O1 Cd1 N3 83.91(15) . . ?
N4 Cd1 N3 68.79(17) . . ?
N1 Cd1 O2 76.92(14) . . ?
O4 Cd1 O2 89.47(13) . . ?
O1 Cd1 O2 132.03(13) . . ?
N4 Cd1 O2 80.84(15) . . ?
N3 Cd1 O2 143.63(16) . . ?
O4 Cd2 N5 79.51(15) . . ?
O4 Cd2 O1 76.04(13) . . ?
N5 Cd2 O1 114.75(15) . . ?
O4 Cd2 N8 106.23(15) . . ?
N5 Cd2 N8 159.13(16) . . ?
O1 Cd2 N8 86.10(15) . . ?
O4 Cd2 N7 121.92(15) . . ?
N5 Cd2 N7 90.48(15) . . ?
O1 Cd2 N7 152.38(15) . . ?
N8 Cd2 N7 69.32(15) . . ?
O4 Cd2 O5 149.62(14) . . ?
N5 Cd2 O5 77.83(15) . . ?
O1 Cd2 O5 95.46(14) . . ?
N8 Cd2 O5 102.13(15) . . ?
N7 Cd2 O5 78.33(15) . . ?
C1 O1 Cd2 133.1(3) . . ?
C1 O1 Cd1 122.9(3) . . ?
Cd2 O1 Cd1 99.05(14) . . ?
C14 O2 Cd1 133.5(4) . . ?
C32 O4 Cd1 121.1(3) . . ?
C32 O4 Cd2 124.6(3) . . ?
Cd1 O4 Cd2 102.42(15) . . ?
C45 O5 Cd2 137.6(4) . . ?
C7 N1 C8 104.0(4) . . ?
C7 N1 Cd1 125.6(4) . . ?
C8 N1 Cd1 128.8(4) . . ?
C7 N2 C9 103.3(4) . . ?
C22 N3 C26 117.9(5) . . ?
C22 N3 Cd1 124.3(4) . . ?
C26 N3 Cd1 113.9(4) . . ?
C31 N4 C27 118.3(5) . . ?
C31 N4 Cd1 123.3(4) . . ?
C27 N4 Cd1 117.0(4) . . ?
C38 N5 C39 105.3(5) . . ?
C38 N5 Cd2 126.9(4) . . ?
C39 N5 Cd2 127.7(4) . . ?
C38 N6 C40 104.4(5) . . ?
C57 N7 C53 118.5(5) . . ?
C57 N7 Cd2 118.3(3) . . ?
C53 N7 Cd2 121.9(4) . . ?
C58 N8 C62 118.9(5) . . ?
C58 N8 Cd2 119.5(4) . . ?
C62 N8 Cd2 121.4(4) . . ?
O1 C1 C2 120.1(5) . . ?
O1 C1 C6 123.3(5) . . ?
C2 C1 C6 116.6(5) . . ?
C3 C2 C1 122.9(6) . . ?
C2 C3 C4 119.9(6) . . ?
C5 C4 C3 118.3(6) . . ?
C4 C5 C6 122.8(6) . . ?
C5 C6 C1 119.1(6) . . ?
C5 C6 C7 117.2(5) . . ?
C1 C6 C7 123.6(5) . . ?
N2 C7 N1 115.6(5) . . ?
N2 C7 C6 119.8(5) . . ?
N1 C7 C6 124.6(5) . . ?
N1 C8 C13 132.0(5) . . ?
N1 C8 C9 107.5(5) . . ?
C13 C8 C9 120.6(5) . . ?
N2 C9 C10 129.6(5) . . ?
N2 C9 C8 109.5(5) . . ?
C10 C9 C8 120.9(6) . . ?
C11 C10 C9 118.4(5) . . ?
C10 C11 C12 122.0(5) . . ?
C11 C12 C13 120.8(5) . . ?
C11 C12 C21 117.9(5) . . ?
C13 C12 C21 121.3(5) . . ?
C8 C13 C12 117.3(5) . . ?
C8 C13 C14 122.2(5) . . ?
C12 C13 C14 120.4(5) . . ?
O2 C14 C13 122.0(5) . . ?
O2 C14 C15 119.1(5) . . ?
C13 C14 C15 118.8(5) . . ?
C16 C15 C20 119.6(5) . . ?
C16 C15 C14 119.7(5) . . ?
C20 C15 C14 120.8(5) . . ?
C15 C16 C17 119.9(5) . . ?
C18 C17 C16 119.4(6) . . ?
C19 C18 C17 121.4(6) . . ?
C18 C19 C20 120.2(6) . . ?
C19 C20 C15 119.5(5) . . ?
C19 C20 C21 120.3(5) . . ?
C15 C20 C21 120.2(5) . . ?
O3 C21 C12 122.3(6) . . ?
O3 C21 C20 119.6(6) . . ?
C12 C21 C20 118.1(5) . . ?
N3 C22 C23 124.5(6) . . ?
C24 C23 C22 116.9(6) . . ?
C23 C24 C25 120.0(6) . . ?
C24 C25 C26 119.4(6) . . ?
N3 C26 C25 121.2(6) . . ?
N3 C26 C27 116.6(5) . . ?
C25 C26 C27 122.1(6) . . ?
N4 C27 C28 120.3(6) . . ?
N4 C27 C26 116.8(5) . . ?
C28 C27 C26 122.9(6) . . ?
C29 C28 C27 120.8(6) . . ?
C28 C29 C30 118.7(6) . . ?
C29 C30 C31 118.8(6) . . ?
N4 C31 C30 123.1(6) . . ?
O4 C32 C33 118.8(5) . . ?
O4 C32 C37 122.1(5) . . ?
C33 C32 C37 119.1(5) . . ?
C34 C33 C32 122.2(6) . . ?
C35 C34 C33 119.0(6) . . ?
C36 C35 C34 120.3(6) . . ?
C35 C36 C37 122.7(6) . . ?
C36 C37 C32 116.7(6) . . ?
C36 C37 C38 118.6(5) . . ?
C32 C37 C38 124.6(5) . . ?
N6 C38 N5 113.8(5) . . ?
N6 C38 C37 122.0(5) . . ?
N5 C38 C37 124.1(5) . . ?
N5 C39 C44 132.4(5) . . ?
N5 C39 C40 106.8(5) . . ?
C44 C39 C40 120.8(5) . . ?
N6 C40 C41 129.5(5) . . ?
N6 C40 C39 109.7(5) . . ?
C41 C40 C39 120.8(6) . . ?
C42 C41 C40 118.0(6) . . ?
C41 C42 C43 122.2(6) . . ?
C42 C43 C44 121.1(6) . . ?
C42 C43 C52 119.2(5) . . ?
C44 C43 C52 119.8(5) . . ?
C39 C44 C43 117.0(5) . . ?
C39 C44 C45 122.1(5) . . ?
C43 C44 C45 120.8(5) . . ?
O5 C45 C44 122.3(5) . . ?
O5 C45 C46 118.2(5) . . ?
C44 C45 C46 119.5(5) . . ?
C47 C46 C51 119.7(6) . . ?
C47 C46 C45 119.6(5) . . ?
C51 C46 C45 120.7(5) . . ?
C46 C47 C48 120.6(6) . . ?
C47 C48 C49 118.9(6) . . ?
C50 C49 C48 120.8(7) . . ?
C49 C50 C51 120.3(6) . . ?
C50 C51 C46 119.7(6) . . ?
C50 C51 C52 119.9(5) . . ?
C46 C51 C52 120.5(5) . . ?
O6 C52 C51 120.5(6) . . ?
O6 C52 C43 120.8(6) . . ?
C51 C52 C43 118.7(5) . . ?
N7 C53 C54 123.0(5) . . ?
C53 C54 C55 118.3(5) . . ?
C54 C55 C56 119.5(6) . . ?
C57 C56 C55 119.0(6) . . ?
N7 C57 C56 121.6(5) . . ?
N7 C57 C58 115.6(5) . . ?
C56 C57 C58 122.8(5) . . ?
N8 C58 C59 121.3(5) . . ?
N8 C58 C57 116.1(5) . . ?
C59 C58 C57 122.6(5) . . ?
C60 C59 C58 118.8(6) . . ?
C61 C60 C59 120.1(6) . . ?
C60 C61 C62 118.8(6) . . ?
N8 C62 C61 122.1(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
O1S H1S N6 0.82 1.96 2.731(7) 155.6 .
O2S H2S O3S 0.82 2.08 2.825(12) 150.5 .
O3S H3S O1S 0.82 2.02 2.827(13) 168.0 .
O3SA H3SA O1S 0.82 1.81 2.582(13) 157.3 .
O4S H4S N2 0.82 2.01 2.828(9) 171.8 1_665
O4SA H4SA N2 0.82 2.25 2.915(17) 139.1 1_665

_refine_diff_density_max         1.136
_refine_diff_density_min         -0.917
_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_5
_database_code_depnum_ccdc_archive 'CCDC 1584242'
_audit_update_record             
;
2017-11-06 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H24 Cu N4 O4'
_chemical_formula_weight         640.13

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.4821(9)
_cell_length_b                   12.9049(10)
_cell_length_c                   22.1401(17)
_cell_angle_alpha                92.519(2)
_cell_angle_beta                 91.393(2)
_cell_angle_gamma                116.245(2)
_cell_volume                     2936.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    922
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      21.40

_exptl_crystal_description       Plate
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_F_000             1316
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.793
_shelx_estimated_absorpt_T_min   0.742
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6542
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 Sheldrick, G.M. SADABS: Program for absorption correction
 using area detector data. University of Göttingen, Germany, 1996.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21051
_diffrn_reflns_av_unetI/netI     0.1343
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.763
_diffrn_reflns_theta_max         28.309
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             14259
_reflns_number_gt                6285
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BRUKER Smart'
_computing_cell_refinement       'BRUKER Smart'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0615P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14259
_refine_ls_number_parameters     815
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1486
_refine_ls_wR_factor_gt          0.1184
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_restrained_S_all      0.879
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.39591(4) 0.08267(4) 0.09141(2) 0.04310(15) Uani 1 1 d . . . . .
O1 O 0.4695(3) -0.0107(2) 0.12524(12) 0.0557(7) Uani 1 1 d . . . . .
O2 O 0.3017(2) 0.1699(2) 0.04958(11) 0.0504(7) Uani 1 1 d . . . . .
O3 O 0.4650(4) 0.5038(3) -0.11033(14) 0.0906(11) Uani 1 1 d . . . . .
N1 N 0.5363(3) 0.1543(2) 0.04080(12) 0.0392(7) Uani 1 1 d . . . . .
N2 N 0.7300(3) 0.2057(3) -0.00304(13) 0.0473(8) Uani 1 1 d . . . . .
N3 N 0.2286(3) -0.0061(3) 0.13291(13) 0.0427(8) Uani 1 1 d . . . . .
N4 N 0.4116(4) 0.2056(3) 0.17120(14) 0.0569(9) Uani 1 1 d . . . . .
C1 C 0.5819(4) -0.0103(3) 0.11359(17) 0.0453(10) Uani 1 1 d . . . . .
C2 C 0.6185(4) -0.0831(4) 0.14700(19) 0.0594(12) Uani 1 1 d . . . . .
H2 H 0.5635 -0.1277 0.1757 0.071 Uiso 1 1 calc R U . . .
C3 C 0.7323(4) -0.0894(4) 0.1381(2) 0.0667(13) Uani 1 1 d . . . . .
H3 H 0.7531 -0.1384 0.1608 0.080 Uiso 1 1 calc R U . . .
C4 C 0.8176(4) -0.0241(4) 0.0960(2) 0.0647(12) Uani 1 1 d . . . . .
H4 H 0.8949 -0.0291 0.0900 0.078 Uiso 1 1 calc R U . . .
C5 C 0.7853(4) 0.0473(4) 0.06381(18) 0.0532(11) Uani 1 1 d . . . . .
H5 H 0.8419 0.0913 0.0354 0.064 Uiso 1 1 calc R U . . .
C6 C 0.6699(3) 0.0573(3) 0.07165(15) 0.0404(9) Uani 1 1 d . . . . .
C7 C 0.6461(3) 0.1383(3) 0.03623(15) 0.0404(9) Uani 1 1 d . . . . .
C8 C 0.5499(4) 0.2361(3) 0.00125(15) 0.0399(9) Uani 1 1 d . . . . .
C9 C 0.6705(4) 0.2681(3) -0.02582(16) 0.0450(10) Uani 1 1 d . . . . .
C10 C 0.7097(4) 0.3529(4) -0.06768(17) 0.0557(11) Uani 1 1 d . . . . .
H10 H 0.7889 0.3755 -0.0857 0.067 Uiso 1 1 calc R U . . .
C11 C 0.6296(4) 0.4030(4) -0.08202(16) 0.0558(11) Uani 1 1 d . . . . .
H11 H 0.6565 0.4602 -0.1097 0.067 Uiso 1 1 calc R U . . .
C12 C 0.5102(4) 0.3711(3) -0.05660(16) 0.0478(10) Uani 1 1 d . . . . .
C13 C 0.4673(4) 0.2851(3) -0.01358(15) 0.0397(9) Uani 1 1 d . . . . .
C14 C 0.3417(4) 0.2470(3) 0.01302(16) 0.0428(9) Uani 1 1 d . . . . .
C15 C 0.2598(4) 0.3049(3) -0.00393(17) 0.0471(10) Uani 1 1 d . . . . .
C16 C 0.1417(4) 0.2741(4) 0.02137(19) 0.0591(11) Uani 1 1 d . . . . .
H16 H 0.1127 0.2161 0.0486 0.071 Uiso 1 1 calc R U . . .
C17 C 0.0653(4) 0.3288(4) 0.0066(2) 0.0712(13) Uani 1 1 d . . . . .
H17 H -0.0145 0.3075 0.0240 0.085 Uiso 1 1 calc R U . . .
C18 C 0.1083(5) 0.4152(4) -0.0341(2) 0.0713(14) Uani 1 1 d . . . . .
H18 H 0.0575 0.4521 -0.0439 0.086 Uiso 1 1 calc R U . . .
C19 C 0.2259(5) 0.4464(4) -0.0599(2) 0.0643(12) Uani 1 1 d . . . . .
H19 H 0.2541 0.5041 -0.0873 0.077 Uiso 1 1 calc R U . . .
C20 C 0.3027(4) 0.3924(3) -0.04533(17) 0.0493(10) Uani 1 1 d . . . . .
C21 C 0.4294(4) 0.4273(4) -0.07336(18) 0.0575(11) Uani 1 1 d . . . . .
C22 C 0.1438(4) -0.1131(4) 0.11722(18) 0.0509(10) Uani 1 1 d . . . . .
H22 H 0.1597 -0.1504 0.0838 0.061 Uiso 1 1 calc R U . . .
C23 C 0.0315(4) -0.1735(4) 0.1480(2) 0.0626(12) Uani 1 1 d . . . . .
H23 H -0.0255 -0.2491 0.1351 0.075 Uiso 1 1 calc R U . . .
C24 C 0.0056(4) -0.1214(5) 0.1970(2) 0.0690(14) Uani 1 1 d . . . . .
H24 H -0.0678 -0.1616 0.2187 0.083 Uiso 1 1 calc R U . . .
C25 C 0.0908(5) -0.0066(5) 0.21418(19) 0.0610(12) Uani 1 1 d . . . . .
C26 C 0.2041(4) 0.0475(4) 0.18187(16) 0.0447(10) Uani 1 1 d . . . . .
C27 C 0.2991(5) 0.1614(4) 0.20099(18) 0.0540(11) Uani 1 1 d . . . . .
C28 C 0.2755(6) 0.2208(5) 0.2507(2) 0.0763(15) Uani 1 1 d . . . . .
C29 C 0.3759(8) 0.3302(6) 0.2675(2) 0.101(2) Uani 1 1 d . . . . .
H29 H 0.3646 0.3740 0.2992 0.122 Uiso 1 1 calc R U . . .
C30 C 0.4877(8) 0.3736(5) 0.2391(3) 0.103(2) Uani 1 1 d . . . . .
H30 H 0.5542 0.4457 0.2517 0.124 Uiso 1 1 calc R U . . .
C31 C 0.5037(5) 0.3084(4) 0.1898(2) 0.0789(15) Uani 1 1 d . . . . .
H31 H 0.5812 0.3389 0.1699 0.095 Uiso 1 1 calc R U . . .
C32 C 0.0717(6) 0.0578(6) 0.2642(2) 0.0840(17) Uani 1 1 d . . . . .
H32 H -0.0032 0.0235 0.2857 0.101 Uiso 1 1 calc R U . . .
C33 C 0.1585(7) 0.1654(6) 0.2803(2) 0.0948(19) Uani 1 1 d . . . . .
H33 H 0.1415 0.2053 0.3122 0.114 Uiso 1 1 calc R U . . .
Cu2 Cu 0.95552(4) 0.71006(4) 0.36893(2) 0.04524(15) Uani 1 1 d . . . . .
O4 O 0.8339(3) 0.6880(3) 0.30342(12) 0.0647(8) Uani 1 1 d . . . . .
O5 O 1.0733(2) 0.6766(2) 0.43439(11) 0.0481(7) Uani 1 1 d . . . . .
O6 O 1.0073(3) 0.5824(3) 0.66895(12) 0.0703(9) Uani 1 1 d . . . . .
N5 N 0.8279(3) 0.6747(2) 0.42657(13) 0.0398(7) Uani 1 1 d . . . . .
N6 N 0.6335(3) 0.6336(3) 0.46867(14) 0.0495(8) Uani 1 1 d . . . . .
N7 N 1.0902(3) 0.7334(3) 0.30907(13) 0.0453(8) Uani 1 1 d . . . . .
N8 N 1.0965(3) 0.8938(3) 0.39148(15) 0.0547(9) Uani 1 1 d . . . . .
C34 C 0.7161(4) 0.6802(3) 0.30683(18) 0.0509(10) Uani 1 1 d . . . . .
C35 C 0.6487(5) 0.6780(3) 0.2518(2) 0.0664(13) Uani 1 1 d . . . . .
H35 H 0.6893 0.6827 0.2154 0.080 Uiso 1 1 calc R U . . .
C36 C 0.5258(5) 0.6692(4) 0.2509(2) 0.0769(15) Uani 1 1 d . . . . .
H36 H 0.4845 0.6677 0.2140 0.092 Uiso 1 1 calc R U . . .
C37 C 0.4608(5) 0.6624(4) 0.3036(2) 0.0811(16) Uani 1 1 d . . . . .
H37 H 0.3776 0.6578 0.3027 0.097 Uiso 1 1 calc R U . . .
C38 C 0.5230(4) 0.6628(4) 0.3569(2) 0.0672(13) Uani 1 1 d . . . . .
H38 H 0.4801 0.6574 0.3926 0.081 Uiso 1 1 calc R U . . .
C39 C 0.6490(4) 0.6712(3) 0.36014(18) 0.0483(10) Uani 1 1 d . . . . .
C40 C 0.7023(4) 0.6614(3) 0.41934(17) 0.0454(10) Uani 1 1 d . . . . .
C41 C 0.8375(3) 0.6506(3) 0.48558(15) 0.0366(8) Uani 1 1 d . . . . .
C42 C 0.7151(4) 0.6244(3) 0.51062(17) 0.0424(9) Uani 1 1 d . . . . .
C43 C 0.6969(4) 0.5907(3) 0.57003(16) 0.0482(10) Uani 1 1 d . . . . .
H43 H 0.6175 0.5723 0.5872 0.058 Uiso 1 1 calc R U . . .
C44 C 0.7961(4) 0.5850(3) 0.60302(16) 0.0451(10) Uani 1 1 d . . . . .
H44 H 0.7831 0.5630 0.6427 0.054 Uiso 1 1 calc R U . . .
C45 C 0.9176(4) 0.6115(3) 0.57837(15) 0.0405(9) Uani 1 1 d . . . . .
C46 C 0.9389(3) 0.6431(3) 0.51803(15) 0.0356(8) Uani 1 1 d . . . . .
C47 C 1.0577(3) 0.6587(3) 0.48907(16) 0.0375(9) Uani 1 1 d . . . . .
C48 C 1.1602(3) 0.6476(3) 0.52563(16) 0.0389(9) Uani 1 1 d . . . . .
C49 C 1.2757(4) 0.6624(3) 0.49941(18) 0.0500(10) Uani 1 1 d . . . . .
H49 H 1.2889 0.6816 0.4593 0.060 Uiso 1 1 calc R U . . .
C50 C 1.3702(4) 0.6486(3) 0.5329(2) 0.0573(11) Uani 1 1 d . . . . .
H50 H 1.4465 0.6575 0.5152 0.069 Uiso 1 1 calc R U . . .
C51 C 1.3518(4) 0.6217(4) 0.5924(2) 0.0612(12) Uani 1 1 d . . . . .
H51 H 1.4158 0.6122 0.6146 0.073 Uiso 1 1 calc R U . . .
C52 C 1.2395(4) 0.6086(3) 0.61965(18) 0.0537(11) Uani 1 1 d . . . . .
H52 H 1.2289 0.5916 0.6601 0.064 Uiso 1 1 calc R U . . .
C53 C 1.1423(3) 0.6207(3) 0.58646(16) 0.0409(9) Uani 1 1 d . . . . .
C54 C 1.0198(4) 0.6028(3) 0.61544(17) 0.0458(10) Uani 1 1 d . . . . .
C55 C 1.0812(4) 0.6557(4) 0.26574(18) 0.0572(11) Uani 1 1 d . . . . .
H55 H 1.0107 0.5827 0.2646 0.069 Uiso 1 1 calc R U . . .
C56 C 1.1722(5) 0.6784(4) 0.22205(19) 0.0693(14) Uani 1 1 d . . . . .
H56 H 1.1620 0.6218 0.1921 0.083 Uiso 1 1 calc R U . . .
C57 C 1.2768(5) 0.7843(5) 0.2233(2) 0.0657(13) Uani 1 1 d . . . . .
H57 H 1.3381 0.8008 0.1940 0.079 Uiso 1 1 calc R U . . .
C58 C 1.2911(4) 0.8674(4) 0.26859(19) 0.0543(11) Uani 1 1 d . . . . .
C59 C 1.1943(4) 0.8387(3) 0.31064(17) 0.0452(10) Uani 1 1 d . . . . .
C60 C 1.1998(4) 0.9233(3) 0.35624(18) 0.0496(10) Uani 1 1 d . . . . .
C61 C 1.3065(4) 1.0329(4) 0.3609(2) 0.0628(12) Uani 1 1 d . . . . .
C62 C 1.3049(5) 1.1120(4) 0.4059(2) 0.0844(16) Uani 1 1 d . . . . .
H62 H 1.3746 1.1852 0.4114 0.101 Uiso 1 1 calc R U . . .
C63 C 1.2012(6) 1.0818(4) 0.4416(2) 0.0946(18) Uani 1 1 d . . . . .
H63 H 1.1987 1.1334 0.4716 0.114 Uiso 1 1 calc R U . . .
C64 C 1.0992(5) 0.9713(4) 0.4319(2) 0.0755(14) Uani 1 1 d . . . . .
H64 H 1.0280 0.9515 0.4559 0.091 Uiso 1 1 calc R U . . .
C65 C 1.3988(4) 0.9812(5) 0.2743(2) 0.0719(14) Uani 1 1 d . . . . .
H65 H 1.4645 1.0016 0.2470 0.086 Uiso 1 1 calc R U . . .
C66 C 1.4056(5) 1.0582(4) 0.3186(2) 0.0792(15) Uani 1 1 d . . . . .
H66 H 1.4773 1.1305 0.3218 0.095 Uiso 1 1 calc R U . . .
O1S O 0.9226(12) 0.4243(7) 0.1587(4) 0.349(8) Uani 1 1 d . . . . .
C1S C 0.9297(13) 0.3479(10) 0.1766(4) 0.160(4) Uani 1 1 d . . . . .
C2S C 1.0361(10) 0.3251(9) 0.1825(4) 0.193(4) Uani 1 1 d . . . . .
H2S1 H 1.0937 0.3591 0.1506 0.289 Uiso 1 1 calc R U . . .
H2S2 H 1.0075 0.2430 0.1800 0.289 Uiso 1 1 calc R U . . .
H2S3 H 1.0810 0.3575 0.2209 0.289 Uiso 1 1 calc R U . . .
C3S C 0.8144(10) 0.2571(12) 0.2060(6) 0.274(8) Uani 1 1 d . . . . .
H3S1 H 0.8070 0.2862 0.2456 0.411 Uiso 1 1 calc R U . . .
H3S2 H 0.8265 0.1885 0.2093 0.411 Uiso 1 1 calc R U . . .
H3S3 H 0.7366 0.2389 0.1818 0.411 Uiso 1 1 calc R U . . .
O2S O -0.1473(10) 0.0655(9) 0.4173(5) 0.312(5) Uani 1 1 d . . . . .
C4S C -0.2553(13) 0.0272(10) 0.3972(7) 0.195(6) Uani 1 1 d . . . . .
C5S C -0.2720(10) 0.0035(12) 0.3353(6) 0.251(6) Uani 1 1 d . . . . .
H5S1 H -0.2285 0.0741 0.3153 0.377 Uiso 1 1 calc R U . . .
H5S2 H -0.3630 -0.0316 0.3238 0.377 Uiso 1 1 calc R U . . .
H5S3 H -0.2360 -0.0486 0.3239 0.377 Uiso 1 1 calc R U . . .
C6S C -0.3713(13) -0.0047(12) 0.4333(5) 0.270(7) Uani 1 1 d . . . . .
H6S1 H -0.4047 -0.0846 0.4424 0.405 Uiso 1 1 calc R U . . .
H6S2 H -0.4366 0.0069 0.4108 0.405 Uiso 1 1 calc R U . . .
H6S3 H -0.3480 0.0429 0.4704 0.405 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.889(3) . ?
Cu1 O1 1.918(3) . ?
Cu1 N3 2.019(3) . ?
Cu1 O2 2.101(2) . ?
Cu1 N4 2.271(3) . ?
O1 C1 1.320(4) . ?
O2 C14 1.242(4) . ?
O3 C21 1.241(4) . ?
N1 C8 1.359(4) . ?
N1 C7 1.371(4) . ?
N2 C7 1.344(4) . ?
N2 C9 1.369(5) . ?
N3 C22 1.315(5) . ?
N3 C26 1.362(4) . ?
N4 C31 1.318(5) . ?
N4 C27 1.361(5) . ?
C1 C6 1.407(5) . ?
C1 C2 1.415(5) . ?
C2 C3 1.363(5) . ?
C3 C4 1.386(5) . ?
C4 C5 1.358(5) . ?
C5 C6 1.401(5) . ?
C6 C7 1.449(5) . ?
C8 C13 1.393(5) . ?
C8 C9 1.415(5) . ?
C9 C10 1.391(5) . ?
C10 C11 1.376(5) . ?
C11 C12 1.387(5) . ?
C12 C13 1.419(5) . ?
C12 C21 1.459(5) . ?
C13 C14 1.453(5) . ?
C14 C15 1.487(5) . ?
C15 C16 1.375(5) . ?
C15 C20 1.407(5) . ?
C16 C17 1.388(6) . ?
C17 C18 1.387(6) . ?
C18 C19 1.375(6) . ?
C19 C20 1.384(5) . ?
C20 C21 1.480(6) . ?
C22 C23 1.391(5) . ?
C23 C24 1.359(6) . ?
C24 C25 1.395(6) . ?
C25 C26 1.406(5) . ?
C25 C32 1.434(6) . ?
C26 C27 1.426(6) . ?
C27 C28 1.412(6) . ?
C28 C29 1.398(8) . ?
C28 C33 1.408(7) . ?
C29 C30 1.339(8) . ?
C30 C31 1.412(7) . ?
C32 C33 1.328(7) . ?
Cu2 N5 1.880(3) . ?
Cu2 O4 1.910(3) . ?
Cu2 N7 1.991(3) . ?
Cu2 O5 2.143(3) . ?
Cu2 N8 2.226(3) . ?
O4 C34 1.316(5) . ?
O5 C47 1.245(4) . ?
O6 C54 1.223(4) . ?
N5 C41 1.369(4) . ?
N5 C40 1.379(4) . ?
N6 C40 1.331(4) . ?
N6 C42 1.350(4) . ?
N7 C55 1.325(5) . ?
N7 C59 1.354(5) . ?
N8 C64 1.301(5) . ?
N8 C60 1.354(5) . ?
C34 C39 1.406(5) . ?
C34 C35 1.421(5) . ?
C35 C36 1.365(6) . ?
C36 C37 1.386(6) . ?
C37 C38 1.361(6) . ?
C38 C39 1.402(5) . ?
C39 C40 1.467(5) . ?
C41 C46 1.395(5) . ?
C41 C42 1.424(5) . ?
C42 C43 1.395(5) . ?
C43 C44 1.370(5) . ?
C44 C45 1.412(5) . ?
C45 C46 1.409(5) . ?
C45 C54 1.463(5) . ?
C46 C47 1.458(5) . ?
C47 C48 1.474(5) . ?
C48 C49 1.399(5) . ?
C48 C53 1.403(5) . ?
C49 C50 1.379(5) . ?
C50 C51 1.374(6) . ?
C51 C52 1.382(5) . ?
C52 C53 1.391(5) . ?
C53 C54 1.487(5) . ?
C55 C56 1.384(5) . ?
C56 C57 1.362(6) . ?
C57 C58 1.387(6) . ?
C58 C59 1.399(5) . ?
C58 C65 1.440(6) . ?
C59 C60 1.434(5) . ?
C60 C61 1.400(5) . ?
C61 C62 1.401(6) . ?
C61 C66 1.424(6) . ?
C62 C63 1.363(6) . ?
C63 C64 1.390(6) . ?
C65 C66 1.340(6) . ?
O1S C1S 1.113(10) . ?
C1S C2S 1.382(11) . ?
C1S C3S 1.513(15) . ?
O2S C4S 1.180(11) . ?
C4S C5S 1.380(14) . ?
C4S C6S 1.477(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 O1 92.77(11) . . ?
N1 Cu1 N3 170.69(12) . . ?
O1 Cu1 N3 90.71(11) . . ?
N1 Cu1 O2 88.91(11) . . ?
O1 Cu1 O2 174.28(11) . . ?
N3 Cu1 O2 86.83(11) . . ?
N1 Cu1 N4 110.23(13) . . ?
O1 Cu1 N4 102.37(12) . . ?
N3 Cu1 N4 77.37(13) . . ?
O2 Cu1 N4 82.14(11) . . ?
C1 O1 Cu1 127.6(2) . . ?
C14 O2 Cu1 130.4(3) . . ?
C8 N1 C7 105.0(3) . . ?
C8 N1 Cu1 126.3(2) . . ?
C7 N1 Cu1 128.7(2) . . ?
C7 N2 C9 104.1(3) . . ?
C22 N3 C26 117.7(3) . . ?
C22 N3 Cu1 124.7(3) . . ?
C26 N3 Cu1 117.6(3) . . ?
C31 N4 C27 118.6(4) . . ?
C31 N4 Cu1 131.8(4) . . ?
C27 N4 Cu1 109.4(3) . . ?
O1 C1 C6 126.1(3) . . ?
O1 C1 C2 117.1(3) . . ?
C6 C1 C2 116.9(3) . . ?
C3 C2 C1 121.6(4) . . ?
C2 C3 C4 121.3(4) . . ?
C5 C4 C3 118.2(4) . . ?
C4 C5 C6 122.6(4) . . ?
C5 C6 C1 119.5(3) . . ?
C5 C6 C7 118.3(3) . . ?
C1 C6 C7 122.3(3) . . ?
N2 C7 N1 114.1(3) . . ?
N2 C7 C6 123.4(3) . . ?
N1 C7 C6 122.5(3) . . ?
N1 C8 C13 130.3(3) . . ?
N1 C8 C9 107.5(3) . . ?
C13 C8 C9 122.2(3) . . ?
N2 C9 C10 131.4(4) . . ?
N2 C9 C8 109.4(3) . . ?
C10 C9 C8 119.2(4) . . ?
C11 C10 C9 119.0(4) . . ?
C10 C11 C12 122.3(4) . . ?
C11 C12 C13 120.1(4) . . ?
C11 C12 C21 120.0(4) . . ?
C13 C12 C21 119.8(4) . . ?
C8 C13 C12 117.1(3) . . ?
C8 C13 C14 120.9(3) . . ?
C12 C13 C14 122.0(3) . . ?
O2 C14 C13 122.6(3) . . ?
O2 C14 C15 119.4(3) . . ?
C13 C14 C15 118.0(3) . . ?
C16 C15 C20 119.3(4) . . ?
C16 C15 C14 120.1(4) . . ?
C20 C15 C14 120.5(4) . . ?
C15 C16 C17 120.7(4) . . ?
C18 C17 C16 119.7(5) . . ?
C19 C18 C17 120.2(4) . . ?
C18 C19 C20 120.4(4) . . ?
C19 C20 C15 119.7(4) . . ?
C19 C20 C21 119.8(4) . . ?
C15 C20 C21 120.6(4) . . ?
O3 C21 C12 121.3(4) . . ?
O3 C21 C20 119.7(4) . . ?
C12 C21 C20 119.0(3) . . ?
N3 C22 C23 123.4(4) . . ?
C24 C23 C22 119.7(4) . . ?
C23 C24 C25 118.9(4) . . ?
C24 C25 C26 118.0(4) . . ?
C24 C25 C32 123.8(5) . . ?
C26 C25 C32 118.2(5) . . ?
N3 C26 C25 122.2(4) . . ?
N3 C26 C27 117.9(4) . . ?
C25 C26 C27 119.9(4) . . ?
N4 C27 C28 123.1(5) . . ?
N4 C27 C26 117.3(4) . . ?
C28 C27 C26 119.5(4) . . ?
C29 C28 C33 125.6(6) . . ?
C29 C28 C27 115.5(6) . . ?
C33 C28 C27 118.9(5) . . ?
C30 C29 C28 121.8(6) . . ?
C29 C30 C31 119.2(6) . . ?
N4 C31 C30 121.8(5) . . ?
C33 C32 C25 121.4(5) . . ?
C32 C33 C28 122.0(5) . . ?
N5 Cu2 O4 92.59(12) . . ?
N5 Cu2 N7 174.73(12) . . ?
O4 Cu2 N7 88.96(12) . . ?
N5 Cu2 O5 88.27(11) . . ?
O4 Cu2 O5 161.27(11) . . ?
N7 Cu2 O5 88.65(11) . . ?
N5 Cu2 N8 105.35(12) . . ?
O4 Cu2 N8 114.46(13) . . ?
N7 Cu2 N8 78.51(13) . . ?
O5 Cu2 N8 83.21(11) . . ?
C34 O4 Cu2 127.4(3) . . ?
C47 O5 Cu2 130.2(2) . . ?
C41 N5 C40 103.8(3) . . ?
C41 N5 Cu2 127.2(2) . . ?
C40 N5 Cu2 129.0(2) . . ?
C40 N6 C42 104.0(3) . . ?
C55 N7 C59 118.0(3) . . ?
C55 N7 Cu2 124.6(3) . . ?
C59 N7 Cu2 117.3(3) . . ?
C64 N8 C60 117.5(4) . . ?
C64 N8 Cu2 132.9(3) . . ?
C60 N8 Cu2 109.5(3) . . ?
O4 C34 C39 125.9(4) . . ?
O4 C34 C35 117.5(4) . . ?
C39 C34 C35 116.6(4) . . ?
C36 C35 C34 121.5(5) . . ?
C35 C36 C37 121.7(4) . . ?
C38 C37 C36 117.8(5) . . ?
C37 C38 C39 122.7(5) . . ?
C38 C39 C34 119.7(4) . . ?
C38 C39 C40 118.0(4) . . ?
C34 C39 C40 122.2(4) . . ?
N6 C40 N5 115.1(3) . . ?
N6 C40 C39 123.6(3) . . ?
N5 C40 C39 121.2(3) . . ?
N5 C41 C46 130.4(3) . . ?
N5 C41 C42 107.0(3) . . ?
C46 C41 C42 122.5(3) . . ?
N6 C42 C43 131.4(4) . . ?
N6 C42 C41 110.1(3) . . ?
C43 C42 C41 118.5(4) . . ?
C44 C43 C42 119.9(4) . . ?
C43 C44 C45 121.7(3) . . ?
C46 C45 C44 120.1(3) . . ?
C46 C45 C54 120.4(3) . . ?
C44 C45 C54 119.4(3) . . ?
C41 C46 C45 117.3(3) . . ?
C41 C46 C47 121.0(3) . . ?
C45 C46 C47 121.5(3) . . ?
O5 C47 C46 122.3(3) . . ?
O5 C47 C48 119.3(3) . . ?
C46 C47 C48 118.3(3) . . ?
C49 C48 C53 119.5(3) . . ?
C49 C48 C47 119.9(3) . . ?
C53 C48 C47 120.6(3) . . ?
C50 C49 C48 120.1(4) . . ?
C51 C50 C49 120.0(4) . . ?
C50 C51 C52 120.9(4) . . ?
C51 C52 C53 119.9(4) . . ?
C52 C53 C48 119.4(3) . . ?
C52 C53 C54 119.7(3) . . ?
C48 C53 C54 120.9(3) . . ?
O6 C54 C45 121.9(4) . . ?
O6 C54 C53 119.9(4) . . ?
C45 C54 C53 118.1(3) . . ?
N7 C55 C56 122.8(4) . . ?
C57 C56 C55 119.4(5) . . ?
C56 C57 C58 119.5(4) . . ?
C57 C58 C59 117.7(4) . . ?
C57 C58 C65 123.8(4) . . ?
C59 C58 C65 118.4(4) . . ?
N7 C59 C58 122.5(4) . . ?
N7 C59 C60 117.3(3) . . ?
C58 C59 C60 120.2(4) . . ?
N8 C60 C61 122.9(4) . . ?
N8 C60 C59 117.2(3) . . ?
C61 C60 C59 119.8(4) . . ?
C60 C61 C62 116.8(4) . . ?
C60 C61 C66 118.5(5) . . ?
C62 C61 C66 124.6(4) . . ?
C63 C62 C61 120.1(4) . . ?
C62 C63 C64 118.0(5) . . ?
N8 C64 C63 124.6(5) . . ?
C66 C65 C58 120.8(4) . . ?
C65 C66 C61 122.1(4) . . ?
O1S C1S C2S 129.7(16) . . ?
O1S C1S C3S 119.6(14) . . ?
C2S C1S C3S 110.3(11) . . ?
O2S C4S C5S 115.9(17) . . ?
O2S C4S C6S 125.0(16) . . ?
C5S C4S C6S 118.9(11) . . ?

_refine_diff_density_max         0.540
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.070

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

data_6
_database_code_depnum_ccdc_archive 'CCDC 1584243'
_audit_update_record             
;
2017-11-06 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H18 Cu N4 O3'
_chemical_formula_weight         558.03

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   13.703(3)
_cell_length_b                   9.786(2)
_cell_length_c                   20.080(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.637(4)
_cell_angle_gamma                90
_cell_volume                     2566.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    941
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      26.02

_exptl_crystal_description       Plate
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_F_000             1140
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.892
_shelx_estimated_absorpt_T_min   0.690
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6895
_exptl_absorpt_correction_T_max  0.9550
_exptl_absorpt_process_details   
;
 Sheldrick, G.M. SADABS: Program for absorption correction
 using area detector data. University of Göttingen, Germany, 1996.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29261
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.559
_diffrn_reflns_theta_max         26.444
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5270
_reflns_number_gt                3211
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BRUKER Smart'
_computing_cell_refinement       'BRUKER Smart'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5270
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.1014
_refine_ls_wR_factor_gt          0.0858
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_restrained_S_all      0.958
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.25834(3) 0.61170(3) 0.15466(2) 0.03681(13) Uani 1 1 d . . . . .
O1 O 0.28975(16) 0.6501(2) 0.25249(10) 0.0499(6) Uani 1 1 d . . . . .
O2 O 0.20333(15) 0.59334(19) 0.04744(10) 0.0409(5) Uani 1 1 d . . . . .
O3 O -0.04237(18) 0.2203(2) -0.11980(11) 0.0665(7) Uani 1 1 d . . . . .
N1 N 0.19156(16) 0.4470(2) 0.16358(11) 0.0349(6) Uani 1 1 d . . . . .
N2 N 0.13297(18) 0.2648(2) 0.21114(13) 0.0437(6) Uani 1 1 d . . . . .
N3 N 0.31815(17) 0.7932(2) 0.13836(11) 0.0348(6) Uani 1 1 d . . . . .
N4 N 0.42146(19) 0.5576(3) 0.16235(12) 0.0430(6) Uani 1 1 d . . . . .
C1 C 0.2787(2) 0.5699(3) 0.30217(15) 0.0401(7) Uani 1 1 d . . . . .
C2 C 0.3184(2) 0.6158(3) 0.37162(15) 0.0485(8) Uani 1 1 d . . . . .
H2 H 0.3532 0.6986 0.3802 0.058 Uiso 1 1 calc R U . . .
C3 C 0.3073(3) 0.5425(4) 0.42664(17) 0.0613(10) Uani 1 1 d . . . . .
H3 H 0.3337 0.5765 0.4718 0.074 Uiso 1 1 calc R U . . .
C4 C 0.2572(3) 0.4181(4) 0.41595(18) 0.0765(12) Uani 1 1 d . . . . .
H4 H 0.2501 0.3680 0.4535 0.092 Uiso 1 1 calc R U . . .
C5 C 0.2185(3) 0.3703(4) 0.34944(16) 0.0609(10) Uani 1 1 d . . . . .
H5 H 0.1841 0.2871 0.3422 0.073 Uiso 1 1 calc R U . . .
C6 C 0.2288(2) 0.4421(3) 0.29186(15) 0.0403(7) Uani 1 1 d . . . . .
C7 C 0.1853(2) 0.3828(3) 0.22277(14) 0.0373(7) Uani 1 1 d . . . . .
C8 C 0.1365(2) 0.3663(3) 0.11014(14) 0.0343(7) Uani 1 1 d . . . . .
C9 C 0.1002(2) 0.2535(3) 0.14006(16) 0.0403(7) Uani 1 1 d . . . . .
C10 C 0.0369(2) 0.1578(3) 0.09626(17) 0.0489(8) Uani 1 1 d . . . . .
H10 H 0.0121 0.0830 0.1146 0.059 Uiso 1 1 calc R U . . .
C11 C 0.0124(2) 0.1763(3) 0.02581(17) 0.0486(8) Uani 1 1 d . . . . .
H11 H -0.0303 0.1127 -0.0034 0.058 Uiso 1 1 calc R U . . .
C12 C 0.0481(2) 0.2861(3) -0.00471(15) 0.0390(7) Uani 1 1 d . . . . .
C13 C 0.11259(19) 0.3848(3) 0.03837(14) 0.0326(6) Uani 1 1 d . . . . .
C14 C 0.1493(2) 0.5026(3) 0.00929(14) 0.0343(7) Uani 1 1 d . . . . .
C15 C 0.1217(2) 0.5159(3) -0.06724(14) 0.0362(7) Uani 1 1 d . . . . .
C16 C 0.1583(2) 0.6241(3) -0.09727(15) 0.0458(8) Uani 1 1 d . . . . .
H16 H 0.2010 0.6887 -0.0688 0.055 Uiso 1 1 calc R U . . .
C17 C 0.1320(2) 0.6370(3) -0.16910(16) 0.0529(9) Uani 1 1 d . . . . .
H17 H 0.1567 0.7102 -0.1888 0.063 Uiso 1 1 calc R U . . .
C18 C 0.0695(2) 0.5419(3) -0.21135(16) 0.0516(9) Uani 1 1 d . . . . .
H18 H 0.0518 0.5507 -0.2597 0.062 Uiso 1 1 calc R U . . .
C19 C 0.0326(2) 0.4332(3) -0.18245(16) 0.0473(8) Uani 1 1 d . . . . .
H19 H -0.0096 0.3691 -0.2115 0.057 Uiso 1 1 calc R U . . .
C20 C 0.0577(2) 0.4183(3) -0.11083(15) 0.0370(7) Uani 1 1 d . . . . .
C21 C 0.0165(2) 0.3012(3) -0.08126(15) 0.0429(7) Uani 1 1 d . . . . .
C22 C 0.2629(2) 0.9076(3) 0.12220(16) 0.0447(8) Uani 1 1 d . . . . .
H22 H 0.1937 0.9044 0.1189 0.054 Uiso 1 1 calc R U . . .
C23 C 0.3038(3) 1.0295(3) 0.11038(16) 0.0530(9) Uani 1 1 d . . . . .
H23 H 0.2633 1.1075 0.0998 0.064 Uiso 1 1 calc R U . . .
C24 C 0.4049(3) 1.0344(3) 0.11443(18) 0.0585(9) Uani 1 1 d . . . . .
H24 H 0.4341 1.1158 0.1060 0.070 Uiso 1 1 calc R U . . .
C25 C 0.4630(3) 0.9179(3) 0.13106(17) 0.0513(8) Uani 1 1 d . . . . .
H25 H 0.5319 0.9197 0.1336 0.062 Uiso 1 1 calc R U . . .
C26 C 0.4192(2) 0.7988(3) 0.14398(14) 0.0377(7) Uani 1 1 d . . . . .
C27 C 0.4771(2) 0.6699(3) 0.16452(14) 0.0405(7) Uani 1 1 d . . . . .
C28 C 0.5833(3) 0.6654(4) 0.18551(17) 0.0632(10) Uani 1 1 d . . . . .
H28 H 0.6209 0.7452 0.1873 0.076 Uiso 1 1 calc R U . . .
C29 C 0.6322(3) 0.5433(5) 0.20341(19) 0.0755(12) Uani 1 1 d . . . . .
H29 H 0.7034 0.5392 0.2174 0.091 Uiso 1 1 calc R U . . .
C30 C 0.5762(3) 0.4278(4) 0.20072(17) 0.0697(12) Uani 1 1 d . . . . .
H30 H 0.6081 0.3434 0.2122 0.084 Uiso 1 1 calc R U . . .
C31 C 0.4706(3) 0.4383(4) 0.18053(16) 0.0587(9) Uani 1 1 d . . . . .
H31 H 0.4321 0.3596 0.1795 0.070 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.888(2) . ?
Cu1 O1 1.9164(19) . ?
Cu1 N3 2.024(2) . ?
Cu1 O2 2.0622(19) . ?
Cu1 N4 2.256(2) . ?
O1 C1 1.313(3) . ?
O2 C14 1.257(3) . ?
O3 C21 1.224(3) . ?
N1 C8 1.362(3) . ?
N1 C7 1.370(3) . ?
N2 C7 1.342(3) . ?
N2 C9 1.365(4) . ?
N3 C22 1.336(3) . ?
N3 C26 1.356(3) . ?
N4 C27 1.330(4) . ?
N4 C31 1.342(4) . ?
C1 C2 1.408(4) . ?
C1 C6 1.411(4) . ?
C2 C3 1.364(4) . ?
C3 C4 1.381(5) . ?
C4 C5 1.362(4) . ?
C5 C6 1.396(4) . ?
C6 C7 1.454(4) . ?
C8 C13 1.390(4) . ?
C8 C9 1.417(4) . ?
C9 C10 1.392(4) . ?
C10 C11 1.363(4) . ?
C11 C12 1.397(4) . ?
C12 C13 1.414(4) . ?
C12 C21 1.473(4) . ?
C13 C14 1.450(4) . ?
C14 C15 1.473(4) . ?
C15 C16 1.386(4) . ?
C15 C20 1.408(4) . ?
C16 C17 1.382(4) . ?
C17 C18 1.371(4) . ?
C18 C19 1.379(4) . ?
C19 C20 1.381(4) . ?
C20 C21 1.479(4) . ?
C22 C23 1.368(4) . ?
C23 C24 1.364(4) . ?
C24 C25 1.373(4) . ?
C25 C26 1.371(4) . ?
C26 C27 1.481(4) . ?
C27 C28 1.388(4) . ?
C28 C29 1.363(5) . ?
C29 C30 1.359(5) . ?
C30 C31 1.383(5) . ?

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 Cu1 O1 91.99(9) . . ?
N1 Cu1 N3 174.81(9) . . ?
O1 Cu1 N3 91.02(8) . . ?
N1 Cu1 O2 89.44(8) . . ?
O1 Cu1 O2 169.99(9) . . ?
N3 Cu1 O2 86.87(8) . . ?
N1 Cu1 N4 106.98(9) . . ?
O1 Cu1 N4 93.76(9) . . ?
N3 Cu1 N4 77.02(9) . . ?
O2 Cu1 N4 95.29(8) . . ?
C1 O1 Cu1 128.31(19) . . ?
C14 O2 Cu1 131.26(18) . . ?
C8 N1 C7 104.6(2) . . ?
C8 N1 Cu1 126.10(19) . . ?
C7 N1 Cu1 129.29(19) . . ?
C7 N2 C9 104.0(2) . . ?
C22 N3 C26 118.4(2) . . ?
C22 N3 Cu1 123.19(19) . . ?
C26 N3 Cu1 118.40(19) . . ?
C27 N4 C31 118.3(3) . . ?
C27 N4 Cu1 110.78(19) . . ?
C31 N4 Cu1 128.9(2) . . ?
O1 C1 C2 117.6(3) . . ?
O1 C1 C6 125.5(3) . . ?
C2 C1 C6 116.9(3) . . ?
C3 C2 C1 122.0(3) . . ?
C2 C3 C4 120.6(3) . . ?
C5 C4 C3 118.9(3) . . ?
C4 C5 C6 122.2(3) . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 C7 118.3(3) . . ?
C1 C6 C7 122.2(3) . . ?
N2 C7 N1 114.5(2) . . ?
N2 C7 C6 123.5(3) . . ?
N1 C7 C6 122.0(3) . . ?
N1 C8 C13 129.9(3) . . ?
N1 C8 C9 107.5(2) . . ?
C13 C8 C9 122.6(3) . . ?
N2 C9 C10 131.3(3) . . ?
N2 C9 C8 109.4(2) . . ?
C10 C9 C8 119.2(3) . . ?
C11 C10 C9 118.5(3) . . ?
C10 C11 C12 123.3(3) . . ?
C11 C12 C13 119.6(3) . . ?
C11 C12 C21 120.3(3) . . ?
C13 C12 C21 120.1(3) . . ?
C8 C13 C12 116.9(3) . . ?
C8 C13 C14 121.3(2) . . ?
C12 C13 C14 121.7(3) . . ?
O2 C14 C13 121.9(3) . . ?
O2 C14 C15 119.4(3) . . ?
C13 C14 C15 118.7(2) . . ?
C16 C15 C20 119.2(3) . . ?
C16 C15 C14 120.6(3) . . ?
C20 C15 C14 120.2(3) . . ?
C17 C16 C15 120.6(3) . . ?
C18 C17 C16 120.0(3) . . ?
C17 C18 C19 120.2(3) . . ?
C18 C19 C20 120.8(3) . . ?
C19 C20 C15 119.1(3) . . ?
C19 C20 C21 119.7(3) . . ?
C15 C20 C21 121.2(3) . . ?
O3 C21 C12 121.6(3) . . ?
O3 C21 C20 120.4(3) . . ?
C12 C21 C20 118.0(2) . . ?
N3 C22 C23 122.7(3) . . ?
C24 C23 C22 118.8(3) . . ?
C23 C24 C25 119.3(3) . . ?
C26 C25 C24 119.8(3) . . ?
N3 C26 C25 120.9(3) . . ?
N3 C26 C27 115.9(2) . . ?
C25 C26 C27 123.2(3) . . ?
N4 C27 C28 121.5(3) . . ?
N4 C27 C26 116.2(2) . . ?
C28 C27 C26 122.4(3) . . ?
C29 C28 C27 119.6(4) . . ?
C30 C29 C28 119.5(4) . . ?
C29 C30 C31 118.5(4) . . ?
N4 C31 C30 122.6(4) . . ?

_refine_diff_density_max         0.325
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.056

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.500 143 30 ' '
2 0.500 0.500 0.000 143 30 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?



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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1584241'
_audit_update_record             
;
2017-11-06 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C255 H176 N32 Ni8 O33'
_chemical_formula_weight         4685.95

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'
N N 0.0311 0.0180 '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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.0581(5)
_cell_length_b                   21.9334(9)
_cell_length_c                   22.0213(9)
_cell_angle_alpha                62.112(2)
_cell_angle_beta                 87.140(2)
_cell_angle_gamma                73.869(2)
_cell_volume                     5331.3(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    13758
_cell_measurement_theta_min      0.88
_cell_measurement_theta_max      65.08

_exptl_crystal_description       Prism
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             2418
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.438
_shelx_estimated_absorpt_T_min   0.633
_shelx_estimated_absorpt_T_max   0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_process_details   
;
 Sheldrick, G.M. SADABS: Program for absorption correction
 using area detector data. University of Göttingen, Germany, 1996.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'FR591-KappaCCD2000 Bruker-Nonius'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46717
_diffrn_reflns_av_unetI/netI     0.1144
_diffrn_reflns_av_R_equivalents  0.2007
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.380
_diffrn_reflns_theta_max         65.139
_diffrn_reflns_theta_full        58.930
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             16951
_reflns_number_gt                14466
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Nonius Collect - HKL2000'
_computing_cell_refinement       'Nonius Collect - HKL2000'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1613P)²+4.2754P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0119(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         16951
_refine_ls_number_parameters     1512
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0903
_refine_ls_wR_factor_ref         0.2578
_refine_ls_wR_factor_gt          0.2434
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.33224(5) 0.15105(3) 0.10975(3) 0.0444(2) Uani 1 1 d . . . . .
Ni2 Ni 0.21554(5) 0.31158(3) 0.00942(3) 0.0456(2) Uani 1 1 d . . . . .
O1 O 0.2538(2) 0.21031(14) 0.01218(14) 0.0480(6) Uani 1 1 d . . . . .
O2 O 0.4222(2) 0.10299(14) 0.20747(14) 0.0487(6) Uani 1 1 d . . . . .
O3 O 0.8370(3) 0.04941(17) 0.28053(18) 0.0665(8) Uani 1 1 d . . . . .
O4 O 0.3065(2) 0.25314(14) 0.10201(13) 0.0454(6) Uani 1 1 d . . . . .
O5 O 0.1352(2) 0.36625(15) -0.09082(14) 0.0534(7) Uani 1 1 d . . . . .
O6 O 0.2819(3) 0.44755(19) -0.34230(17) 0.0788(11) Uani 1 1 d . . . . .
N1 N 0.4688(3) 0.14829(17) 0.06807(17) 0.0450(7) Uani 1 1 d . . . . .
N2 N 0.5921(3) 0.15941(18) -0.01103(19) 0.0530(8) Uani 1 1 d . . . . .
N3 N 0.3101(3) 0.05849(18) 0.11091(17) 0.0529(8) Uani 1 1 d . . . . .
N4 N 0.2006(3) 0.13813(18) 0.16474(17) 0.0488(8) Uani 1 1 d . . . . .
N5 N 0.3444(3) 0.33555(17) -0.03361(17) 0.0467(7) Uani 1 1 d . . . . .
N6 N 0.5156(3) 0.34283(19) -0.04903(19) 0.0548(8) Uani 1 1 d . . . . .
N7 N 0.1618(3) 0.39718(19) 0.03087(19) 0.0576(9) Uani 1 1 d . . . . .
N8 N 0.0687(3) 0.2994(2) 0.04640(18) 0.0569(9) Uani 1 1 d . . . . .
C1 C 0.2933(3) 0.2055(2) -0.0437(2) 0.0495(9) Uani 1 1 d . . . . .
C2 C 0.2191(4) 0.2212(2) -0.0969(2) 0.0561(10) Uani 1 1 d . . . . .
H2 H 0.1448 0.2314 -0.0911 0.067 Uiso 1 1 calc R U . . .
C3 C 0.2535(4) 0.2220(2) -0.1576(2) 0.0628(11) Uani 1 1 d . . . . .
H3 H 0.2020 0.2335 -0.1931 0.075 Uiso 1 1 calc R U . . .
C4 C 0.3607(4) 0.2065(3) -0.1676(2) 0.0635(12) Uani 1 1 d . . . . .
H4 H 0.3832 0.2076 -0.2098 0.076 Uiso 1 1 calc R U . . .
C5 C 0.4347(4) 0.1892(2) -0.1155(2) 0.0574(10) Uani 1 1 d . . . . .
H5 H 0.5087 0.1788 -0.1223 0.069 Uiso 1 1 calc R U . . .
C6 C 0.4035(4) 0.1866(2) -0.0519(2) 0.0507(9) Uani 1 1 d . . . . .
C7 C 0.4886(3) 0.1661(2) 0.0009(2) 0.0480(9) Uani 1 1 d . . . . .
C8 C 0.5665(3) 0.1303(2) 0.1009(2) 0.0478(9) Uani 1 1 d . . . . .
C9 C 0.6427(3) 0.1377(2) 0.0521(2) 0.0527(10) Uani 1 1 d . . . . .
C10 C 0.7506(4) 0.1232(2) 0.0721(3) 0.0599(11) Uani 1 1 d . . . . .
H10 H 0.8028 0.1280 0.0399 0.072 Uiso 1 1 calc R U . . .
C11 C 0.7784(4) 0.1017(2) 0.1405(3) 0.0604(11) Uani 1 1 d . . . . .
H11 H 0.8514 0.0913 0.1548 0.073 Uiso 1 1 calc R U . . .
C12 C 0.7043(3) 0.0945(2) 0.1892(2) 0.0533(10) Uani 1 1 d . . . . .
C13 C 0.5948(3) 0.1087(2) 0.1700(2) 0.0472(9) Uani 1 1 d . . . . .
C14 C 0.5164(3) 0.09930(19) 0.2206(2) 0.0467(9) Uani 1 1 d . . . . .
C15 C 0.5496(3) 0.0858(2) 0.2906(2) 0.0499(9) Uani 1 1 d . . . . .
C16 C 0.4739(4) 0.0898(2) 0.3359(2) 0.0565(10) Uani 1 1 d . . . . .
H16 H 0.4000 0.1015 0.3225 0.068 Uiso 1 1 calc R U . . .
C17 C 0.5063(4) 0.0767(3) 0.4011(2) 0.0643(11) Uani 1 1 d . . . . .
H17 H 0.4542 0.0789 0.4323 0.077 Uiso 1 1 calc R U . . .
C18 C 0.6127(4) 0.0607(3) 0.4211(3) 0.0664(12) Uani 1 1 d . . . . .
H18 H 0.6335 0.0522 0.4658 0.080 Uiso 1 1 calc R U . . .
C19 C 0.6899(4) 0.0570(2) 0.3761(3) 0.0626(12) Uani 1 1 d . . . . .
H19 H 0.7634 0.0453 0.3901 0.075 Uiso 1 1 calc R U . . .
C20 C 0.6584(4) 0.0706(2) 0.3101(2) 0.0538(10) Uani 1 1 d . . . . .
C21 C 0.7404(3) 0.0703(2) 0.2609(2) 0.0560(10) Uani 1 1 d . . . . .
C22 C 0.3674(5) 0.0241(2) 0.0778(2) 0.0662(12) Uani 1 1 d . . . . .
H22 H 0.4336 0.0328 0.0623 0.079 Uiso 1 1 calc R U . . .
C23 C 0.3319(6) -0.0238(3) 0.0656(3) 0.0801(17) Uani 1 1 d . . . . .
H23 H 0.3745 -0.0489 0.0435 0.096 Uiso 1 1 calc R U . . .
C24 C 0.2334(6) -0.0345(3) 0.0864(3) 0.0889(19) Uani 1 1 d . . . . .
H24 H 0.2062 -0.0657 0.0773 0.107 Uiso 1 1 calc R U . . .
C25 C 0.1758(5) 0.0010(3) 0.1205(3) 0.0804(16) Uani 1 1 d . . . . .
H25 H 0.1085 -0.0058 0.1356 0.096 Uiso 1 1 calc R U . . .
C26 C 0.2159(4) 0.0463(2) 0.1327(2) 0.0587(11) Uani 1 1 d . . . . .
C27 C 0.1607(4) 0.0860(2) 0.1706(2) 0.0570(11) Uani 1 1 d . . . . .
C28 C 0.0762(4) 0.0698(3) 0.2105(3) 0.0704(14) Uani 1 1 d . . . . .
H28 H 0.0491 0.0322 0.2145 0.084 Uiso 1 1 calc R U . . .
C29 C 0.0323(4) 0.1094(3) 0.2444(2) 0.0706(13) Uani 1 1 d . . . . .
H29 H -0.0255 0.0994 0.2717 0.085 Uiso 1 1 calc R U . . .
C30 C 0.0727(4) 0.1623(3) 0.2383(2) 0.0654(12) Uani 1 1 d . . . . .
H30 H 0.0432 0.1902 0.2608 0.079 Uiso 1 1 calc R U . . .
C31 C 0.1581(3) 0.1755(2) 0.1984(2) 0.0523(9) Uani 1 1 d . . . . .
H31 H 0.1871 0.2120 0.1950 0.063 Uiso 1 1 calc R U . . .
C32 C 0.3877(3) 0.2710(2) 0.1170(2) 0.0460(9) Uani 1 1 d . . . . .
C33 C 0.4051(3) 0.2578(2) 0.1854(2) 0.0499(9) Uani 1 1 d . . . . .
H33 H 0.3553 0.2409 0.2174 0.060 Uiso 1 1 calc R U . . .
C34 C 0.4925(4) 0.2689(2) 0.2069(2) 0.0551(10) Uani 1 1 d . . . . .
H34 H 0.5024 0.2589 0.2535 0.066 Uiso 1 1 calc R U . . .
C35 C 0.5657(4) 0.2945(2) 0.1615(3) 0.0604(11) Uani 1 1 d . . . . .
H35 H 0.6269 0.3008 0.1768 0.072 Uiso 1 1 calc R U . . .
C36 C 0.5485(3) 0.3108(2) 0.0933(2) 0.0539(10) Uani 1 1 d . . . . .
H36 H 0.5983 0.3291 0.0618 0.065 Uiso 1 1 calc R U . . .
C37 C 0.4593(3) 0.3011(2) 0.0694(2) 0.0492(9) Uani 1 1 d . . . . .
C38 C 0.4414(3) 0.3252(2) -0.0043(2) 0.0486(9) Uani 1 1 d . . . . .
C39 C 0.3570(3) 0.3623(2) -0.1026(2) 0.0497(9) Uani 1 1 d . . . . .
C40 C 0.4643(4) 0.3657(2) -0.1117(2) 0.0550(10) Uani 1 1 d . . . . .
C41 C 0.5001(4) 0.3897(3) -0.1770(2) 0.0646(12) Uani 1 1 d . . . . .
H41 H 0.5715 0.3923 -0.1839 0.078 Uiso 1 1 calc R U . . .
C42 C 0.4274(4) 0.4099(3) -0.2322(2) 0.0641(12) Uani 1 1 d . . . . .
H42 H 0.4508 0.4262 -0.2772 0.077 Uiso 1 1 calc R U . . .
C43 C 0.3220(4) 0.4073(2) -0.2240(2) 0.0568(11) Uani 1 1 d . . . . .
C44 C 0.2835(4) 0.3838(2) -0.1577(2) 0.0511(9) Uani 1 1 d . . . . .
C45 C 0.1722(4) 0.3846(2) -0.1485(2) 0.0535(10) Uani 1 1 d . . . . .
C46 C 0.0982(4) 0.4097(2) -0.2093(2) 0.0605(11) Uani 1 1 d . . . . .
C47 C -0.0080(4) 0.4119(3) -0.2017(3) 0.0685(13) Uani 1 1 d . . . . .
H47 H -0.0326 0.3950 -0.1570 0.082 Uiso 1 1 calc R U . . .
C48 C -0.0798(5) 0.4393(3) -0.2598(3) 0.0792(15) Uani 1 1 d . . . . .
H48 H -0.1535 0.4425 -0.2546 0.095 Uiso 1 1 calc R U . . .
C49 C -0.0437(5) 0.4614(3) -0.3245(3) 0.0773(15) Uani 1 1 d . . . . .
H49 H -0.0921 0.4790 -0.3637 0.093 Uiso 1 1 calc R U . . .
C50 C 0.0643(5) 0.4580(3) -0.3322(3) 0.0731(14) Uani 1 1 d . . . . .
H50 H 0.0889 0.4735 -0.3768 0.088 Uiso 1 1 calc R U . . .
C51 C 0.1361(4) 0.4320(2) -0.2753(2) 0.0612(11) Uani 1 1 d . . . . .
C52 C 0.2494(4) 0.4303(2) -0.2847(2) 0.0659(13) Uani 1 1 d . . . . .
C53 C 0.2148(5) 0.4445(2) 0.0217(3) 0.0677(13) Uani 1 1 d . . . . .
H53 H 0.2759 0.4449 -0.0036 0.081 Uiso 1 1 calc R U . . .
C54 C 0.1846(7) 0.4932(3) 0.0476(3) 0.095(2) Uani 1 1 d . . . . .
H54 H 0.2254 0.5248 0.0425 0.114 Uiso 1 1 calc R U . . .
C55 C 0.0911(9) 0.4936(4) 0.0817(4) 0.146(4) Uani 1 1 d . . . . .
H55 H 0.0663 0.5267 0.0993 0.175 Uiso 1 1 calc R U . . .
C56 C 0.0352(8) 0.4462(4) 0.0896(4) 0.134(4) Uani 1 1 d . . . . .
H56 H -0.0289 0.4469 0.1120 0.160 Uiso 1 1 calc R U . . .
C57 C 0.0724(5) 0.3974(3) 0.0650(3) 0.0769(15) Uani 1 1 d . . . . .
C58 C 0.0183(4) 0.3454(3) 0.0703(3) 0.0724(15) Uani 1 1 d . . . . .
C59 C -0.0806(5) 0.3433(3) 0.0960(3) 0.098(2) Uani 1 1 d . . . . .
H59 H -0.1155 0.3755 0.1130 0.117 Uiso 1 1 calc R U . . .
C60 C -0.1277(5) 0.2942(4) 0.0965(3) 0.101(2) Uani 1 1 d . . . . .
H60 H -0.1944 0.2914 0.1153 0.121 Uiso 1 1 calc R U . . .
C61 C -0.0782(4) 0.2497(3) 0.0701(3) 0.0820(16) Uani 1 1 d . . . . .
H61 H -0.1112 0.2169 0.0684 0.098 Uiso 1 1 calc R U . . .
C62 C 0.0218(4) 0.2531(3) 0.0457(2) 0.0648(12) Uani 1 1 d . . . . .
H62 H 0.0573 0.2215 0.0280 0.078 Uiso 1 1 calc R U . . .
Ni3 Ni 0.87189(5) 0.16256(3) 0.59967(3) 0.0440(2) Uani 1 1 d . . . . .
Ni4 Ni 0.73443(6) 0.32023(4) 0.50596(3) 0.0491(2) Uani 1 1 d . . . . .
O101 O 0.7702(2) 0.21824(14) 0.51085(14) 0.0468(6) Uani 1 1 d . . . . .
O102 O 0.9835(2) 0.11690(15) 0.68571(14) 0.0485(6) Uani 1 1 d . . . . .
O103 O 1.4098(3) 0.0712(2) 0.7135(2) 0.0781(10) Uani 1 1 d . . . . .
O104 O 0.8459(2) 0.26497(14) 0.58986(14) 0.0493(6) Uani 1 1 d . . . . .
O105 O 0.6339(3) 0.36964(16) 0.41307(15) 0.0611(8) Uani 1 1 d . . . . .
O106 O 0.7221(6) 0.4477(3) 0.1494(2) 0.128(2) Uani 1 1 d . . . . .
N101 N 0.9929(3) 0.16553(17) 0.54160(17) 0.0455(7) Uani 1 1 d . . . . .
N102 N 1.0922(3) 0.17591(18) 0.45133(18) 0.0532(8) Uani 1 1 d . . . . .
N103 N 0.8534(3) 0.06665(17) 0.60984(17) 0.0482(7) Uani 1 1 d . . . . .
N104 N 0.7561(3) 0.14493(17) 0.66826(17) 0.0472(7) Uani 1 1 d . . . . .
N105 N 0.8511(3) 0.34936(18) 0.4485(2) 0.0555(9) Uani 1 1 d . . . . .
N106 N 1.0174(4) 0.3599(3) 0.4168(3) 0.0830(14) Uani 1 1 d . . . . .
N107 N 0.6848(3) 0.4074(2) 0.52601(19) 0.0619(10) Uani 1 1 d . . . . .
N108 N 0.5988(3) 0.3027(2) 0.55627(18) 0.0562(9) Uani 1 1 d . . . . .
C101 C 0.7921(3) 0.2120(2) 0.4536(2) 0.0480(9) Uani 1 1 d . . . . .
C102 C 0.7066(4) 0.2215(2) 0.4112(2) 0.0558(10) Uani 1 1 d . . . . .
H102 H 0.6364 0.2286 0.4256 0.067 Uiso 1 1 calc R U . . .
C103 C 0.7214(4) 0.2206(2) 0.3486(2) 0.0617(11) Uani 1 1 d . . . . .
H103 H 0.6617 0.2275 0.3207 0.074 Uiso 1 1 calc R U . . .
C104 C 0.8232(4) 0.2097(3) 0.3268(3) 0.0644(12) Uani 1 1 d . . . . .
H104 H 0.8336 0.2102 0.2836 0.077 Uiso 1 1 calc R U . . .
C105 C 0.9088(4) 0.1983(2) 0.3683(2) 0.0580(11) Uani 1 1 d . . . . .
H105 H 0.9784 0.1902 0.3532 0.070 Uiso 1 1 calc R U . . .
C106 C 0.8980(3) 0.1981(2) 0.4327(2) 0.0489(9) Uani 1 1 d . . . . .
C107 C 0.9935(3) 0.1817(2) 0.4738(2) 0.0460(8) Uani 1 1 d . . . . .
C108 C 1.0976(3) 0.1476(2) 0.5645(2) 0.0467(9) Uani 1 1 d . . . . .
C109 C 1.1588(3) 0.1552(2) 0.5073(2) 0.0512(9) Uani 1 1 d . . . . .
C110 C 1.2702(3) 0.1392(2) 0.5166(3) 0.0572(10) Uani 1 1 d . . . . .
H110 H 1.3129 0.1428 0.4795 0.069 Uiso 1 1 calc R U . . .
C111 C 1.3165(3) 0.1180(2) 0.5812(3) 0.0604(11) Uani 1 1 d . . . . .
H111 H 1.3919 0.1078 0.5878 0.072 Uiso 1 1 calc R U . . .
C112 C 1.2558(3) 0.1111(2) 0.6373(3) 0.0555(10) Uani 1 1 d . . . . .
C113 C 1.1435(3) 0.1253(2) 0.6297(2) 0.0497(9) Uani 1 1 d . . . . .
C114 C 1.0807(3) 0.1125(2) 0.6890(2) 0.0496(9) Uani 1 1 d . . . . .
C115 C 1.1347(4) 0.0924(2) 0.7559(2) 0.0560(10) Uani 1 1 d . . . . .
C116 C 1.0754(4) 0.0860(2) 0.8115(2) 0.0635(11) Uani 1 1 d . . . . .
H116 H 1.0001 0.0949 0.8063 0.076 Uiso 1 1 calc R U . . .
C117 C 1.1249(5) 0.0668(3) 0.8747(3) 0.0749(14) Uani 1 1 d . . . . .
H117 H 1.0841 0.0626 0.9126 0.090 Uiso 1 1 calc R U . . .
C118 C 1.2351(5) 0.0538(3) 0.8817(3) 0.0775(15) Uani 1 1 d . . . . .
H118 H 1.2696 0.0408 0.9247 0.093 Uiso 1 1 calc R U . . .
C119 C 1.2945(4) 0.0593(3) 0.8276(3) 0.0695(13) Uani 1 1 d . . . . .
H119 H 1.3699 0.0493 0.8337 0.083 Uiso 1 1 calc R U . . .
C120 C 1.2457(4) 0.0795(2) 0.7635(2) 0.0582(11) Uani 1 1 d . . . . .
C121 C 1.3111(4) 0.0864(2) 0.7050(3) 0.0602(11) Uani 1 1 d . . . . .
C122 C 0.9050(4) 0.0303(2) 0.5770(2) 0.0559(10) Uani 1 1 d . . . . .
H122 H 0.9672 0.0412 0.5557 0.067 Uiso 1 1 calc R U . . .
C123 C 0.8716(4) -0.0224(2) 0.5730(2) 0.0598(11) Uani 1 1 d . . . . .
H123 H 0.9104 -0.0476 0.5498 0.072 Uiso 1 1 calc R U . . .
C124 C 0.7804(4) -0.0376(2) 0.6035(3) 0.0645(12) Uani 1 1 d . . . . .
H124 H 0.7544 -0.0726 0.6005 0.077 Uiso 1 1 calc R U . . .
C125 C 0.7272(4) -0.0013(2) 0.6384(2) 0.0595(11) Uani 1 1 d . . . . .
H125 H 0.6651 -0.0116 0.6603 0.071 Uiso 1 1 calc R U . . .
C126 C 0.7656(3) 0.0501(2) 0.6410(2) 0.0496(9) Uani 1 1 d . . . . .
C127 C 0.7166(3) 0.0906(2) 0.6786(2) 0.0495(9) Uani 1 1 d . . . . .
C128 C 0.6358(3) 0.0740(2) 0.7220(2) 0.0574(10) Uani 1 1 d . . . . .
H128 H 0.6081 0.0360 0.7281 0.069 Uiso 1 1 calc R U . . .
C129 C 0.5970(4) 0.1138(3) 0.7558(2) 0.0610(11) Uani 1 1 d . . . . .
H129 H 0.5411 0.1041 0.7850 0.073 Uiso 1 1 calc R U . . .
C130 C 0.6399(4) 0.1678(3) 0.7470(2) 0.0594(11) Uani 1 1 d . . . . .
H130 H 0.6158 0.1945 0.7713 0.071 Uiso 1 1 calc R U . . .
C131 C 0.7188(3) 0.1827(2) 0.7021(2) 0.0520(9) Uani 1 1 d . . . . .
H131 H 0.7472 0.2208 0.6952 0.062 Uiso 1 1 calc R U . . .
C132 C 0.9285(3) 0.2874(2) 0.5963(2) 0.0544(10) Uani 1 1 d . . . . .
C133 C 0.9620(4) 0.2740(3) 0.6612(3) 0.0643(12) Uani 1 1 d . . . . .
H133 H 0.9254 0.2500 0.6996 0.077 Uiso 1 1 calc R U . . .
C134 C 1.0472(4) 0.2948(3) 0.6716(4) 0.0826(17) Uani 1 1 d . . . . .
H134 H 1.0681 0.2852 0.7166 0.099 Uiso 1 1 calc R U . . .
C135 C 1.1033(4) 0.3298(3) 0.6165(4) 0.0880(18) Uani 1 1 d . . . . .
H135 H 1.1619 0.3442 0.6235 0.106 Uiso 1 1 calc R U . . .
C136 C 1.0716(4) 0.3430(3) 0.5520(4) 0.0798(16) Uani 1 1 d . . . . .
H136 H 1.1103 0.3660 0.5145 0.096 Uiso 1 1 calc R U . . .
C137 C 0.9837(4) 0.3236(2) 0.5392(3) 0.0636(12) Uani 1 1 d . . . . .
C138 C 0.9520(4) 0.3430(2) 0.4687(3) 0.0660(13) Uani 1 1 d . . . . .
C139 C 0.8484(4) 0.3722(2) 0.3793(3) 0.0656(13) Uani 1 1 d . . . . .
C140 C 0.9523(6) 0.3784(3) 0.3598(3) 0.0854(19) Uani 1 1 d . . . . .
C141 C 0.9671(8) 0.4042(4) 0.2881(4) 0.121(3) Uani 1 1 d . . . . .
H141 H 1.0340 0.4109 0.2720 0.145 Uiso 1 1 calc R U . . .
C142 C 0.8852(8) 0.4189(4) 0.2432(4) 0.118(3) Uani 1 1 d . . . . .
H142 H 0.8973 0.4347 0.1960 0.142 Uiso 1 1 calc R U . . .
C143 C 0.7868(6) 0.4123(3) 0.2623(3) 0.0872(19) Uani 1 1 d . . . . .
C144 C 0.7645(5) 0.3890(2) 0.3328(2) 0.0710(15) Uani 1 1 d . . . . .
C145 C 0.6567(4) 0.3863(2) 0.3528(2) 0.0648(12) Uani 1 1 d . . . . .
C146 C 0.5700(6) 0.4048(2) 0.3002(2) 0.0739(16) Uani 1 1 d . . . . .
C147 C 0.4700(5) 0.4003(3) 0.3183(3) 0.0794(16) Uani 1 1 d . . . . .
H147 H 0.4556 0.3849 0.3651 0.095 Uiso 1 1 calc R U . . .
C148 C 0.3889(6) 0.4177(3) 0.2698(3) 0.098(2) Uani 1 1 d . . . . .
H148 H 0.3200 0.4140 0.2840 0.117 Uiso 1 1 calc R U . . .
C149 C 0.4059(8) 0.4400(4) 0.2027(4) 0.104(2) Uani 1 1 d . . . . .
H149 H 0.3495 0.4519 0.1699 0.124 Uiso 1 1 calc R U . . .
C150 C 0.5032(8) 0.4450(3) 0.1829(3) 0.105(3) Uani 1 1 d . . . . .
H150 H 0.5145 0.4616 0.1355 0.126 Uiso 1 1 calc R U . . .
C151 C 0.5914(6) 0.4261(3) 0.2316(3) 0.0870(19) Uani 1 1 d . . . . .
C152 C 0.7019(8) 0.4307(3) 0.2100(3) 0.108(3) Uani 1 1 d . . . . .
C153 C 0.5995(5) 0.4071(3) 0.5641(2) 0.0753(15) Uani 1 1 d . . . . .
C154 C 0.5601(7) 0.4589(3) 0.5845(3) 0.101(2) Uani 1 1 d . . . . .
H154 H 0.4991 0.4589 0.6098 0.121 Uiso 1 1 calc R U . . .
C155 C 0.6112(8) 0.5100(3) 0.5672(3) 0.124(3) Uani 1 1 d . . . . .
H155 H 0.5845 0.5467 0.5803 0.149 Uiso 1 1 calc R U . . .
C156 C 0.7034(7) 0.5102(3) 0.5302(3) 0.097(2) Uani 1 1 d . . . . .
H156 H 0.7419 0.5442 0.5206 0.117 Uiso 1 1 calc R U . . .
C157 C 0.7340(5) 0.4578(2) 0.5090(2) 0.0680(13) Uani 1 1 d . . . . .
H157 H 0.7922 0.4581 0.4813 0.082 Uiso 1 1 calc R U . . .
C158 C 0.5545(4) 0.2504(3) 0.5660(2) 0.0637(12) Uani 1 1 d . . . . .
H158 H 0.5872 0.2184 0.5483 0.076 Uiso 1 1 calc R U . . .
C159 C 0.4652(4) 0.2412(4) 0.6001(3) 0.0816(16) Uani 1 1 d . . . . .
H159 H 0.4371 0.2033 0.6061 0.098 Uiso 1 1 calc R U . . .
C160 C 0.4168(5) 0.2871(4) 0.6253(3) 0.0925(19) Uani 1 1 d . . . . .
H160 H 0.3555 0.2810 0.6500 0.111 Uiso 1 1 calc R U . . .
C161 C 0.4573(5) 0.3423(4) 0.6148(3) 0.090(2) Uani 1 1 d . . . . .
H161 H 0.4235 0.3756 0.6310 0.108 Uiso 1 1 calc R U . . .
C162 C 0.5501(4) 0.3488(3) 0.5796(2) 0.0663(13) Uani 1 1 d . . . . .
O1S O 0.7328(4) 0.3027(2) 0.9477(3) 0.0657(11) Uani 0.7 1 d . . P A 1
H1S H 0.6689 0.3106 0.9571 0.099 Uiso 0.7 1 calc R U P A 1
C1S C 0.7587(4) 0.3669(3) 0.9148(3) 0.0726(13) Uani 0.7 1 d . . P A 1
H1S1 H 0.7255 0.3972 0.9361 0.109 Uiso 0.7 1 calc R U P A 1
H1S2 H 0.7323 0.3919 0.8659 0.109 Uiso 0.7 1 calc R U P A 1
H1S3 H 0.8367 0.3571 0.9192 0.109 Uiso 0.7 1 calc R U P A 1
O1SA O 0.6879(9) 0.3895(7) 0.9525(8) 0.080(3) Uani 0.3 1 d . . P B 2
H1SA H 0.6253 0.3957 0.9385 0.120 Uiso 0.3 1 calc R U P B 2
C1SA C 0.7587(4) 0.3669(3) 0.9148(3) 0.0726(13) Uani 0.3 1 d . . P B 2
H1S4 H 0.7274 0.3425 0.8963 0.109 Uiso 0.3 1 calc R U P B 2
H1S5 H 0.8246 0.3333 0.9443 0.109 Uiso 0.3 1 calc R U P B 2
H1S6 H 0.7753 0.4085 0.8766 0.109 Uiso 0.3 1 calc R U P B 2
O2S O 0.6786(7) 0.3123(4) 0.7375(4) 0.079(2) Uani 0.5 1 d . . P . .
H2S H 0.7079 0.2706 0.7693 0.118 Uiso 0.5 1 calc R U P . .
C2S C 0.7424(8) 0.3550(5) 0.7274(5) 0.066(2) Uani 0.5 1 d . . P . .
H2S1 H 0.7014 0.3981 0.7306 0.099 Uiso 0.5 1 calc R U P . .
H2S2 H 0.7684 0.3694 0.6816 0.099 Uiso 0.5 1 calc R U P . .
H2S3 H 0.8035 0.3285 0.7627 0.099 Uiso 0.5 1 calc R U P . .
O3S O 0.2061(3) 0.2082(2) 0.3339(2) 0.0807(11) Uani 1 1 d . . . . .
H3S H 0.1665 0.1997 0.3664 0.121 Uiso 1 1 calc R U . . .
C3S C 0.2341(10) 0.2690(5) 0.3193(5) 0.175(5) Uani 1 1 d . . . . .
H3S1 H 0.2017 0.2878 0.3504 0.263 Uiso 1 1 calc R U . . .
H3S2 H 0.2084 0.3054 0.2714 0.263 Uiso 1 1 calc R U . . .
H3S3 H 0.3122 0.2572 0.3255 0.263 Uiso 1 1 calc R U . . .
O4S O 0.2188(3) 0.3845(2) 0.4025(3) 0.0922(12) Uani 1 1 d . . . . .
H4S H 0.1634 0.3763 0.3943 0.138 Uiso 1 1 calc R U . . .
C4S C 0.2909(6) 0.3209(3) 0.4474(5) 0.130(3) Uani 1 1 d . . . . .
H4S1 H 0.3386 0.3304 0.4727 0.195 Uiso 1 1 calc R U . . .
H4S2 H 0.3332 0.2982 0.4215 0.195 Uiso 1 1 calc R U . . .
H4S3 H 0.2523 0.2885 0.4801 0.195 Uiso 1 1 calc R U . . .
O5S O 0.6981(5) 0.2278(3) 0.8785(3) 0.1184(19) Uani 1 1 d D . . . .
H5S1 H 0.662(7) 0.201(5) 0.903(5) 0.178 Uiso 1 1 d D U . . .
H5S2 H 0.758(4) 0.200(5) 0.881(6) 0.178 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.963(3) . ?
Ni1 O1 2.055(3) . ?
Ni1 N4 2.060(3) . ?
Ni1 O4 2.094(3) . ?
Ni1 N3 2.117(3) . ?
Ni1 O2 2.137(3) . ?
Ni2 N5 1.967(3) . ?
Ni2 O4 2.040(3) . ?
Ni2 N7 2.075(4) . ?
Ni2 N8 2.082(4) . ?
Ni2 O1 2.109(3) . ?
Ni2 O5 2.113(3) . ?
O1 C1 1.350(5) . ?
O2 C14 1.249(5) . ?
O3 C21 1.239(5) . ?
O4 C32 1.332(5) . ?
O5 C45 1.256(5) . ?
O6 C52 1.232(6) . ?
N1 C8 1.361(5) . ?
N1 C7 1.373(5) . ?
N2 C7 1.344(5) . ?
N2 C9 1.377(6) . ?
N3 C22 1.344(6) . ?
N3 C26 1.349(6) . ?
N4 C27 1.335(6) . ?
N4 C31 1.343(5) . ?
N5 C38 1.363(5) . ?
N5 C39 1.369(5) . ?
N6 C38 1.348(5) . ?
N6 C40 1.365(6) . ?
N7 C53 1.337(7) . ?
N7 C57 1.357(7) . ?
N8 C62 1.331(6) . ?
N8 C58 1.348(6) . ?
C1 C2 1.407(6) . ?
C1 C6 1.410(6) . ?
C2 C3 1.382(6) . ?
C3 C4 1.379(7) . ?
C4 C5 1.378(7) . ?
C5 C6 1.418(6) . ?
C6 C7 1.465(6) . ?
C8 C13 1.399(6) . ?
C8 C9 1.412(6) . ?
C9 C10 1.400(6) . ?
C10 C11 1.383(7) . ?
C11 C12 1.391(7) . ?
C12 C13 1.418(6) . ?
C12 C21 1.467(6) . ?
C13 C14 1.457(6) . ?
C14 C15 1.488(6) . ?
C15 C16 1.385(6) . ?
C15 C20 1.407(6) . ?
C16 C17 1.390(6) . ?
C17 C18 1.376(7) . ?
C18 C19 1.391(7) . ?
C19 C20 1.398(6) . ?
C20 C21 1.486(7) . ?
C22 C23 1.392(7) . ?
C23 C24 1.388(10) . ?
C24 C25 1.381(9) . ?
C25 C26 1.373(6) . ?
C26 C27 1.498(7) . ?
C27 C28 1.395(7) . ?
C28 C29 1.388(8) . ?
C29 C30 1.353(7) . ?
C30 C31 1.393(6) . ?
C32 C33 1.413(6) . ?
C32 C37 1.415(6) . ?
C33 C34 1.379(6) . ?
C34 C35 1.381(7) . ?
C35 C36 1.386(6) . ?
C36 C37 1.409(6) . ?
C37 C38 1.461(6) . ?
C39 C44 1.395(6) . ?
C39 C40 1.424(6) . ?
C40 C41 1.387(6) . ?
C41 C42 1.397(7) . ?
C42 C43 1.393(7) . ?
C43 C44 1.419(6) . ?
C43 C52 1.474(7) . ?
C44 C45 1.454(6) . ?
C45 C46 1.475(6) . ?
C46 C47 1.378(7) . ?
C46 C51 1.412(6) . ?
C47 C48 1.402(7) . ?
C48 C49 1.379(8) . ?
C49 C50 1.397(9) . ?
C50 C51 1.388(7) . ?
C51 C52 1.477(8) . ?
C53 C54 1.391(7) . ?
C54 C55 1.401(12) . ?
C55 C56 1.373(13) . ?
C56 C57 1.379(8) . ?
C57 C58 1.459(9) . ?
C58 C59 1.387(8) . ?
C59 C60 1.376(11) . ?
C60 C61 1.360(10) . ?
C61 C62 1.396(7) . ?
Ni3 N101 1.978(3) . ?
Ni3 O101 2.050(3) . ?
Ni3 N104 2.066(3) . ?
Ni3 O104 2.083(3) . ?
Ni3 N103 2.091(3) . ?
Ni3 O102 2.100(3) . ?
Ni4 N105 1.981(4) . ?
Ni4 O104 2.048(3) . ?
Ni4 N108 2.073(4) . ?
Ni4 N107 2.084(4) . ?
Ni4 O101 2.105(3) . ?
Ni4 O105 2.118(3) . ?
O101 C101 1.338(5) . ?
O102 C114 1.249(5) . ?
O103 C121 1.238(6) . ?
O104 C132 1.343(5) . ?
O105 C145 1.244(5) . ?
O106 C152 1.242(7) . ?
N101 C107 1.363(5) . ?
N101 C108 1.365(5) . ?
N102 C107 1.352(5) . ?
N102 C109 1.358(6) . ?
N103 C122 1.343(5) . ?
N103 C126 1.355(5) . ?
N104 C131 1.341(5) . ?
N104 C127 1.348(5) . ?
N105 C138 1.360(7) . ?
N105 C139 1.362(6) . ?
N106 C138 1.362(6) . ?
N106 C140 1.380(9) . ?
N107 C157 1.327(7) . ?
N107 C153 1.361(7) . ?
N108 C162 1.336(6) . ?
N108 C158 1.349(6) . ?
C101 C102 1.399(6) . ?
C101 C106 1.432(6) . ?
C102 C103 1.391(6) . ?
C103 C104 1.386(7) . ?
C104 C105 1.370(7) . ?
C105 C106 1.417(6) . ?
C106 C107 1.436(6) . ?
C108 C113 1.387(6) . ?
C108 C109 1.425(6) . ?
C109 C110 1.400(6) . ?
C110 C111 1.385(7) . ?
C111 C112 1.404(7) . ?
C112 C113 1.414(6) . ?
C112 C121 1.473(7) . ?
C113 C114 1.461(6) . ?
C114 C115 1.478(6) . ?
C115 C116 1.387(7) . ?
C115 C120 1.401(6) . ?
C116 C117 1.385(7) . ?
C117 C118 1.388(8) . ?
C118 C119 1.363(8) . ?
C119 C120 1.395(7) . ?
C120 C121 1.480(7) . ?
C122 C123 1.384(6) . ?
C123 C124 1.383(7) . ?
C124 C125 1.386(7) . ?
C125 C126 1.379(6) . ?
C126 C127 1.483(6) . ?
C127 C128 1.394(6) . ?
C128 C129 1.379(7) . ?
C129 C130 1.377(7) . ?
C130 C131 1.388(6) . ?
C132 C133 1.387(7) . ?
C132 C137 1.422(7) . ?
C133 C134 1.379(7) . ?
C134 C135 1.396(10) . ?
C135 C136 1.371(9) . ?
C136 C137 1.412(7) . ?
C137 C138 1.453(8) . ?
C139 C144 1.385(8) . ?
C139 C140 1.426(8) . ?
C140 C141 1.430(9) . ?
C141 C142 1.356(12) . ?
C142 C143 1.357(11) . ?
C143 C144 1.433(7) . ?
C143 C152 1.471(11) . ?
C144 C145 1.462(8) . ?
C145 C146 1.493(8) . ?
C146 C147 1.362(9) . ?
C146 C151 1.397(8) . ?
C147 C148 1.382(8) . ?
C148 C149 1.351(10) . ?
C149 C150 1.339(11) . ?
C150 C151 1.445(10) . ?
C151 C152 1.513(11) . ?
C153 C154 1.372(7) . ?
C153 C162 1.482(8) . ?
C154 C155 1.355(11) . ?
C155 C156 1.420(11) . ?
C156 C157 1.388(7) . ?
C158 C159 1.366(7) . ?
C159 C160 1.364(9) . ?
C160 C161 1.371(10) . ?
C161 C162 1.410(8) . ?
O1S C1S 1.381(7) . ?
O1SA C1SA 1.359(13) . ?
O2S C2S 1.358(12) . ?
O3S C3S 1.368(8) . ?
O4S C4S 1.372(8) . ?

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 O1 88.77(13) . . ?
N1 Ni1 N4 171.25(14) . . ?
O1 Ni1 N4 98.23(12) . . ?
N1 Ni1 O4 95.85(12) . . ?
O1 Ni1 O4 82.62(10) . . ?
N4 Ni1 O4 90.29(12) . . ?
N1 Ni1 N3 97.33(14) . . ?
O1 Ni1 N3 87.88(12) . . ?
N4 Ni1 N3 77.80(14) . . ?
O4 Ni1 N3 163.57(13) . . ?
N1 Ni1 O2 87.66(12) . . ?
O1 Ni1 O2 171.44(10) . . ?
N4 Ni1 O2 86.09(12) . . ?
O4 Ni1 O2 90.00(10) . . ?
N3 Ni1 O2 100.29(12) . . ?
N5 Ni2 O4 87.83(12) . . ?
N5 Ni2 N7 97.15(14) . . ?
O4 Ni2 N7 89.23(13) . . ?
N5 Ni2 N8 172.83(14) . . ?
O4 Ni2 N8 97.71(12) . . ?
N7 Ni2 N8 78.47(16) . . ?
N5 Ni2 O1 95.11(12) . . ?
O4 Ni2 O1 82.62(10) . . ?
N7 Ni2 O1 165.00(13) . . ?
N8 Ni2 O1 90.13(13) . . ?
N5 Ni2 O5 87.88(13) . . ?
O4 Ni2 O5 173.62(11) . . ?
N7 Ni2 O5 95.99(13) . . ?
N8 Ni2 O5 86.95(13) . . ?
O1 Ni2 O5 93.07(11) . . ?
C1 O1 Ni1 124.2(3) . . ?
C1 O1 Ni2 117.9(2) . . ?
Ni1 O1 Ni2 96.68(11) . . ?
C14 O2 Ni1 129.3(3) . . ?
C32 O4 Ni2 123.1(2) . . ?
C32 O4 Ni1 119.9(2) . . ?
Ni2 O4 Ni1 97.59(11) . . ?
C45 O5 Ni2 130.1(3) . . ?
C8 N1 C7 104.4(3) . . ?
C8 N1 Ni1 126.0(3) . . ?
C7 N1 Ni1 129.5(3) . . ?
C7 N2 C9 103.8(3) . . ?
C22 N3 C26 119.1(4) . . ?
C22 N3 Ni1 125.0(3) . . ?
C26 N3 Ni1 113.9(3) . . ?
C27 N4 C31 118.8(4) . . ?
C27 N4 Ni1 117.2(3) . . ?
C31 N4 Ni1 123.9(3) . . ?
C38 N5 C39 104.3(3) . . ?
C38 N5 Ni2 130.3(3) . . ?
C39 N5 Ni2 125.2(3) . . ?
C38 N6 C40 104.3(4) . . ?
C53 N7 C57 119.4(4) . . ?
C53 N7 Ni2 125.3(3) . . ?
C57 N7 Ni2 114.7(3) . . ?
C62 N8 C58 119.6(4) . . ?
C62 N8 Ni2 125.5(3) . . ?
C58 N8 Ni2 114.8(4) . . ?
O1 C1 C2 117.3(4) . . ?
O1 C1 C6 123.8(4) . . ?
C2 C1 C6 118.9(4) . . ?
C3 C2 C1 120.5(4) . . ?
C4 C3 C2 121.5(5) . . ?
C5 C4 C3 118.8(4) . . ?
C4 C5 C6 121.8(4) . . ?
C1 C6 C5 118.4(4) . . ?
C1 C6 C7 124.1(4) . . ?
C5 C6 C7 117.5(4) . . ?
N2 C7 N1 114.5(4) . . ?
N2 C7 C6 123.5(4) . . ?
N1 C7 C6 121.9(4) . . ?
N1 C8 C13 129.8(4) . . ?
N1 C8 C9 108.1(4) . . ?
C13 C8 C9 122.0(4) . . ?
N2 C9 C10 130.7(4) . . ?
N2 C9 C8 109.1(4) . . ?
C10 C9 C8 120.2(4) . . ?
C11 C10 C9 117.7(4) . . ?
C10 C11 C12 123.0(4) . . ?
C11 C12 C13 120.2(4) . . ?
C11 C12 C21 119.7(4) . . ?
C13 C12 C21 120.1(4) . . ?
C8 C13 C12 116.9(4) . . ?
C8 C13 C14 121.9(4) . . ?
C12 C13 C14 121.1(4) . . ?
O2 C14 C13 122.7(4) . . ?
O2 C14 C15 118.8(4) . . ?
C13 C14 C15 118.6(4) . . ?
C16 C15 C20 119.7(4) . . ?
C16 C15 C14 120.5(4) . . ?
C20 C15 C14 119.8(4) . . ?
C15 C16 C17 119.7(4) . . ?
C18 C17 C16 121.0(5) . . ?
C17 C18 C19 120.1(4) . . ?
C18 C19 C20 119.6(5) . . ?
C19 C20 C15 119.8(4) . . ?
C19 C20 C21 119.4(4) . . ?
C15 C20 C21 120.7(4) . . ?
O3 C21 C12 121.1(4) . . ?
O3 C21 C20 120.4(4) . . ?
C12 C21 C20 118.5(4) . . ?
N3 C22 C23 121.6(5) . . ?
C24 C23 C22 119.0(6) . . ?
C25 C24 C23 118.6(5) . . ?
C26 C25 C24 119.9(6) . . ?
N3 C26 C25 121.7(5) . . ?
N3 C26 C27 114.3(4) . . ?
C25 C26 C27 123.9(5) . . ?
N4 C27 C28 121.6(5) . . ?
N4 C27 C26 114.5(4) . . ?
C28 C27 C26 123.9(4) . . ?
C29 C28 C27 118.9(5) . . ?
C30 C29 C28 119.4(4) . . ?
C29 C30 C31 119.1(5) . . ?
N4 C31 C30 122.2(4) . . ?
O4 C32 C33 117.8(4) . . ?
O4 C32 C37 124.6(4) . . ?
C33 C32 C37 117.6(4) . . ?
C34 C33 C32 121.7(4) . . ?
C33 C34 C35 120.7(4) . . ?
C34 C35 C36 119.0(4) . . ?
C35 C36 C37 121.7(4) . . ?
C36 C37 C32 119.1(4) . . ?
C36 C37 C38 118.7(4) . . ?
C32 C37 C38 122.2(4) . . ?
N6 C38 N5 114.8(4) . . ?
N6 C38 C37 123.6(4) . . ?
N5 C38 C37 121.5(3) . . ?
N5 C39 C44 129.8(4) . . ?
N5 C39 C40 107.8(4) . . ?
C44 C39 C40 122.4(4) . . ?
N6 C40 C41 131.0(4) . . ?
N6 C40 C39 108.9(4) . . ?
C41 C40 C39 120.2(4) . . ?
C40 C41 C42 117.6(5) . . ?
C43 C42 C41 122.7(4) . . ?
C42 C43 C44 120.5(4) . . ?
C42 C43 C52 119.7(4) . . ?
C44 C43 C52 119.8(4) . . ?
C39 C44 C43 116.6(4) . . ?
C39 C44 C45 121.9(4) . . ?
C43 C44 C45 121.4(4) . . ?
O5 C45 C44 122.8(4) . . ?
O5 C45 C46 118.1(4) . . ?
C44 C45 C46 119.1(4) . . ?
C47 C46 C51 120.2(4) . . ?
C47 C46 C45 119.9(4) . . ?
C51 C46 C45 119.9(4) . . ?
C46 C47 C48 120.1(5) . . ?
C49 C48 C47 120.1(6) . . ?
C48 C49 C50 119.8(5) . . ?
C51 C50 C49 120.7(5) . . ?
C50 C51 C46 119.0(5) . . ?
C50 C51 C52 119.9(4) . . ?
C46 C51 C52 121.2(4) . . ?
O6 C52 C43 121.2(5) . . ?
O6 C52 C51 120.2(5) . . ?
C43 C52 C51 118.6(4) . . ?
N7 C53 C54 123.0(6) . . ?
C53 C54 C55 117.0(7) . . ?
C56 C55 C54 120.0(6) . . ?
C55 C56 C57 119.8(7) . . ?
N7 C57 C56 120.8(6) . . ?
N7 C57 C58 115.2(4) . . ?
C56 C57 C58 123.9(6) . . ?
N8 C58 C59 120.6(6) . . ?
N8 C58 C57 115.9(4) . . ?
C59 C58 C57 123.5(5) . . ?
C60 C59 C58 119.6(6) . . ?
C61 C60 C59 119.6(5) . . ?
C60 C61 C62 118.8(6) . . ?
N8 C62 C61 121.7(5) . . ?
N101 Ni3 O101 88.08(12) . . ?
N101 Ni3 N104 172.30(13) . . ?
O101 Ni3 N104 97.13(12) . . ?
N101 Ni3 O104 96.69(12) . . ?
O101 Ni3 O104 82.71(11) . . ?
N104 Ni3 O104 89.62(12) . . ?
N101 Ni3 N103 96.03(13) . . ?
O101 Ni3 N103 89.09(12) . . ?
N104 Ni3 N103 78.45(13) . . ?
O104 Ni3 N103 164.60(13) . . ?
N101 Ni3 O102 88.42(12) . . ?
O101 Ni3 O102 172.73(11) . . ?
N104 Ni3 O102 87.02(12) . . ?
O104 Ni3 O102 91.38(11) . . ?
N103 Ni3 O102 97.62(12) . . ?
N105 Ni4 O104 87.61(14) . . ?
N105 Ni4 N108 172.31(15) . . ?
O104 Ni4 N108 99.04(13) . . ?
N105 Ni4 N107 97.72(15) . . ?
O104 Ni4 N107 91.05(13) . . ?
N108 Ni4 N107 78.43(16) . . ?
N105 Ni4 O101 95.26(12) . . ?
O104 Ni4 O101 82.20(11) . . ?
N108 Ni4 O101 89.49(13) . . ?
N107 Ni4 O101 165.10(13) . . ?
N105 Ni4 O105 87.53(15) . . ?
O104 Ni4 O105 172.12(11) . . ?
N108 Ni4 O105 86.25(13) . . ?
N107 Ni4 O105 95.75(13) . . ?
O101 Ni4 O105 92.07(11) . . ?
C101 O101 Ni3 123.8(2) . . ?
C101 O101 Ni4 119.6(2) . . ?
Ni3 O101 Ni4 96.98(11) . . ?
C114 O102 Ni3 130.3(3) . . ?
C132 O104 Ni4 123.7(3) . . ?
C132 O104 Ni3 120.5(2) . . ?
Ni4 O104 Ni3 97.77(11) . . ?
C145 O105 Ni4 130.4(3) . . ?
C107 N101 C108 105.3(3) . . ?
C107 N101 Ni3 129.7(3) . . ?
C108 N101 Ni3 124.9(3) . . ?
C107 N102 C109 104.7(3) . . ?
C122 N103 C126 118.3(4) . . ?
C122 N103 Ni3 126.2(3) . . ?
C126 N103 Ni3 114.0(3) . . ?
C131 N104 C127 119.1(4) . . ?
C131 N104 Ni3 125.4(3) . . ?
C127 N104 Ni3 115.6(3) . . ?
C138 N105 C139 105.9(4) . . ?
C138 N105 Ni4 129.0(3) . . ?
C139 N105 Ni4 124.6(4) . . ?
C138 N106 C140 103.2(5) . . ?
C157 N107 C153 119.8(4) . . ?
C157 N107 Ni4 125.3(3) . . ?
C153 N107 Ni4 114.7(4) . . ?
C162 N108 C158 117.6(4) . . ?
C162 N108 Ni4 116.3(4) . . ?
C158 N108 Ni4 126.0(3) . . ?
O101 C101 C102 118.2(4) . . ?
O101 C101 C106 123.4(4) . . ?
C102 C101 C106 118.4(4) . . ?
C103 C102 C101 121.9(4) . . ?
C104 C103 C102 120.0(4) . . ?
C105 C104 C103 119.3(4) . . ?
C104 C105 C106 122.8(4) . . ?
C105 C106 C101 117.5(4) . . ?
C105 C106 C107 118.2(4) . . ?
C101 C106 C107 124.2(4) . . ?
N102 C107 N101 113.7(4) . . ?
N102 C107 C106 124.1(4) . . ?
N101 C107 C106 122.0(3) . . ?
N101 C108 C113 130.1(4) . . ?
N101 C108 C109 107.1(4) . . ?
C113 C108 C109 122.8(4) . . ?
N102 C109 C110 131.5(4) . . ?
N102 C109 C108 109.2(4) . . ?
C110 C109 C108 119.3(4) . . ?
C111 C110 C109 118.3(4) . . ?
C110 C111 C112 122.2(4) . . ?
C111 C112 C113 120.5(4) . . ?
C111 C112 C121 119.1(4) . . ?
C113 C112 C121 120.4(4) . . ?
C108 C113 C112 116.8(4) . . ?
C108 C113 C114 122.2(4) . . ?
C112 C113 C114 120.9(4) . . ?
O102 C114 C113 122.6(4) . . ?
O102 C114 C115 118.5(4) . . ?
C113 C114 C115 118.8(4) . . ?
C116 C115 C120 119.8(4) . . ?
C116 C115 C114 120.0(4) . . ?
C120 C115 C114 120.2(4) . . ?
C117 C116 C115 120.7(5) . . ?
C116 C117 C118 119.1(5) . . ?
C119 C118 C117 120.9(5) . . ?
C118 C119 C120 120.8(5) . . ?
C119 C120 C115 118.8(5) . . ?
C119 C120 C121 120.1(4) . . ?
C115 C120 C121 121.1(4) . . ?
O103 C121 C112 121.5(5) . . ?
O103 C121 C120 120.2(4) . . ?
C112 C121 C120 118.3(4) . . ?
N103 C122 C123 122.9(4) . . ?
C124 C123 C122 118.3(4) . . ?
C123 C124 C125 119.4(4) . . ?
C126 C125 C124 119.2(4) . . ?
N103 C126 C125 121.9(4) . . ?
N103 C126 C127 114.6(3) . . ?
C125 C126 C127 123.5(4) . . ?
N104 C127 C128 121.8(4) . . ?
N104 C127 C126 115.2(3) . . ?
C128 C127 C126 123.1(4) . . ?
C129 C128 C127 118.7(4) . . ?
C130 C129 C128 119.5(4) . . ?
C129 C130 C131 119.2(4) . . ?
N104 C131 C130 121.7(4) . . ?
O104 C132 C133 118.6(4) . . ?
O104 C132 C137 122.6(4) . . ?
C133 C132 C137 118.8(4) . . ?
C134 C133 C132 121.6(6) . . ?
C133 C134 C135 120.7(6) . . ?
C136 C135 C134 118.4(5) . . ?
C135 C136 C137 122.5(6) . . ?
C136 C137 C132 118.0(5) . . ?
C136 C137 C138 118.9(5) . . ?
C132 C137 C138 123.1(4) . . ?
N105 C138 N106 114.3(5) . . ?
N105 C138 C137 121.9(4) . . ?
N106 C138 C137 123.7(5) . . ?
N105 C139 C144 129.9(5) . . ?
N105 C139 C140 106.8(5) . . ?
C144 C139 C140 123.2(5) . . ?
N106 C140 C139 109.8(5) . . ?
N106 C140 C141 133.5(6) . . ?
C139 C140 C141 116.7(7) . . ?
C142 C141 C140 119.7(7) . . ?
C141 C142 C143 123.3(6) . . ?
C142 C143 C144 120.4(7) . . ?
C142 C143 C152 119.7(6) . . ?
C144 C143 C152 119.8(7) . . ?
C139 C144 C143 116.6(6) . . ?
C139 C144 C145 122.7(4) . . ?
C143 C144 C145 120.6(6) . . ?
O105 C145 C144 121.9(5) . . ?
O105 C145 C146 118.1(5) . . ?
C144 C145 C146 120.0(5) . . ?
C147 C146 C151 119.2(6) . . ?
C147 C146 C145 120.9(5) . . ?
C151 C146 C145 119.9(6) . . ?
C146 C147 C148 121.3(6) . . ?
C149 C148 C147 121.2(8) . . ?
C150 C149 C148 119.2(8) . . ?
C149 C150 C151 121.9(6) . . ?
C146 C151 C150 117.1(7) . . ?
C146 C151 C152 120.5(6) . . ?
C150 C151 C152 122.4(6) . . ?
O106 C152 C143 120.1(9) . . ?
O106 C152 C151 120.8(8) . . ?
C143 C152 C151 119.1(5) . . ?
N107 C153 C154 122.0(6) . . ?
N107 C153 C162 115.3(4) . . ?
C154 C153 C162 122.7(6) . . ?
C155 C154 C153 117.9(7) . . ?
C154 C155 C156 121.9(5) . . ?
C157 C156 C155 116.0(7) . . ?
N107 C157 C156 122.4(6) . . ?
N108 C158 C159 123.5(5) . . ?
C160 C159 C158 118.9(6) . . ?
C159 C160 C161 119.5(5) . . ?
C160 C161 C162 118.8(5) . . ?
N108 C162 C161 121.6(6) . . ?
N108 C162 C153 114.9(4) . . ?
C161 C162 C153 123.4(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
O1S H1S N6 0.84 1.92 2.734(6) 163.9 1_556
O1SA H1SA N6 0.84 2.01 2.725(11) 141.9 1_556
O2S H2S O5S 0.84 2.15 2.752(9) 128.7 .
O3S H3S N102 0.84 1.98 2.809(5) 171.7 1_455
O4S H4S N106 0.84 2.03 2.803(6) 152.2 1_455
O5S H5S1 N2 0.82(2) 1.98(5) 2.737(6) 152(10) 1_556

_refine_diff_density_max         0.983
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.106



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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1584239'
_audit_update_record             
;
2017-11-06 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H28 Co2 N4 O8'
_chemical_formula_weight         858.56

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/a'
_space_group_name_Hall           '-P 2yab'

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

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

_cell_length_a                   8.0853(3)
_cell_length_b                   15.3810(4)
_cell_length_c                   14.5164(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.739(1)
_cell_angle_gamma                90
_cell_volume                     1773.64(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    918
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      22.48

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_F_000             876
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.002
_shelx_estimated_absorpt_T_min   0.864
_shelx_estimated_absorpt_T_max   0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 Sheldrick, G.M. SADABS: Program for absorption correction
 using area detector data. University of Göttingen, Germany, 1996.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11983
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.947
_diffrn_reflns_theta_max         28.245
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4346
_reflns_number_gt                2747
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BRUKER Smart'
_computing_cell_refinement       'BRUKER Smart'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0545P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4346
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1221
_refine_ls_wR_factor_gt          0.1049
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.65233(5) 0.03459(2) 0.07378(3) 0.02686(14) Uani 1 1 d . . . . .
O1 O 0.5431(3) 0.04628(12) -0.06756(13) 0.0286(5) Uani 1 1 d . . . . .
O2 O 0.7408(3) 0.04049(12) 0.22456(14) 0.0363(5) Uani 1 1 d . . . . .
O3 O 0.9226(4) 0.30069(16) 0.47176(17) 0.0687(9) Uani 1 1 d . . . . .
O4 O 0.8339(3) -0.04974(14) 0.06346(16) 0.0391(6) Uani 1 1 d . . . . .
N1 N 0.7060(3) 0.16041(15) 0.07528(15) 0.0286(6) Uani 1 1 d . . . . .
N2 N 0.7254(4) 0.30066(16) 0.02596(17) 0.0347(7) Uani 1 1 d . . . . .
C1 C 0.5784(4) 0.10823(18) -0.12784(19) 0.0256(6) Uani 1 1 d . . . . .
C2 C 0.5414(4) 0.0921(2) -0.2248(2) 0.0325(7) Uani 1 1 d . . . . .
H2 H 0.4915 0.0396 -0.2463 0.039 Uiso 1 1 calc R U . . .
C3 C 0.5773(5) 0.1524(2) -0.2893(2) 0.0400(8) Uani 1 1 d . . . . .
H3 H 0.5496 0.1402 -0.3531 0.048 Uiso 1 1 calc R U . . .
C4 C 0.6538(5) 0.2304(2) -0.2596(2) 0.0430(9) Uani 1 1 d . . . . .
H4 H 0.6799 0.2702 -0.3029 0.052 Uiso 1 1 calc R U . . .
C5 C 0.6909(4) 0.2483(2) -0.1650(2) 0.0358(8) Uani 1 1 d . . . . .
H5 H 0.7437 0.3005 -0.1450 0.043 Uiso 1 1 calc R U . . .
C6 C 0.6509(4) 0.18960(18) -0.09760(19) 0.0271(7) Uani 1 1 d . . . . .
C7 C 0.6922(4) 0.21640(18) 0.0013(2) 0.0284(7) Uani 1 1 d . . . . .
C8 C 0.7534(4) 0.21231(18) 0.1533(2) 0.0281(7) Uani 1 1 d . . . . .
C9 C 0.7657(4) 0.29936(19) 0.1221(2) 0.0332(7) Uani 1 1 d . . . . .
C10 C 0.8112(4) 0.3660(2) 0.1867(2) 0.0388(8) Uani 1 1 d . . . . .
H10 H 0.8172 0.4232 0.1667 0.047 Uiso 1 1 calc R U . . .
C11 C 0.8470(5) 0.3459(2) 0.2806(2) 0.0406(8) Uani 1 1 d . . . . .
H11 H 0.8805 0.3900 0.3239 0.049 Uiso 1 1 calc R U . . .
C12 C 0.8343(5) 0.2606(2) 0.3127(2) 0.0352(8) Uani 1 1 d . . . . .
C13 C 0.7870(4) 0.19132(19) 0.2491(2) 0.0304(7) Uani 1 1 d . . . . .
C14 C 0.7724(4) 0.10226(19) 0.2805(2) 0.0295(7) Uani 1 1 d . . . . .
C15 C 0.7957(4) 0.0852(2) 0.3828(2) 0.0345(7) Uani 1 1 d . . . . .
C16 C 0.7677(5) 0.0025(2) 0.4155(2) 0.0435(9) Uani 1 1 d . . . . .
H16 H 0.7390 -0.0429 0.3731 0.052 Uiso 1 1 calc R U . . .
C17 C 0.7821(5) -0.0127(3) 0.5104(2) 0.0517(10) Uani 1 1 d . . . . .
H17 H 0.7611 -0.0679 0.5317 0.062 Uiso 1 1 calc R U . . .
C18 C 0.8276(5) 0.0537(3) 0.5735(2) 0.0554(11) Uani 1 1 d . . . . .
H18 H 0.8377 0.0430 0.6373 0.067 Uiso 1 1 calc R U . . .
C19 C 0.8583(5) 0.1363(3) 0.5429(2) 0.0489(10) Uani 1 1 d . . . . .
H19 H 0.8900 0.1806 0.5863 0.059 Uiso 1 1 calc R U . . .
C20 C 0.8421(5) 0.1536(2) 0.4477(2) 0.0380(8) Uani 1 1 d . . . . .
C21 C 0.8711(5) 0.2430(2) 0.4155(2) 0.0422(9) Uani 1 1 d . . . . .
C22 C 0.9990(5) -0.0509(2) 0.1195(3) 0.0558(10) Uani 1 1 d . . . . .
H22A H 1.0144 -0.0002 0.1588 0.084 Uiso 1 1 calc R U . . .
H22B H 1.0810 -0.0510 0.0795 0.084 Uiso 1 1 calc R U . . .
H22C H 1.0125 -0.1022 0.1579 0.084 Uiso 1 1 calc R U . . .
H40 H 0.809(5) -0.101(3) 0.038(3) 0.066(13) Uiso 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
Co1 N1 1.982(2) . ?
Co1 O4 1.985(2) . ?
Co1 O1 2.000(2) 3_655 ?
Co1 O1 2.0850(19) . ?
Co1 O2 2.174(2) . ?
Co1 Co1 3.1340(8) 3_655 ?
O1 C1 1.359(3) . ?
O1 Co1 2.000(2) 3_655 ?
O2 C14 1.245(3) . ?
O3 C21 1.225(4) . ?
O4 C22 1.428(4) . ?
N1 C7 1.364(3) . ?
N1 C8 1.381(3) . ?
N2 C7 1.358(4) . ?
N2 C9 1.372(4) . ?
C1 C2 1.406(4) . ?
C1 C6 1.417(4) . ?
C2 C3 1.386(4) . ?
C3 C4 1.382(5) . ?
C4 C5 1.378(4) . ?
C5 C6 1.413(4) . ?
C6 C7 1.472(4) . ?
C8 C13 1.404(4) . ?
C8 C9 1.423(4) . ?
C9 C10 1.392(4) . ?
C10 C11 1.374(4) . ?
C11 C12 1.403(4) . ?
C12 C13 1.415(4) . ?
C12 C21 1.490(4) . ?
C13 C14 1.456(4) . ?
C14 C15 1.484(4) . ?
C15 C16 1.391(4) . ?
C15 C20 1.415(4) . ?
C16 C17 1.381(5) . ?
C17 C18 1.376(5) . ?
C18 C19 1.383(5) . ?
C19 C20 1.389(4) . ?
C20 C21 1.486(5) . ?

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 Co1 O4 118.38(10) . . ?
N1 Co1 O1 141.00(10) . 3_655 ?
O4 Co1 O1 100.32(9) . 3_655 ?
N1 Co1 O1 88.75(8) . . ?
O4 Co1 O1 99.54(9) . . ?
O1 Co1 O1 79.80(8) 3_655 . ?
N1 Co1 O2 85.29(8) . . ?
O4 Co1 O2 89.66(9) . . ?
O1 Co1 O2 100.39(8) 3_655 . ?
O1 Co1 O2 170.63(8) . . ?
N1 Co1 Co1 118.77(8) . 3_655 ?
O4 Co1 Co1 102.98(7) . 3_655 ?
O1 Co1 Co1 40.90(5) 3_655 3_655 ?
O1 Co1 Co1 38.90(5) . 3_655 ?
O2 Co1 Co1 140.48(6) . 3_655 ?
C1 O1 Co1 131.75(18) . 3_655 ?
C1 O1 Co1 126.34(18) . . ?
Co1 O1 Co1 100.20(8) 3_655 . ?
C14 O2 Co1 132.67(19) . . ?
C22 O4 Co1 126.2(2) . . ?
C7 N1 C8 104.5(2) . . ?
C7 N1 Co1 128.46(19) . . ?
C8 N1 Co1 126.88(18) . . ?
C7 N2 C9 104.6(2) . . ?
O1 C1 C2 119.3(3) . . ?
O1 C1 C6 123.0(2) . . ?
C2 C1 C6 117.7(3) . . ?
C3 C2 C1 121.7(3) . . ?
C4 C3 C2 120.6(3) . . ?
C5 C4 C3 119.1(3) . . ?
C4 C5 C6 121.8(3) . . ?
C5 C6 C1 119.0(3) . . ?
C5 C6 C7 117.2(3) . . ?
C1 C6 C7 123.7(2) . . ?
N2 C7 N1 114.4(3) . . ?
N2 C7 C6 121.5(2) . . ?
N1 C7 C6 124.2(2) . . ?
N1 C8 C13 130.8(3) . . ?
N1 C8 C9 107.9(2) . . ?
C13 C8 C9 121.3(3) . . ?
N2 C9 C10 131.1(3) . . ?
N2 C9 C8 108.7(3) . . ?
C10 C9 C8 120.2(3) . . ?
C11 C10 C9 118.9(3) . . ?
C10 C11 C12 121.7(3) . . ?
C11 C12 C13 121.0(3) . . ?
C11 C12 C21 119.2(3) . . ?
C13 C12 C21 119.8(3) . . ?
C8 C13 C12 116.9(3) . . ?
C8 C13 C14 121.0(3) . . ?
C12 C13 C14 122.1(3) . . ?
O2 C14 C13 122.1(3) . . ?
O2 C14 C15 119.3(3) . . ?
C13 C14 C15 118.5(3) . . ?
C16 C15 C20 119.5(3) . . ?
C16 C15 C14 120.3(3) . . ?
C20 C15 C14 120.2(3) . . ?
C17 C16 C15 120.4(3) . . ?
C18 C17 C16 120.0(3) . . ?
C17 C18 C19 120.7(3) . . ?
C18 C19 C20 120.3(3) . . ?
C19 C20 C15 119.0(3) . . ?
C19 C20 C21 119.9(3) . . ?
C15 C20 C21 121.1(3) . . ?
O3 C21 C20 121.0(3) . . ?
O3 C21 C12 121.1(3) . . ?
C20 C21 C12 118.0(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
O4 H40 N2 0.88(4) 1.76(4) 2.641(3) 172(4) 2_645

_refine_diff_density_max         0.767
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.084

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1584240'
_audit_update_record             
;
2017-11-06 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H36 Co2 N8 O6'
_chemical_formula_weight         1154.89

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'

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

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

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

_cell_length_a                   11.7724(13)
_cell_length_b                   15.8207(18)
_cell_length_c                   18.432(2)
_cell_angle_alpha                67.749(2)
_cell_angle_beta                 75.899(2)
_cell_angle_gamma                72.405(2)
_cell_volume                     2996.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    933
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      21.86

_exptl_crystal_description       Prism
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_F_000             1180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.611
_shelx_estimated_absorpt_T_min   0.766
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6449
_exptl_absorpt_correction_T_max  0.9165
_exptl_absorpt_process_details   
;
 Sheldrick, G.M. SADABS: Program for absorption correction
 using area detector data. University of Göttingen, Germany, 1996.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27076
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.537
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             12059
_reflns_number_gt                6070
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BRUKER Smart'
_computing_cell_refinement       'BRUKER Smart'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0459P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12059
_refine_ls_number_parameters     740
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1052
_refine_ls_wR_factor_gt          0.0866
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_restrained_S_all      0.893
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.55981(3) 0.86788(3) 0.29760(2) 0.04617(12) Uani 1 1 d . . . . .
Co2 Co 0.36226(3) 0.77591(3) 0.29579(2) 0.04798(13) Uani 1 1 d . . . . .
O1 O 0.39082(16) 0.90799(13) 0.26227(10) 0.0484(5) Uani 1 1 d . . . . .
O2 O 0.71194(17) 0.80560(14) 0.36391(11) 0.0602(6) Uani 1 1 d . . . . .
O3 O 0.7334(3) 0.69410(18) 0.67598(14) 0.1057(9) Uani 1 1 d . . . . .
O4 O 0.53045(16) 0.73494(12) 0.33432(10) 0.0484(5) Uani 1 1 d . . . . .
O5 O 0.57605(18) 1.01114(13) 0.23116(11) 0.0593(6) Uani 1 1 d . . . . .
O6 O 0.8164(3) 1.17935(18) -0.04605(14) 0.1108(10) Uani 1 1 d . . . . .
N1 N 0.4752(2) 0.91166(15) 0.38982(12) 0.0473(6) Uani 1 1 d . . . . .
N2 N 0.3265(2) 0.98174(18) 0.46881(14) 0.0625(7) Uani 1 1 d . . . . .
N3 N 0.6770(2) 0.83546(16) 0.20721(12) 0.0482(6) Uani 1 1 d . . . . .
N4 N 0.8121(2) 0.7492(2) 0.13426(15) 0.0644(7) Uani 1 1 d . . . . .
N5 N 0.2696(2) 0.78238(16) 0.40947(13) 0.0515(6) Uani 1 1 d . . . . .
N6 N 0.1776(2) 0.82188(15) 0.27889(13) 0.0501(6) Uani 1 1 d . . . . .
N7 N 0.3757(2) 0.63339(17) 0.30766(15) 0.0553(7) Uani 1 1 d . . . . .
N8 N 0.4434(2) 0.77011(18) 0.17970(13) 0.0538(6) Uani 1 1 d . . . . .
C1 C 0.3137(3) 0.9884(2) 0.26603(16) 0.0506(8) Uani 1 1 d . . . . .
C2 C 0.2477(3) 1.0437(2) 0.20376(19) 0.0692(10) Uani 1 1 d . . . . .
H2 H 0.2562 1.0225 0.1616 0.083 Uiso 1 1 calc R U . . .
C3 C 0.1705(3) 1.1286(3) 0.2031(2) 0.0949(13) Uani 1 1 d . . . . .
H3 H 0.1291 1.1647 0.1603 0.114 Uiso 1 1 calc R U . . .
C4 C 0.1542(3) 1.1604(3) 0.2656(3) 0.0906(13) Uani 1 1 d . . . . .
H4 H 0.1007 1.2174 0.2654 0.109 Uiso 1 1 calc R U . . .
C5 C 0.2166(3) 1.1083(2) 0.3279(2) 0.0704(10) Uani 1 1 d . . . . .
H5 H 0.2046 1.1304 0.3699 0.085 Uiso 1 1 calc R U . . .
C6 C 0.2984(3) 1.0223(2) 0.32981(17) 0.0511(8) Uani 1 1 d . . . . .
C7 C 0.3654(3) 0.9721(2) 0.39664(17) 0.0507(8) Uani 1 1 d . . . . .
C8 C 0.5095(3) 0.8794(2) 0.46254(16) 0.0497(8) Uani 1 1 d . . . . .
C9 C 0.4162(3) 0.9229(2) 0.51181(17) 0.0594(9) Uani 1 1 d . . . . .
C10 C 0.4292(4) 0.8977(3) 0.59105(19) 0.0781(11) Uani 1 1 d . . . . .
H10 H 0.3703 0.9249 0.6248 0.094 Uiso 1 1 calc R U . . .
C11 C 0.5301(4) 0.8321(3) 0.61885(19) 0.0814(12) Uani 1 1 d . . . . .
H11 H 0.5365 0.8144 0.6722 0.098 Uiso 1 1 calc R U . . .
C12 C 0.6227(3) 0.7911(2) 0.57073(18) 0.0657(9) Uani 1 1 d . . . . .
C13 C 0.6146(3) 0.8160(2) 0.48959(16) 0.0525(8) Uani 1 1 d . . . . .
C14 C 0.7137(3) 0.7802(2) 0.43654(18) 0.0551(8) Uani 1 1 d . . . . .
C15 C 0.8214(3) 0.7139(2) 0.4690(2) 0.0635(9) Uani 1 1 d . . . . .
C16 C 0.9154(3) 0.6768(3) 0.4192(2) 0.0809(11) Uani 1 1 d . . . . .
H16 H 0.9083 0.6922 0.3663 0.097 Uiso 1 1 calc R U . . .
C17 C 1.0188(4) 0.6176(3) 0.4478(3) 0.1056(14) Uani 1 1 d . . . . .
H17 H 1.0817 0.5932 0.4142 0.127 Uiso 1 1 calc R U . . .
C18 C 1.0294(5) 0.5945(3) 0.5259(3) 0.1216(18) Uani 1 1 d . . . . .
H18 H 1.1005 0.5556 0.5446 0.146 Uiso 1 1 calc R U . . .
C19 C 0.9371(5) 0.6279(3) 0.5768(3) 0.1075(15) Uani 1 1 d . . . . .
H19 H 0.9448 0.6107 0.6298 0.129 Uiso 1 1 calc R U . . .
C20 C 0.8314(4) 0.6878(2) 0.5487(2) 0.0737(10) Uani 1 1 d . . . . .
C21 C 0.7294(4) 0.7227(2) 0.6040(2) 0.0790(11) Uani 1 1 d . . . . .
C22 C 0.6170(3) 0.6595(2) 0.32807(17) 0.0494(8) Uani 1 1 d . . . . .
C23 C 0.6120(3) 0.5730(2) 0.38806(18) 0.0606(9) Uani 1 1 d . . . . .
H23 H 0.5543 0.5711 0.4329 0.073 Uiso 1 1 calc R U . . .
C24 C 0.6911(3) 0.4911(2) 0.3817(2) 0.0764(10) Uani 1 1 d . . . . .
H24 H 0.6853 0.4345 0.4217 0.092 Uiso 1 1 calc R U . . .
C25 C 0.7789(3) 0.4923(3) 0.3164(2) 0.0801(11) Uani 1 1 d . . . . .
H25 H 0.8304 0.4366 0.3113 0.096 Uiso 1 1 calc R U . . .
C26 C 0.7891(3) 0.5770(3) 0.2592(2) 0.0722(10) Uani 1 1 d . . . . .
H26 H 0.8500 0.5777 0.2161 0.087 Uiso 1 1 calc R U . . .
C27 C 0.7113(3) 0.6620(2) 0.26330(17) 0.0536(8) Uani 1 1 d . . . . .
C28 C 0.7324(3) 0.7484(2) 0.20078(17) 0.0520(8) Uani 1 1 d . . . . .
C29 C 0.7243(2) 0.8964(2) 0.13963(16) 0.0492(8) Uani 1 1 d . . . . .
C30 C 0.8078(3) 0.8417(3) 0.09520(18) 0.0609(9) Uani 1 1 d . . . . .
C31 C 0.8710(3) 0.8872(3) 0.0230(2) 0.0822(11) Uani 1 1 d . . . . .
H31 H 0.9259 0.8531 -0.0075 0.099 Uiso 1 1 calc R U . . .
C32 C 0.8503(3) 0.9827(3) -0.00172(19) 0.0816(11) Uani 1 1 d . . . . .
H32 H 0.8925 1.0129 -0.0496 0.098 Uiso 1 1 calc R U . . .
C33 C 0.7684(3) 1.0378(3) 0.04171(17) 0.0640(9) Uani 1 1 d . . . . .
C34 C 0.7031(3) 0.9931(2) 0.11465(15) 0.0490(8) Uani 1 1 d . . . . .
C35 C 0.6200(3) 1.0485(2) 0.16200(16) 0.0515(8) Uani 1 1 d . . . . .
C36 C 0.5895(3) 1.1514(2) 0.12744(16) 0.0549(8) Uani 1 1 d . . . . .
C37 C 0.4953(3) 1.2042(2) 0.16524(18) 0.0669(9) Uani 1 1 d . . . . .
H37 H 0.4488 1.1742 0.2110 0.080 Uiso 1 1 calc R U . . .
C38 C 0.4701(4) 1.3008(3) 0.1356(2) 0.0826(11) Uani 1 1 d . . . . .
H38 H 0.4064 1.3362 0.1608 0.099 Uiso 1 1 calc R U . . .
C39 C 0.5407(4) 1.3447(3) 0.0678(2) 0.0933(13) Uani 1 1 d . . . . .
H39 H 0.5258 1.4099 0.0484 0.112 Uiso 1 1 calc R U . . .
C40 C 0.6329(4) 1.2926(3) 0.0287(2) 0.0833(12) Uani 1 1 d . . . . .
H40 H 0.6785 1.3230 -0.0174 0.100 Uiso 1 1 calc R U . . .
C41 C 0.6581(3) 1.1958(2) 0.05724(17) 0.0653(9) Uani 1 1 d . . . . .
C42 C 0.7529(3) 1.1404(3) 0.01319(18) 0.0744(11) Uani 1 1 d . . . . .
C43 C 0.3150(3) 0.7577(2) 0.47564(18) 0.0616(9) Uani 1 1 d . . . . .
H43 H 0.3952 0.7254 0.4772 0.074 Uiso 1 1 calc R U . . .
C44 C 0.2473(4) 0.7781(3) 0.54329(18) 0.0754(11) Uani 1 1 d . . . . .
H44 H 0.2813 0.7578 0.5893 0.090 Uiso 1 1 calc R U . . .
C45 C 0.1316(4) 0.8276(3) 0.5408(2) 0.0787(11) Uani 1 1 d . . . . .
H45 H 0.0864 0.8429 0.5850 0.094 Uiso 1 1 calc R U . . .
C46 C 0.0796(3) 0.8559(2) 0.47216(19) 0.0644(9) Uani 1 1 d . . . . .
C47 C -0.0434(4) 0.9069(2) 0.4639(2) 0.0813(12) Uani 1 1 d . . . . .
H47 H -0.0917 0.9276 0.5048 0.098 Uiso 1 1 calc R U . . .
C48 C -0.0894(3) 0.9252(2) 0.3981(2) 0.0844(12) Uani 1 1 d . . . . .
H48 H -0.1691 0.9583 0.3946 0.101 Uiso 1 1 calc R U . . .
C49 C -0.0195(3) 0.8955(2) 0.3336(2) 0.0651(9) Uani 1 1 d . . . . .
C50 C -0.0635(3) 0.9058(2) 0.2665(2) 0.0791(11) Uani 1 1 d . . . . .
H50 H -0.1442 0.9342 0.2617 0.095 Uiso 1 1 calc R U . . .
C51 C 0.0092(3) 0.8754(3) 0.2088(2) 0.0783(11) Uani 1 1 d . . . . .
H51 H -0.0205 0.8813 0.1644 0.094 Uiso 1 1 calc R U . . .
C52 C 0.1305(3) 0.8347(2) 0.21650(18) 0.0647(9) Uani 1 1 d . . . . .
H52 H 0.1809 0.8155 0.1753 0.078 Uiso 1 1 calc R U . . .
C53 C 0.1022(3) 0.8508(2) 0.33800(17) 0.0522(8) Uani 1 1 d . . . . .
C54 C 0.1526(3) 0.82943(19) 0.40825(17) 0.0513(8) Uani 1 1 d . . . . .
C55 C 0.3444(3) 0.5658(2) 0.3718(2) 0.0699(10) Uani 1 1 d . . . . .
H55 H 0.2969 0.5821 0.4150 0.084 Uiso 1 1 calc R U . . .
C56 C 0.3789(4) 0.4711(3) 0.3780(3) 0.0918(12) Uani 1 1 d . . . . .
H56 H 0.3549 0.4255 0.4241 0.110 Uiso 1 1 calc R U . . .
C57 C 0.4490(4) 0.4474(3) 0.3146(3) 0.0958(13) Uani 1 1 d . . . . .
H57 H 0.4735 0.3847 0.3175 0.115 Uiso 1 1 calc R U . . .
C58 C 0.4841(3) 0.5158(3) 0.2460(2) 0.0757(10) Uani 1 1 d . . . . .
C59 C 0.5587(4) 0.4964(3) 0.1777(3) 0.0971(13) Uani 1 1 d . . . . .
H59 H 0.5845 0.4346 0.1779 0.116 Uiso 1 1 calc R U . . .
C60 C 0.5921(4) 0.5645(3) 0.1138(3) 0.0956(14) Uani 1 1 d . . . . .
H60 H 0.6414 0.5494 0.0706 0.115 Uiso 1 1 calc R U . . .
C61 C 0.5537(3) 0.6602(3) 0.1105(2) 0.0695(10) Uani 1 1 d . . . . .
C62 C 0.5862(3) 0.7349(3) 0.0460(2) 0.0823(12) Uani 1 1 d . . . . .
H62 H 0.6353 0.7237 0.0012 0.099 Uiso 1 1 calc R U . . .
C63 C 0.5462(3) 0.8242(3) 0.04840(18) 0.0753(10) Uani 1 1 d . . . . .
H63 H 0.5656 0.8745 0.0050 0.090 Uiso 1 1 calc R U . . .
C64 C 0.4757(3) 0.8387(2) 0.11727(17) 0.0617(9) Uani 1 1 d . . . . .
H64 H 0.4503 0.8995 0.1192 0.074 Uiso 1 1 calc R U . . .
C65 C 0.4809(3) 0.6816(2) 0.17666(18) 0.0547(8) Uani 1 1 d . . . . .
C66 C 0.4452(3) 0.6085(2) 0.2454(2) 0.0576(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 2.003(2) . ?
Co1 N3 2.010(2) . ?
Co1 O4 2.0612(19) . ?
Co1 O1 2.0831(18) . ?
Co1 O5 2.1723(19) . ?
Co1 O2 2.1817(19) . ?
Co1 Co2 3.1061(6) . ?
Co2 O1 2.0511(19) . ?
Co2 O4 2.0990(18) . ?
Co2 N6 2.134(2) . ?
Co2 N5 2.138(2) . ?
Co2 N7 2.141(3) . ?
Co2 N8 2.145(2) . ?
O1 C1 1.337(3) . ?
O2 C14 1.247(3) . ?
O3 C21 1.236(4) . ?
O4 C22 1.337(3) . ?
O5 C35 1.239(3) . ?
O6 C42 1.226(3) . ?
N1 C8 1.357(3) . ?
N1 C7 1.367(3) . ?
N2 C7 1.348(3) . ?
N2 C9 1.365(4) . ?
N3 C29 1.367(3) . ?
N3 C28 1.371(3) . ?
N4 C28 1.349(3) . ?
N4 C30 1.355(4) . ?
N5 C43 1.325(3) . ?
N5 C54 1.355(3) . ?
N6 C52 1.318(3) . ?
N6 C53 1.359(3) . ?
N7 C55 1.321(4) . ?
N7 C66 1.354(4) . ?
N8 C64 1.318(3) . ?
N8 C65 1.353(3) . ?
C1 C2 1.396(4) . ?
C1 C6 1.420(4) . ?
C2 C3 1.374(4) . ?
C3 C4 1.373(5) . ?
C4 C5 1.366(4) . ?
C5 C6 1.403(4) . ?
C6 C7 1.457(4) . ?
C8 C13 1.399(4) . ?
C8 C9 1.426(4) . ?
C9 C10 1.395(4) . ?
C10 C11 1.378(5) . ?
C11 C12 1.390(4) . ?
C12 C13 1.415(4) . ?
C12 C21 1.476(5) . ?
C13 C14 1.450(4) . ?
C14 C15 1.468(4) . ?
C15 C16 1.390(4) . ?
C15 C20 1.392(4) . ?
C16 C17 1.374(4) . ?
C17 C18 1.373(6) . ?
C18 C19 1.367(6) . ?
C19 C20 1.395(5) . ?
C20 C21 1.489(5) . ?
C22 C23 1.403(4) . ?
C22 C27 1.416(4) . ?
C23 C24 1.375(4) . ?
C24 C25 1.380(4) . ?
C25 C26 1.374(4) . ?
C26 C27 1.397(4) . ?
C27 C28 1.460(4) . ?
C29 C34 1.381(4) . ?
C29 C30 1.420(4) . ?
C30 C31 1.401(4) . ?
C31 C32 1.364(4) . ?
C32 C33 1.404(4) . ?
C33 C34 1.415(4) . ?
C33 C42 1.472(4) . ?
C34 C35 1.460(4) . ?
C35 C36 1.469(4) . ?
C36 C37 1.385(4) . ?
C36 C41 1.402(4) . ?
C37 C38 1.376(4) . ?
C38 C39 1.386(5) . ?
C39 C40 1.380(5) . ?
C40 C41 1.379(4) . ?
C41 C42 1.477(5) . ?
C43 C44 1.400(4) . ?
C44 C45 1.352(4) . ?
C45 C46 1.400(4) . ?
C46 C54 1.402(4) . ?
C46 C47 1.441(4) . ?
C47 C48 1.345(5) . ?
C48 C49 1.423(4) . ?
C49 C50 1.389(4) . ?
C49 C53 1.400(4) . ?
C50 C51 1.339(4) . ?
C51 C52 1.395(4) . ?
C53 C54 1.436(4) . ?
C55 C56 1.394(4) . ?
C56 C57 1.365(5) . ?
C57 C58 1.385(5) . ?
C58 C66 1.395(4) . ?
C58 C59 1.428(5) . ?
C59 C60 1.332(5) . ?
C60 C61 1.425(5) . ?
C61 C62 1.394(5) . ?
C61 C65 1.401(4) . ?
C62 C63 1.361(5) . ?
C63 C64 1.395(4) . ?
C65 C66 1.430(4) . ?

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 Co1 N3 166.17(9) . . ?
N1 Co1 O4 102.38(8) . . ?
N3 Co1 O4 87.04(8) . . ?
N1 Co1 O1 86.18(8) . . ?
N3 Co1 O1 105.19(8) . . ?
O4 Co1 O1 83.06(7) . . ?
N1 Co1 O5 87.76(8) . . ?
N3 Co1 O5 85.07(8) . . ?
O4 Co1 O5 165.22(7) . . ?
O1 Co1 O5 86.97(7) . . ?
N1 Co1 O2 84.55(8) . . ?
N3 Co1 O2 85.83(8) . . ?
O4 Co1 O2 87.31(7) . . ?
O1 Co1 O2 164.89(7) . . ?
O5 Co1 O2 104.53(8) . . ?
N1 Co1 Co2 96.45(7) . . ?
N3 Co1 Co2 97.32(7) . . ?
O4 Co1 Co2 42.17(5) . . ?
O1 Co1 Co2 40.91(5) . . ?
O5 Co1 Co2 126.79(6) . . ?
O2 Co1 Co2 128.68(6) . . ?
O1 Co2 O4 82.91(7) . . ?
O1 Co2 N6 95.68(8) . . ?
O4 Co2 N6 168.55(8) . . ?
O1 Co2 N5 92.04(8) . . ?
O4 Co2 N5 91.64(8) . . ?
N6 Co2 N5 77.03(9) . . ?
O1 Co2 N7 164.30(9) . . ?
O4 Co2 N7 89.71(8) . . ?
N6 Co2 N7 94.24(9) . . ?
N5 Co2 N7 102.04(9) . . ?
O1 Co2 N8 89.29(9) . . ?
O4 Co2 N8 92.26(8) . . ?
N6 Co2 N8 99.10(9) . . ?
N5 Co2 N8 176.01(9) . . ?
N7 Co2 N8 77.14(10) . . ?
O1 Co2 Co1 41.69(5) . . ?
O4 Co2 Co1 41.24(5) . . ?
N6 Co2 Co1 136.52(6) . . ?
N5 Co2 Co1 93.38(7) . . ?
N7 Co2 Co1 129.20(6) . . ?
N8 Co2 Co1 90.11(7) . . ?
C1 O1 Co2 130.10(17) . . ?
C1 O1 Co1 121.23(18) . . ?
Co2 O1 Co1 97.40(7) . . ?
C14 O2 Co1 130.0(2) . . ?
C22 O4 Co1 123.46(18) . . ?
C22 O4 Co2 125.37(17) . . ?
Co1 O4 Co2 96.59(7) . . ?
C35 O5 Co1 132.13(19) . . ?
C8 N1 C7 104.8(2) . . ?
C8 N1 Co1 126.8(2) . . ?
C7 N1 Co1 128.07(19) . . ?
C7 N2 C9 103.8(2) . . ?
C29 N3 C28 104.4(2) . . ?
C29 N3 Co1 127.0(2) . . ?
C28 N3 Co1 128.50(19) . . ?
C28 N4 C30 103.8(2) . . ?
C43 N5 C54 117.8(3) . . ?
C43 N5 Co2 128.5(2) . . ?
C54 N5 Co2 113.10(19) . . ?
C52 N6 C53 117.1(3) . . ?
C52 N6 Co2 128.9(2) . . ?
C53 N6 Co2 113.63(19) . . ?
C55 N7 C66 117.7(3) . . ?
C55 N7 Co2 128.0(2) . . ?
C66 N7 Co2 113.1(2) . . ?
C64 N8 C65 118.2(3) . . ?
C64 N8 Co2 127.6(2) . . ?
C65 N8 Co2 113.3(2) . . ?
O1 C1 C2 119.2(3) . . ?
O1 C1 C6 122.8(3) . . ?
C2 C1 C6 118.0(3) . . ?
C3 C2 C1 121.7(3) . . ?
C4 C3 C2 120.2(3) . . ?
C5 C4 C3 120.0(3) . . ?
C4 C5 C6 121.5(3) . . ?
C5 C6 C1 118.6(3) . . ?
C5 C6 C7 118.6(3) . . ?
C1 C6 C7 122.8(3) . . ?
N2 C7 N1 114.7(3) . . ?
N2 C7 C6 123.8(3) . . ?
N1 C7 C6 121.5(2) . . ?
N1 C8 C13 129.8(3) . . ?
N1 C8 C9 107.5(3) . . ?
C13 C8 C9 122.8(3) . . ?
N2 C9 C10 132.6(3) . . ?
N2 C9 C8 109.3(3) . . ?
C10 C9 C8 118.0(3) . . ?
C11 C10 C9 119.4(3) . . ?
C10 C11 C12 122.9(3) . . ?
C11 C12 C13 119.7(3) . . ?
C11 C12 C21 120.1(3) . . ?
C13 C12 C21 120.3(3) . . ?
C8 C13 C12 117.2(3) . . ?
C8 C13 C14 121.8(3) . . ?
C12 C13 C14 121.0(3) . . ?
O2 C14 C13 122.3(3) . . ?
O2 C14 C15 118.8(3) . . ?
C13 C14 C15 118.9(3) . . ?
C16 C15 C20 119.3(3) . . ?
C16 C15 C14 119.5(3) . . ?
C20 C15 C14 121.2(3) . . ?
C17 C16 C15 120.3(4) . . ?
C18 C17 C16 120.0(4) . . ?
C19 C18 C17 121.0(4) . . ?
C18 C19 C20 119.6(4) . . ?
C15 C20 C19 119.7(4) . . ?
C15 C20 C21 120.3(3) . . ?
C19 C20 C21 120.0(4) . . ?
O3 C21 C12 121.0(4) . . ?
O3 C21 C20 120.9(4) . . ?
C12 C21 C20 118.1(3) . . ?
O4 C22 C23 118.0(3) . . ?
O4 C22 C27 123.5(3) . . ?
C23 C22 C27 118.5(3) . . ?
C24 C23 C22 121.1(3) . . ?
C23 C24 C25 120.6(3) . . ?
C26 C25 C24 119.0(3) . . ?
C25 C26 C27 122.4(3) . . ?
C26 C27 C22 118.2(3) . . ?
C26 C27 C28 118.1(3) . . ?
C22 C27 C28 123.7(3) . . ?
N4 C28 N3 114.5(3) . . ?
N4 C28 C27 123.1(3) . . ?
N3 C28 C27 122.3(3) . . ?
N3 C29 C34 130.2(3) . . ?
N3 C29 C30 107.2(3) . . ?
C34 C29 C30 122.6(3) . . ?
N4 C30 C31 131.0(3) . . ?
N4 C30 C29 110.1(3) . . ?
C31 C30 C29 118.9(3) . . ?
C32 C31 C30 118.5(3) . . ?
C31 C32 C33 123.2(3) . . ?
C32 C33 C34 119.2(3) . . ?
C32 C33 C42 120.7(3) . . ?
C34 C33 C42 120.1(3) . . ?
C29 C34 C33 117.5(3) . . ?
C29 C34 C35 122.2(3) . . ?
C33 C34 C35 120.2(3) . . ?
O5 C35 C34 121.8(3) . . ?
O5 C35 C36 119.0(3) . . ?
C34 C35 C36 119.2(3) . . ?
C37 C36 C41 120.2(3) . . ?
C37 C36 C35 120.0(3) . . ?
C41 C36 C35 119.7(3) . . ?
C38 C37 C36 120.5(3) . . ?
C37 C38 C39 119.2(4) . . ?
C40 C39 C38 120.7(4) . . ?
C41 C40 C39 120.6(4) . . ?
C40 C41 C36 118.7(3) . . ?
C40 C41 C42 120.4(3) . . ?
C36 C41 C42 120.8(3) . . ?
O6 C42 C33 121.0(4) . . ?
O6 C42 C41 120.5(4) . . ?
C33 C42 C41 118.5(3) . . ?
N5 C43 C44 122.8(3) . . ?
C45 C44 C43 119.1(3) . . ?
C44 C45 C46 120.4(3) . . ?
C45 C46 C54 116.7(3) . . ?
C45 C46 C47 124.8(3) . . ?
C54 C46 C47 118.4(3) . . ?
C48 C47 C46 121.2(3) . . ?
C47 C48 C49 121.8(4) . . ?
C50 C49 C53 117.0(3) . . ?
C50 C49 C48 124.8(4) . . ?
C53 C49 C48 118.2(3) . . ?
C51 C50 C49 120.6(3) . . ?
C50 C51 C52 118.8(3) . . ?
N6 C52 C51 123.6(3) . . ?
N6 C53 C49 122.9(3) . . ?
N6 C53 C54 116.3(3) . . ?
C49 C53 C54 120.7(3) . . ?
N5 C54 C46 123.2(3) . . ?
N5 C54 C53 117.3(3) . . ?
C46 C54 C53 119.5(3) . . ?
N7 C55 C56 123.4(3) . . ?
C57 C56 C55 118.1(4) . . ?
C56 C57 C58 120.7(4) . . ?
C57 C58 C66 117.0(4) . . ?
C57 C58 C59 123.9(4) . . ?
C66 C58 C59 119.0(4) . . ?
C60 C59 C58 121.6(4) . . ?
C59 C60 C61 121.2(4) . . ?
C62 C61 C65 117.1(3) . . ?
C62 C61 C60 124.3(4) . . ?
C65 C61 C60 118.6(4) . . ?
C63 C62 C61 120.3(3) . . ?
C62 C63 C64 118.7(3) . . ?
N8 C64 C63 123.1(3) . . ?
N8 C65 C61 122.7(3) . . ?
N8 C65 C66 117.1(3) . . ?
C61 C65 C66 120.2(3) . . ?
N7 C66 C58 123.1(3) . . ?
N7 C66 C65 117.5(3) . . ?
C58 C66 C65 119.3(3) . . ?

_refine_diff_density_max         0.278
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.045

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 650 160 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?



