# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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 1963321'
loop_
_audit_author_name
_audit_author_address
'Liang Shuang'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-01-06 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            'C33 H17 Cu2 N4 O9'
_chemical_formula_weight         740.61

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           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                   15.6642(7)
_cell_length_b                   14.0331(7)
_cell_length_c                   26.9234(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.8660(10)
_cell_angle_gamma                90
_cell_volume                     5910.8(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5252
_cell_measurement_theta_min      1.515
_cell_measurement_theta_max      28.379

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_F_000             2984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.505
_shelx_estimated_absorpt_T_min   0.806
_shelx_estimated_absorpt_T_max   0.852
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21587
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.515
_diffrn_reflns_theta_max         28.379
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7367
_reflns_number_gt                5359
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_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)+(0.0707P)²+4.2874P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7367
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1259
_refine_ls_wR_factor_gt          0.1116
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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
Cu1 Cu 0.83397(2) 0.19914(3) 0.50935(2) 0.02430(11) Uani 1 1 d . . . . .
O1 O 0.94511(13) 0.19983(15) 0.48215(8) 0.0320(5) Uani 1 1 d . . . . .
N1 N 0.62967(15) 0.14968(19) 0.63762(10) 0.0308(6) Uani 1 1 d . . . . .
C1 C 0.7093(2) 0.4049(2) 0.59843(12) 0.0342(7) Uani 1 1 d . . . . .
H1A H 0.7604 0.4080 0.5824 0.041 Uiso 1 1 d R U . . .
O1W O 0.8861(2) 0.4795(3) 0.5118(2) 0.142(2) Uani 1 1 d . . . . .
Cu2 Cu 0.73623(2) 0.19405(3) 0.60489(2) 0.02605(11) Uani 1 1 d . . . . .
O2 O 0.99709(15) 0.34789(17) 0.47413(10) 0.0473(7) Uani 1 1 d . . . . .
N2 N 0.68258(15) 0.32088(18) 0.61416(9) 0.0271(6) Uani 1 1 d . . . . .
C2 C 0.6636(2) 0.4883(3) 0.60499(15) 0.0440(9) Uani 1 1 d . . . . .
H2A H 0.6830 0.5456 0.5924 0.053 Uiso 1 1 d R U . . .
O3 O 1.64335(14) 0.2597(2) 0.32395(9) 0.0462(6) Uani 1 1 d . . . . .
N3 N 0.44137(16) 0.46517(19) 0.68774(9) 0.0303(6) Uani 1 1 d . . . . .
C3 C 0.5891(2) 0.4853(2) 0.63041(13) 0.0394(8) Uani 1 1 d . . . . .
H3A H 0.5582 0.5408 0.6356 0.047 Uiso 1 1 d R U . . .
O4 O 1.64980(13) 0.25000(16) 0.40585(8) 0.0322(5) Uani 1 1 d . . . . .
N4 N 0.38930(16) 0.28148(19) 0.71814(10) 0.0298(6) Uani 1 1 d . . . . .
C4 C 0.56077(17) 0.3980(2) 0.64821(11) 0.0263(6) Uani 1 1 d . . . . .
O5 O 0.85837(13) 0.07119(15) 0.53388(8) 0.0332(5) Uani 1 1 d . . . . .
C5 C 0.48396(17) 0.3874(2) 0.67641(10) 0.0258(6) Uani 1 1 d . . . . .
O6 O 0.77784(13) 0.06378(15) 0.60124(8) 0.0302(5) Uani 1 1 d . . . . .
C6 C 0.37106(18) 0.4530(2) 0.71429(11) 0.0297(7) Uani 1 1 d . . . . .
O7 O 1.25016(13) 0.28781(15) 0.36865(9) 0.0350(5) Uani 1 1 d . . . . .
C7 C 0.3223(2) 0.5341(3) 0.72712(13) 0.0420(9) Uani 1 1 d . . . . .
H7A H 0.3383 0.5947 0.7170 0.050 Uiso 1 1 d R U . . .
C8 C 0.2523(2) 0.5221(3) 0.75426(14) 0.0475(9) Uani 1 1 d . . . . .
H8A H 0.2207 0.5753 0.7628 0.057 Uiso 1 1 d R U . . .
O8 O 0.78885(12) 0.31328(14) 0.47761(8) 0.0255(4) Uani 1 1 d . . . . .
C9 C 0.2263(2) 0.4314(3) 0.76981(13) 0.0446(9) Uani 1 1 d . . . . .
H9A H 0.1778 0.4253 0.7881 0.054 Uiso 1 1 d R U . . .
C11 C 0.34526(18) 0.3612(2) 0.72988(11) 0.0300(7) Uani 1 1 d . . . . .
C12 C 0.45705(18) 0.2947(2) 0.69119(11) 0.0267(6) Uani 1 1 d . . . . .
C13 C 0.50597(18) 0.2104(2) 0.67700(12) 0.0280(7) Uani 1 1 d . . . . .
C14 C 0.4804(2) 0.1174(3) 0.68633(14) 0.0426(9) Uani 1 1 d . . . . .
H14A H 0.4308 0.1060 0.7030 0.051 Uiso 1 1 d R U . . .
C15 C 0.5286(2) 0.0424(3) 0.67080(17) 0.0555(11) Uani 1 1 d . . . . .
H15A H 0.5117 -0.0201 0.6762 0.067 Uiso 1 1 d R U . . .
C16 C 0.6038(2) 0.0617(3) 0.64665(15) 0.0447(9) Uani 1 1 d . . . . .
H16A H 0.6369 0.0109 0.6366 0.054 Uiso 1 1 d R U . . .
C17 C 0.58037(18) 0.2234(2) 0.65201(11) 0.0248(6) Uani 1 1 d . . . . .
C18 C 0.60886(17) 0.3175(2) 0.63810(10) 0.0237(6) Uani 1 1 d . . . . .
C19 C 1.00052(18) 0.2605(2) 0.46937(11) 0.0258(6) Uani 1 1 d . . . . .
C20 C 1.07719(17) 0.2162(2) 0.44648(10) 0.0221(6) Uani 1 1 d . . . . .
C21 C 1.09094(17) 0.1182(2) 0.45039(10) 0.0228(6) Uani 1 1 d . . . . .
H21A H 1.0549 0.0809 0.4687 0.027 Uiso 1 1 d R U . . .
C22 C 1.15871(17) 0.0762(2) 0.42684(10) 0.0223(6) Uani 1 1 d . . . . .
C23 C 1.21187(17) 0.1326(2) 0.39939(11) 0.0258(6) Uani 1 1 d . . . . .
H23A H 1.2558 0.1048 0.3825 0.031 Uiso 1 1 d R U . . .
C24 C 1.19952(17) 0.2295(2) 0.39721(11) 0.0249(6) Uani 1 1 d . . . . .
C25 C 1.13341(18) 0.2725(2) 0.42077(11) 0.0264(6) Uani 1 1 d . . . . .
H25A H 1.1265 0.3383 0.4195 0.032 Uiso 1 1 d R U . . .
C26 C 1.33696(18) 0.2673(2) 0.36793(12) 0.0274(6) Uani 1 1 d . . . . .
C27 C 1.3844(2) 0.2430(3) 0.41016(13) 0.0467(10) Uani 1 1 d . . . . .
H27A H 1.3581 0.2327 0.4399 0.056 Uiso 1 1 d R U . . .
C28 C 1.4721(2) 0.2338(3) 0.40786(13) 0.0469(10) Uani 1 1 d . . . . .
H28A H 1.5045 0.2169 0.4364 0.056 Uiso 1 1 d R U . . .
C29 C 1.51235(19) 0.2492(2) 0.36427(11) 0.0285(7) Uani 1 1 d . . . . .
C30 C 1.4633(2) 0.2703(3) 0.32220(12) 0.0387(8) Uani 1 1 d . . . . .
H30A H 1.4893 0.2794 0.2923 0.046 Uiso 1 1 d R U . . .
C31 C 1.3749(2) 0.2782(3) 0.32368(12) 0.0380(8) Uani 1 1 d . . . . .
H31A H 1.3419 0.2908 0.2948 0.046 Uiso 1 1 d R U . . .
C32 C 1.60832(18) 0.2514(2) 0.36400(12) 0.0297(7) Uani 1 1 d . . . . .
C33 C 0.82498(17) 0.0278(2) 0.56894(11) 0.0248(6) Uani 1 1 d . . . . .
C100 C 0.27178(19) 0.3524(3) 0.75830(12) 0.0367(8) Uani 1 1 d . . . . .
H10A H 0.2547 0.2927 0.7690 0.044 Uiso 1 1 d 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 O1 1.9222(19) . ?
Cu1 O8 1.932(2) . ?
Cu1 O5 1.945(2) . ?
Cu1 O8 1.9805(18) 7_656 ?
Cu1 O4 2.394(2) 7_756 ?
Cu1 Cu1 3.0130(7) 7_656 ?
Cu1 Cu2 3.0594(5) . ?
O1 C19 1.275(4) . ?
N1 C16 1.325(4) . ?
N1 C17 1.359(4) . ?
N1 Cu2 2.024(2) . ?
C1 N2 1.328(4) . ?
C1 C2 1.386(5) . ?
Cu2 O6 1.945(2) . ?
Cu2 O4 1.985(2) 7_756 ?
Cu2 N2 1.989(3) . ?
Cu2 O8 2.239(2) 7_656 ?
O2 C19 1.234(4) . ?
N2 C18 1.351(3) . ?
C2 C3 1.384(4) . ?
O3 C32 1.240(4) . ?
N3 C5 1.323(4) . ?
N3 C6 1.354(4) . ?
C3 C4 1.397(4) . ?
O4 C32 1.272(4) . ?
O4 Cu2 1.985(2) 7_756 ?
O4 Cu1 2.394(2) 7_756 ?
N4 C12 1.328(4) . ?
N4 C11 1.360(4) . ?
C4 C18 1.391(4) . ?
C4 C5 1.462(4) . ?
O5 C33 1.259(3) . ?
C5 C12 1.430(4) . ?
O6 C33 1.273(3) . ?
C6 C11 1.419(5) . ?
C6 C7 1.423(4) . ?
O7 C26 1.391(3) . ?
O7 C24 1.397(3) . ?
C7 C8 1.359(4) . ?
C8 C9 1.407(5) . ?
O8 Cu1 1.9805(18) 7_656 ?
O8 Cu2 2.239(2) 7_656 ?
C9 C100 1.362(5) . ?
C11 C100 1.419(4) . ?
C12 C13 1.470(4) . ?
C13 C17 1.387(4) . ?
C13 C14 1.392(5) . ?
C14 C15 1.373(5) . ?
C15 C16 1.400(4) . ?
C17 C18 1.450(4) . ?
C19 C20 1.511(4) . ?
C20 C25 1.393(4) . ?
C20 C21 1.395(4) . ?
C21 C22 1.394(3) . ?
C22 C23 1.388(4) . ?
C22 C33 1.486(4) 5_756 ?
C23 C24 1.374(4) . ?
C24 C25 1.380(4) . ?
C26 C31 1.366(4) . ?
C26 C27 1.370(5) . ?
C27 C28 1.384(4) . ?
C28 C29 1.377(4) . ?
C29 C30 1.369(5) . ?
C29 C32 1.504(4) . ?
C30 C31 1.391(4) . ?
C33 C22 1.486(4) 5_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O8 98.37(9) . . ?
O1 Cu1 O5 88.14(9) . . ?
O8 Cu1 O5 167.64(10) . . ?
O1 Cu1 O8 166.99(9) . 7_656 ?
O8 Cu1 O8 79.30(9) . 7_656 ?
O5 Cu1 O8 91.99(8) . 7_656 ?
O1 Cu1 O4 107.87(9) . 7_756 ?
O8 Cu1 O4 101.17(8) . 7_756 ?
O5 Cu1 O4 86.65(9) . 7_756 ?
O8 Cu1 O4 85.12(8) 7_656 7_756 ?
O1 Cu1 Cu1 137.21(7) . 7_656 ?
O8 Cu1 Cu1 40.23(5) . 7_656 ?
O5 Cu1 Cu1 130.49(6) . 7_656 ?
O8 Cu1 Cu1 39.07(6) 7_656 7_656 ?
O4 Cu1 Cu1 93.92(5) 7_756 7_656 ?
O1 Cu1 Cu2 145.21(7) . . ?
O8 Cu1 Cu2 101.76(6) . . ?
O5 Cu1 Cu2 77.93(6) . . ?
O8 Cu1 Cu2 46.96(6) 7_656 . ?
O4 Cu1 Cu2 40.42(5) 7_756 . ?
Cu1 Cu1 Cu2 71.463(13) 7_656 . ?
C19 O1 Cu1 138.4(2) . . ?
C16 N1 C17 118.3(3) . . ?
C16 N1 Cu2 129.2(2) . . ?
C17 N1 Cu2 112.5(2) . . ?
N2 C1 C2 122.4(3) . . ?
O6 Cu2 O4 93.34(9) . 7_756 ?
O6 Cu2 N2 172.76(9) . . ?
O4 Cu2 N2 93.04(10) 7_756 . ?
O6 Cu2 N1 91.07(10) . . ?
O4 Cu2 N1 162.26(11) 7_756 . ?
N2 Cu2 N1 81.82(10) . . ?
O6 Cu2 O8 87.09(8) . 7_656 ?
O4 Cu2 O8 89.32(8) 7_756 7_656 ?
N2 Cu2 O8 96.39(9) . 7_656 ?
N1 Cu2 O8 108.07(9) . 7_656 ?
O6 Cu2 Cu1 78.25(6) . . ?
O4 Cu2 Cu1 51.44(6) 7_756 . ?
N2 Cu2 Cu1 108.47(7) . . ?
N1 Cu2 Cu1 146.25(8) . . ?
O8 Cu2 Cu1 40.29(5) 7_656 . ?
C1 N2 C18 118.2(3) . . ?
C1 N2 Cu2 127.8(2) . . ?
C18 N2 Cu2 113.9(2) . . ?
C3 C2 C1 119.4(3) . . ?
C5 N3 C6 116.8(3) . . ?
C2 C3 C4 119.1(3) . . ?
C32 O4 Cu2 106.74(18) . 7_756 ?
C32 O4 Cu1 149.90(19) . 7_756 ?
Cu2 O4 Cu1 88.14(8) 7_756 7_756 ?
C12 N4 C11 116.1(3) . . ?
C18 C4 C3 117.4(3) . . ?
C18 C4 C5 119.1(3) . . ?
C3 C4 C5 123.4(3) . . ?
C33 O5 Cu1 128.24(18) . . ?
N3 C5 C12 121.8(2) . . ?
N3 C5 C4 118.3(3) . . ?
C12 C5 C4 119.9(3) . . ?
C33 O6 Cu2 127.90(19) . . ?
N3 C6 C11 121.5(3) . . ?
N3 C6 C7 119.2(3) . . ?
C11 C6 C7 119.3(3) . . ?
C26 O7 C24 118.0(2) . . ?
C8 C7 C6 119.3(4) . . ?
C7 C8 C9 121.6(3) . . ?
Cu1 O8 Cu1 100.70(9) . 7_656 ?
Cu1 O8 Cu2 116.28(10) . 7_656 ?
Cu1 O8 Cu2 92.75(8) 7_656 7_656 ?
C100 C9 C8 120.5(3) . . ?
N4 C11 C6 121.5(3) . . ?
N4 C11 C100 119.2(3) . . ?
C6 C11 C100 119.3(3) . . ?
N4 C12 C5 122.3(3) . . ?
N4 C12 C13 118.1(3) . . ?
C5 C12 C13 119.7(2) . . ?
C17 C13 C14 117.8(3) . . ?
C17 C13 C12 118.8(3) . . ?
C14 C13 C12 123.3(3) . . ?
C15 C14 C13 119.8(3) . . ?
C14 C15 C16 118.8(3) . . ?
N1 C16 C15 122.5(3) . . ?
N1 C17 C13 122.8(3) . . ?
N1 C17 C18 115.7(2) . . ?
C13 C17 C18 121.5(3) . . ?
N2 C18 C4 123.3(3) . . ?
N2 C18 C17 115.9(2) . . ?
C4 C18 C17 120.8(2) . . ?
O2 C19 O1 127.0(3) . . ?
O2 C19 C20 119.4(3) . . ?
O1 C19 C20 113.6(3) . . ?
C25 C20 C21 119.8(2) . . ?
C25 C20 C19 120.3(3) . . ?
C21 C20 C19 119.9(2) . . ?
C22 C21 C20 120.0(3) . . ?
C23 C22 C21 119.5(3) . . ?
C23 C22 C33 119.7(2) . 5_756 ?
C21 C22 C33 120.8(2) . 5_756 ?
C24 C23 C22 120.0(2) . . ?
C23 C24 C25 121.3(3) . . ?
C23 C24 O7 121.4(2) . . ?
C25 C24 O7 117.2(3) . . ?
C24 C25 C20 119.2(3) . . ?
C31 C26 C27 120.6(3) . . ?
C31 C26 O7 117.2(3) . . ?
C27 C26 O7 122.0(3) . . ?
C26 C27 C28 119.0(3) . . ?
C29 C28 C27 121.5(3) . . ?
C30 C29 C28 118.5(3) . . ?
C30 C29 C32 120.8(3) . . ?
C28 C29 C32 120.5(3) . . ?
C29 C30 C31 120.8(3) . . ?
C26 C31 C30 119.6(3) . . ?
O3 C32 O4 122.9(3) . . ?
O3 C32 C29 119.5(3) . . ?
O4 C32 C29 117.5(2) . . ?
O5 C33 O6 126.7(3) . . ?
O5 C33 C22 117.1(2) . 5_756 ?
O6 C33 C22 116.1(2) . 5_756 ?
C9 C100 C11 119.9(3) . . ?

_refine_diff_density_max         0.584
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.082

####################################################################### 
# 
# 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 1963322'
loop_
_audit_author_name
_audit_author_address
'Liang Shuang'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-12-27 deposited with the CCDC.	2020-01-06 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         'C33 H18 Co N4 O7, H2 O'
_chemical_formula_sum            'C33 H20 Co N4 O8'
_chemical_formula_weight         659.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.6768(6)
_cell_length_b                   22.9016(18)
_cell_length_c                   15.1581(12)
_cell_angle_alpha                90
_cell_angle_beta                 94.189(2)
_cell_angle_gamma                90
_cell_volume                     2657.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1649
_cell_measurement_theta_min      2.231
_cell_measurement_theta_max      23.084

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_F_000             1348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.713
_shelx_estimated_absorpt_T_min   0.901
_shelx_estimated_absorpt_T_max   0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15601
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.614
_diffrn_reflns_theta_max         25.352
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4855
_reflns_number_gt                2985
_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       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT-plus (Bruker, 2007)'
_computing_data_reduction        'SAINT-plus (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0506P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4855
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_ref         0.1172
_refine_ls_wR_factor_gt          0.0997
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.00890(6) 0.02809(2) 0.13627(3) 0.02862(17) Uani 1 1 d . . . . .
O1W O -0.5895(5) 0.1950(2) -0.5265(3) 0.1208(17) Uani 1 1 d . . . . .
H1A H -0.4731 0.1907 -0.5047 0.145 Uiso 1 1 d R U . . .
H1B H -0.6095 0.2339 -0.5141 0.145 Uiso 1 1 d R U . . .
O1 O 0.8498(3) 0.09060(13) 0.08837(19) 0.0465(8) Uani 1 1 d . . . . .
O2 O 0.9335(3) 0.17196(14) 0.0242(2) 0.0536(9) Uani 1 1 d . . . . .
O3 O 0.1142(3) 0.03864(12) -0.07434(18) 0.0423(8) Uani 1 1 d . . . . .
O4 O 0.2191(3) 0.03967(12) 0.06760(17) 0.0372(7) Uani 1 1 d . . . . .
O5 O -0.2237(4) 0.24283(13) -0.4692(2) 0.0540(9) Uani 1 1 d . . . . .
O6 O -0.2935(4) 0.30695(14) -0.3677(2) 0.0553(9) Uani 1 1 d . . . . .
H6A H -0.3870 0.3120 -0.4057 0.066 Uiso 1 1 d R U . . .
O7 O 0.4283(3) 0.21813(11) -0.19030(18) 0.0372(7) Uani 1 1 d . . . . .
N1 N 0.0250(4) 0.06907(13) 0.2625(2) 0.0305(8) Uani 1 1 d . . . . .
N2 N 0.1279(4) -0.03676(13) 0.22328(19) 0.0274(8) Uani 1 1 d . . . . .
N3 N 0.2283(4) 0.04227(13) 0.5680(2) 0.0298(8) Uani 1 1 d . . . . .
N4 N 0.3539(4) -0.06947(14) 0.5236(2) 0.0309(8) Uani 1 1 d . . . . .
C1 C 0.6444(4) 0.13762(16) -0.0092(2) 0.0238(9) Uani 1 1 d . . . . .
C2 C 0.5184(4) 0.09729(15) 0.0108(2) 0.0244(9) Uani 1 1 d . . . . .
H2 H 0.5434 0.0700 0.0553 0.029 Uiso 1 1 calc R U . . .
C3 C 0.3554(4) 0.09739(15) -0.0351(2) 0.0224(9) Uani 1 1 d . . . . .
C4 C 0.3202(4) 0.13763(15) -0.1037(2) 0.0257(9) Uani 1 1 d . . . . .
H4 H 0.2134 0.1370 -0.1368 0.031 Uiso 1 1 calc R U . . .
C5 C 0.4458(4) 0.17814(15) -0.1215(2) 0.0242(9) Uani 1 1 d . . . . .
C6 C 0.6059(4) 0.17920(16) -0.0742(2) 0.0261(9) Uani 1 1 d . . . . .
H6 H 0.6877 0.2076 -0.0858 0.031 Uiso 1 1 calc R U . . .
C7 C 0.8249(5) 0.13366(19) 0.0383(3) 0.0320(10) Uani 1 1 d . . . . .
C8 C 0.2188(5) 0.05516(16) -0.0122(3) 0.0275(9) Uani 1 1 d . . . . .
C9 C 0.2659(5) 0.22658(16) -0.2376(3) 0.0313(10) Uani 1 1 d . . . . .
C10 C 0.1275(5) 0.25010(17) -0.1985(3) 0.0356(10) Uani 1 1 d . . . . .
H10 H 0.1332 0.2561 -0.1377 0.043 Uiso 1 1 calc R U . . .
C11 C -0.0227(5) 0.26503(18) -0.2510(3) 0.0377(11) Uani 1 1 d . . . . .
H11 H -0.1164 0.2823 -0.2255 0.045 Uiso 1 1 calc R U . . .
C12 C -0.0324(5) 0.25414(17) -0.3408(3) 0.0317(10) Uani 1 1 d . . . . .
C13 C 0.1087(5) 0.22957(18) -0.3777(3) 0.0390(11) Uani 1 1 d . . . . .
H13 H 0.1027 0.2220 -0.4381 0.047 Uiso 1 1 calc R U . . .
C14 C 0.2584(5) 0.21612(18) -0.3266(3) 0.0417(11) Uani 1 1 d . . . . .
H14 H 0.3539 0.2001 -0.3522 0.050 Uiso 1 1 calc R U . . .
C15 C -0.1932(5) 0.26730(19) -0.3990(3) 0.0374(11) Uani 1 1 d . . . . .
C16 C -0.0330(5) 0.12239(18) 0.2821(3) 0.0408(11) Uani 1 1 d . . . . .
H16 H -0.0858 0.1449 0.2366 0.049 Uiso 1 1 calc R U . . .
C17 C -0.0184(6) 0.14543(18) 0.3660(3) 0.0457(12) Uani 1 1 d . . . . .
H17 H -0.0612 0.1826 0.3761 0.055 Uiso 1 1 calc R U . . .
C18 C 0.0590(5) 0.11383(17) 0.4348(3) 0.0379(11) Uani 1 1 d . . . . .
H18 H 0.0701 0.1292 0.4917 0.045 Uiso 1 1 calc R U . . .
C19 C 0.1211(5) 0.05801(16) 0.4175(2) 0.0260(9) Uani 1 1 d . . . . .
C20 C 0.1006(4) 0.03751(16) 0.3307(2) 0.0264(9) Uani 1 1 d . . . . .
C21 C 0.1584(4) -0.02054(16) 0.3085(2) 0.0247(9) Uani 1 1 d . . . . .
C22 C 0.2378(5) -0.05698(16) 0.3731(2) 0.0255(9) Uani 1 1 d . . . . .
C23 C 0.2827(5) -0.11327(17) 0.3483(3) 0.0341(10) Uani 1 1 d . . . . .
H23 H 0.3346 -0.1390 0.3897 0.041 Uiso 1 1 calc R U . . .
C24 C 0.2492(5) -0.13030(17) 0.2618(3) 0.0360(10) Uani 1 1 d . . . . .
H24 H 0.2777 -0.1677 0.2440 0.043 Uiso 1 1 calc R U . . .
C25 C 0.1725(5) -0.09087(17) 0.2016(3) 0.0347(10) Uani 1 1 d . . . . .
H25 H 0.1510 -0.1027 0.1431 0.042 Uiso 1 1 calc R U . . .
C26 C 0.2681(4) -0.03538(16) 0.4636(2) 0.0267(9) Uani 1 1 d . . . . .
C27 C 0.2077(4) 0.02106(16) 0.4861(2) 0.0260(9) Uani 1 1 d . . . . .
C28 C 0.3142(5) 0.00770(17) 0.6297(3) 0.0294(10) Uani 1 1 d . . . . .
C29 C 0.3788(5) -0.04825(17) 0.6072(2) 0.0286(9) Uani 1 1 d . . . . .
C30 C 0.4711(5) -0.08217(19) 0.6728(3) 0.0367(11) Uani 1 1 d . . . . .
H30 H 0.5125 -0.1190 0.6589 0.044 Uiso 1 1 calc R U . . .
C31 C 0.4991(5) -0.0610(2) 0.7559(3) 0.0405(11) Uani 1 1 d . . . . .
H31 H 0.5613 -0.0833 0.7987 0.049 Uiso 1 1 calc R U . . .
C32 C 0.4354(5) -0.0055(2) 0.7787(3) 0.0399(11) Uani 1 1 d . . . . .
H32 H 0.4566 0.0082 0.8362 0.048 Uiso 1 1 calc R U . . .
C33 C 0.3437(5) 0.02795(19) 0.7179(3) 0.0366(10) Uani 1 1 d . . . . .
H33 H 0.3003 0.0640 0.7339 0.044 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
Co1 O1 1.984(3) 1_455 ?
Co1 O3 1.995(3) 3 ?
Co1 O4 2.001(3) . ?
Co1 N1 2.126(3) . ?
Co1 N2 2.146(3) . ?
O1W H1A 0.9353 . ?
O1W H1B 0.9249 . ?
O1 C7 1.251(4) . ?
O2 C7 1.239(5) . ?
O3 C8 1.251(4) . ?
O4 C8 1.261(4) . ?
O5 C15 1.211(5) . ?
O6 C15 1.302(5) . ?
O6 H6A 0.8950 . ?
O7 C5 1.387(4) . ?
O7 C9 1.405(4) . ?
N1 C16 1.341(5) . ?
N1 C20 1.357(4) . ?
N2 C25 1.333(5) . ?
N2 C21 1.349(4) . ?
N3 C27 1.331(5) . ?
N3 C28 1.359(4) . ?
N4 C26 1.335(4) . ?
N4 C29 1.358(4) . ?
C1 C2 1.387(5) . ?
C1 C6 1.387(5) . ?
C1 C7 1.517(5) . ?
C2 C3 1.387(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.400(5) . ?
C3 C8 1.486(5) . ?
C4 C5 1.379(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(4) . ?
C6 H6 0.9300 . ?
C9 C10 1.365(6) . ?
C9 C14 1.367(6) . ?
C10 C11 1.395(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.381(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.375(6) . ?
C12 C15 1.494(5) . ?
C13 C14 1.374(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C16 C17 1.374(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.368(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.396(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.396(5) . ?
C19 C27 1.462(5) . ?
C20 C21 1.449(5) . ?
C21 C22 1.392(5) . ?
C22 C23 1.393(5) . ?
C22 C26 1.461(5) . ?
C23 C24 1.373(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.385(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.423(5) . ?
C28 C33 1.417(5) . ?
C28 C29 1.424(5) . ?
C29 C30 1.411(5) . ?
C30 C31 1.353(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.414(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.356(5) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O3 97.05(11) 1_455 3 ?
O1 Co1 O4 102.24(11) 1_455 . ?
O3 Co1 O4 103.24(12) 3 . ?
O1 Co1 N1 90.26(12) 1_455 . ?
O3 Co1 N1 139.10(12) 3 . ?
O4 Co1 N1 114.43(11) . . ?
O1 Co1 N2 161.30(12) 1_455 . ?
O3 Co1 N2 85.69(11) 3 . ?
O4 Co1 N2 95.07(11) . . ?
N1 Co1 N2 76.02(12) . . ?
H1A O1W H1B 101.5 . . ?
C7 O1 Co1 148.6(3) . 1_655 ?
C8 O3 Co1 147.4(3) . 3 ?
C8 O4 Co1 126.3(2) . . ?
C15 O6 H6A 108.8 . . ?
C5 O7 C9 120.6(3) . . ?
C16 N1 C20 116.5(3) . . ?
C16 N1 Co1 127.1(3) . . ?
C20 N1 Co1 116.4(3) . . ?
C25 N2 C21 117.6(3) . . ?
C25 N2 Co1 126.7(3) . . ?
C21 N2 Co1 115.8(2) . . ?
C27 N3 C28 116.6(3) . . ?
C26 N4 C29 117.1(3) . . ?
C2 C1 C6 119.8(3) . . ?
C2 C1 C7 119.0(3) . . ?
C6 C1 C7 121.2(3) . . ?
C1 C2 C3 120.5(3) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 C8 120.5(3) . . ?
C4 C3 C8 120.1(3) . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 121.3(3) . . ?
C6 C5 O7 114.4(3) . . ?
C4 C5 O7 124.1(3) . . ?
C5 C6 C1 119.6(3) . . ?
C5 C6 H6 120.2 . . ?
C1 C6 H6 120.2 . . ?
O2 C7 O1 126.0(3) . . ?
O2 C7 C1 118.6(4) . . ?
O1 C7 C1 115.4(4) . . ?
O3 C8 O4 126.4(4) . . ?
O3 C8 C3 116.5(4) . . ?
O4 C8 C3 117.1(3) . . ?
C10 C9 C14 121.3(4) . . ?
C10 C9 O7 121.5(4) . . ?
C14 C9 O7 116.8(4) . . ?
C9 C10 C11 119.1(4) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C12 C11 C10 120.1(4) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 119.2(4) . . ?
C13 C12 C15 118.9(4) . . ?
C11 C12 C15 121.9(4) . . ?
C14 C13 C12 120.9(4) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C9 C14 C13 119.4(4) . . ?
C9 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
O5 C15 O6 124.2(4) . . ?
O5 C15 C12 121.6(4) . . ?
O6 C15 C12 114.2(4) . . ?
N1 C16 C17 123.3(4) . . ?
N1 C16 H16 118.4 . . ?
C17 C16 H16 118.4 . . ?
C18 C17 C16 120.2(4) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 118.5(4) . . ?
C17 C18 H18 120.8 . . ?
C19 C18 H18 120.8 . . ?
C18 C19 C20 117.9(3) . . ?
C18 C19 C27 122.7(4) . . ?
C20 C19 C27 119.3(3) . . ?
N1 C20 C19 123.5(4) . . ?
N1 C20 C21 115.7(3) . . ?
C19 C20 C21 120.8(3) . . ?
N2 C21 C22 123.0(3) . . ?
N2 C21 C20 116.1(3) . . ?
C22 C21 C20 120.9(3) . . ?
C21 C22 C23 118.0(3) . . ?
C21 C22 C26 119.2(3) . . ?
C23 C22 C26 122.8(3) . . ?
C24 C23 C22 119.2(4) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C25 119.0(4) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
N2 C25 C24 123.2(4) . . ?
N2 C25 H25 118.4 . . ?
C24 C25 H25 118.4 . . ?
N4 C26 C27 121.4(3) . . ?
N4 C26 C22 118.6(3) . . ?
C27 C26 C22 120.0(3) . . ?
N3 C27 C26 122.5(3) . . ?
N3 C27 C19 117.9(3) . . ?
C26 C27 C19 119.6(3) . . ?
N3 C28 C33 119.6(4) . . ?
N3 C28 C29 121.3(3) . . ?
C33 C28 C29 119.1(4) . . ?
N4 C29 C30 119.3(4) . . ?
N4 C29 C28 121.2(3) . . ?
C30 C29 C28 119.5(4) . . ?
C31 C30 C29 119.8(4) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 121.0(4) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
C33 C32 C31 120.9(4) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C32 C33 C28 119.7(4) . . ?
C32 C33 H33 120.2 . . ?
C28 C33 H33 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.4(6) . . . . ?
C7 C1 C2 C3 -176.0(4) . . . . ?
C1 C2 C3 C4 1.7(5) . . . . ?
C1 C2 C3 C8 -178.5(4) . . . . ?
C2 C3 C4 C5 -2.9(5) . . . . ?
C8 C3 C4 C5 177.2(3) . . . . ?
C3 C4 C5 C6 1.1(6) . . . . ?
C3 C4 C5 O7 176.8(3) . . . . ?
C9 O7 C5 C6 -172.7(4) . . . . ?
C9 O7 C5 C4 11.3(6) . . . . ?
C4 C5 C6 C1 2.1(6) . . . . ?
O7 C5 C6 C1 -174.1(3) . . . . ?
C2 C1 C6 C5 -3.3(6) . . . . ?
C7 C1 C6 C5 174.1(4) . . . . ?
Co1 O1 C7 O2 -38.1(8) 1_655 . . . ?
Co1 O1 C7 C1 141.3(4) 1_655 . . . ?
C2 C1 C7 O2 -175.6(4) . . . . ?
C6 C1 C7 O2 7.0(6) . . . . ?
C2 C1 C7 O1 5.0(5) . . . . ?
C6 C1 C7 O1 -172.4(4) . . . . ?
Co1 O3 C8 O4 -47.0(8) 3 . . . ?
Co1 O3 C8 C3 133.3(4) 3 . . . ?
Co1 O4 C8 O3 -39.9(6) . . . . ?
Co1 O4 C8 C3 139.7(3) . . . . ?
C2 C3 C8 O3 -148.4(4) . . . . ?
C4 C3 C8 O3 31.4(5) . . . . ?
C2 C3 C8 O4 31.8(5) . . . . ?
C4 C3 C8 O4 -148.3(4) . . . . ?
C5 O7 C9 C10 66.3(5) . . . . ?
C5 O7 C9 C14 -120.6(4) . . . . ?
C14 C9 C10 C11 -1.6(6) . . . . ?
O7 C9 C10 C11 171.2(3) . . . . ?
C9 C10 C11 C12 2.2(6) . . . . ?
C10 C11 C12 C13 -1.3(6) . . . . ?
C10 C11 C12 C15 177.6(4) . . . . ?
C11 C12 C13 C14 -0.3(6) . . . . ?
C15 C12 C13 C14 -179.2(4) . . . . ?
C10 C9 C14 C13 0.0(6) . . . . ?
O7 C9 C14 C13 -173.1(3) . . . . ?
C12 C13 C14 C9 1.0(7) . . . . ?
C13 C12 C15 O5 21.7(6) . . . . ?
C11 C12 C15 O5 -157.2(4) . . . . ?
C13 C12 C15 O6 -157.8(4) . . . . ?
C11 C12 C15 O6 23.3(6) . . . . ?
C20 N1 C16 C17 0.3(6) . . . . ?
Co1 N1 C16 C17 179.5(3) . . . . ?
N1 C16 C17 C18 0.2(7) . . . . ?
C16 C17 C18 C19 -0.4(7) . . . . ?
C17 C18 C19 C20 0.0(6) . . . . ?
C17 C18 C19 C27 179.2(4) . . . . ?
C16 N1 C20 C19 -0.6(5) . . . . ?
Co1 N1 C20 C19 -179.9(3) . . . . ?
C16 N1 C20 C21 178.5(3) . . . . ?
Co1 N1 C20 C21 -0.8(4) . . . . ?
C18 C19 C20 N1 0.5(6) . . . . ?
C27 C19 C20 N1 -178.7(3) . . . . ?
C18 C19 C20 C21 -178.6(3) . . . . ?
C27 C19 C20 C21 2.2(5) . . . . ?
C25 N2 C21 C22 1.8(5) . . . . ?
Co1 N2 C21 C22 -178.7(3) . . . . ?
C25 N2 C21 C20 -177.1(3) . . . . ?
Co1 N2 C21 C20 2.4(4) . . . . ?
N1 C20 C21 N2 -1.0(5) . . . . ?
C19 C20 C21 N2 178.1(3) . . . . ?
N1 C20 C21 C22 180.0(3) . . . . ?
C19 C20 C21 C22 -0.9(5) . . . . ?
N2 C21 C22 C23 -1.9(6) . . . . ?
C20 C21 C22 C23 176.9(3) . . . . ?
N2 C21 C22 C26 179.1(3) . . . . ?
C20 C21 C22 C26 -2.0(5) . . . . ?
C21 C22 C23 C24 0.8(6) . . . . ?
C26 C22 C23 C24 179.8(4) . . . . ?
C22 C23 C24 C25 0.3(6) . . . . ?
C21 N2 C25 C24 -0.7(6) . . . . ?
Co1 N2 C25 C24 179.9(3) . . . . ?
C23 C24 C25 N2 -0.4(6) . . . . ?
C29 N4 C26 C27 0.9(5) . . . . ?
C29 N4 C26 C22 -179.6(3) . . . . ?
C21 C22 C26 N4 -176.0(3) . . . . ?
C23 C22 C26 N4 5.1(6) . . . . ?
C21 C22 C26 C27 3.6(5) . . . . ?
C23 C22 C26 C27 -175.4(4) . . . . ?
C28 N3 C27 C26 1.5(5) . . . . ?
C28 N3 C27 C19 -178.0(3) . . . . ?
N4 C26 C27 N3 -2.1(6) . . . . ?
C22 C26 C27 N3 178.4(3) . . . . ?
N4 C26 C27 C19 177.3(3) . . . . ?
C22 C26 C27 C19 -2.2(5) . . . . ?
C18 C19 C27 N3 -0.4(6) . . . . ?
C20 C19 C27 N3 178.7(3) . . . . ?
C18 C19 C27 C26 -179.8(4) . . . . ?
C20 C19 C27 C26 -0.7(5) . . . . ?
C27 N3 C28 C33 178.8(4) . . . . ?
C27 N3 C28 C29 0.1(5) . . . . ?
C26 N4 C29 C30 -179.0(3) . . . . ?
C26 N4 C29 C28 0.7(5) . . . . ?
N3 C28 C29 N4 -1.2(6) . . . . ?
C33 C28 C29 N4 -180.0(4) . . . . ?
N3 C28 C29 C30 178.5(3) . . . . ?
C33 C28 C29 C30 -0.3(6) . . . . ?
N4 C29 C30 C31 178.9(4) . . . . ?
C28 C29 C30 C31 -0.8(6) . . . . ?
C29 C30 C31 C32 0.8(6) . . . . ?
C30 C31 C32 C33 0.3(6) . . . . ?
C31 C32 C33 C28 -1.4(6) . . . . ?
N3 C28 C33 C32 -177.4(4) . . . . ?
C29 C28 C33 C32 1.3(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
O6 H6A O2 0.89 1.72 2.610(4) 175 4_465
O1W H1A O5 0.94 2.29 3.079(5) 142 .
O1W H1B O2 0.92 2.25 3.143(6) 162 4_465

_refine_diff_density_max         0.336
_refine_diff_density_min         -0.434
_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_3
_database_code_depnum_ccdc_archive 'CCDC 1964454'
loop_
_audit_author_name
_audit_author_address
'Liang Shuang'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-11-08 deposited with the CCDC.	2020-01-06 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         'C72 H46 N12 Ni3 O18, 4(H2 O)'
_chemical_formula_sum            'C72 H54 N12 Ni3 O22'
_chemical_formula_weight         1615.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   31.9886(19)
_cell_length_b                   14.0007(7)
_cell_length_c                   15.8473(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.910(2)
_cell_angle_gamma                90
_cell_volume                     7011.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3327
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      23.13

_exptl_crystal_description       block
_exptl_crystal_colour            light-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_F_000             3320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.885
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 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  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20079
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.591
_diffrn_reflns_theta_max         25.166
_diffrn_reflns_theta_full        25.166
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6267
_reflns_number_gt                4367
_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       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0684P)²+9.6787P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6267
_refine_ls_number_parameters     492
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1340
_refine_ls_wR_factor_gt          0.1180
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.003
_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 0.25309(2) 0.19851(3) 0.63132(3) 0.02619(15) Uani 1 1 d . . . . .
Ni2 Ni 0.0000 -0.09349(5) 0.7500 0.0328(2) Uani 1 2 d S T P . .
O1W O 0.20846(8) 0.13632(18) 0.54023(15) 0.0351(6) Uani 1 1 d . . . . .
H1A H 0.1873 0.1322 0.5669 0.042 Uiso 1 1 d R U . . .
H1B H 0.2042 0.1826 0.5042 0.042 Uiso 1 1 d R U . . .
O2W O -0.02335(8) -0.0889(2) 0.86692(17) 0.0443(7) Uani 1 1 d . . . . .
H2A H -0.0030 -0.0693 0.9027 0.053 Uiso 1 1 d R U . . .
H2B H -0.0435 -0.0487 0.8625 0.053 Uiso 1 1 d R U . . .
O3W O -0.08094(16) 0.0462(6) 0.9154(4) 0.192(3) Uani 1 1 d . . . . .
H3A H -0.0992 0.0917 0.9214 0.230 Uiso 1 1 d R U . . .
H3B H -0.0757 0.0176 0.9644 0.230 Uiso 1 1 d R U . . .
O4W O 0.0095(2) -0.2319(6) 1.0170(5) 0.209(3) Uani 1 1 d . . . . .
H4A H -0.0115 -0.1880 0.9851 0.251 Uiso 1 1 d R U . . .
H4B H 0.0081 -0.2152 1.0758 0.251 Uiso 1 1 d R U . . .
O1 O 0.21312(8) 0.19549(17) 0.72497(16) 0.0316(6) Uani 1 1 d . . . . .
O2 O 0.15973(10) 0.1121(3) 0.65398(19) 0.0638(10) Uani 1 1 d . . . . .
O3 O 0.04494(8) 0.0041(2) 0.79046(17) 0.0446(7) Uani 1 1 d . . . . .
O4 O 0.04364(13) 0.0251(4) 0.9267(2) 0.1184(19) Uani 1 1 d . U . . .
O5 O 0.23565(8) 0.66582(17) 1.09822(15) 0.0307(6) Uani 1 1 d . . . . .
O6 O 0.20415(8) 0.68840(17) 0.96353(15) 0.0309(6) Uani 1 1 d . . . . .
O7 O 0.16862(10) 0.2456(2) 1.01705(16) 0.0465(8) Uani 1 1 d . . . . .
N1 N 0.30507(9) 0.2497(2) 0.71261(18) 0.0307(7) Uani 1 1 d . . . . .
N2 N 0.27733(10) 0.0727(2) 0.68270(19) 0.0310(7) Uani 1 1 d . . . . .
N3 N 0.39868(15) -0.0541(4) 0.8675(3) 0.0830(16) Uani 1 1 d . . . . .
N4 N 0.42832(13) 0.1355(4) 0.8984(3) 0.0830(15) Uani 1 1 d . . . . .
N5 N -0.03706(10) -0.2095(2) 0.6981(2) 0.0391(8) Uani 1 1 d . . . . .
N6 N -0.03682(18) -0.5553(4) 0.6882(4) 0.0981(17) Uani 1 1 d . . . . .
C1 C 0.26080(14) -0.0150(3) 0.6711(3) 0.0419(10) Uani 1 1 d . . . . .
H1 H 0.2351 -0.0225 0.6354 0.050 Uiso 1 1 calc R U . . .
C2 C 0.28070(16) -0.0955(3) 0.7105(3) 0.0499(12) Uani 1 1 d . . . . .
H2 H 0.2680 -0.1552 0.7024 0.060 Uiso 1 1 calc R U . . .
C3 C 0.31870(17) -0.0854(3) 0.7608(3) 0.0546(13) Uani 1 1 d . . . . .
H3 H 0.3326 -0.1389 0.7862 0.066 Uiso 1 1 calc R U . . .
C4 C 0.33728(13) 0.0048(3) 0.7746(3) 0.0437(11) Uani 1 1 d . . . . .
C5 C 0.37694(15) 0.0226(4) 0.8307(3) 0.0565(14) Uani 1 1 d . . . . .
C6 C 0.4342(2) -0.0346(7) 0.9172(5) 0.111(3) Uani 1 1 d . . . . .
H6 H 0.4505 -0.0848 0.9428 0.133 Uiso 1 1 calc R U . . .
C7 C 0.4486(2) 0.0595(8) 0.9335(5) 0.110(3) Uani 1 1 d . . . . .
H7 H 0.4737 0.0688 0.9709 0.132 Uiso 1 1 calc R U . . .
C8 C 0.39189(14) 0.1160(4) 0.8455(3) 0.0557(13) Uani 1 1 d . . . . .
C9 C 0.36789(13) 0.1963(3) 0.8052(2) 0.0422(10) Uani 1 1 d . . . . .
C10 C 0.38038(14) 0.2910(4) 0.8189(3) 0.0542(13) Uani 1 1 d . . . . .
H10 H 0.4056 0.3056 0.8542 0.065 Uiso 1 1 calc R U . . .
C11 C 0.35545(15) 0.3619(4) 0.7803(3) 0.0543(12) Uani 1 1 d . . . . .
H11 H 0.3634 0.4255 0.7892 0.065 Uiso 1 1 calc R U . . .
C12 C 0.31792(13) 0.3388(3) 0.7272(3) 0.0408(10) Uani 1 1 d . . . . .
H12 H 0.3012 0.3880 0.7009 0.049 Uiso 1 1 calc R U . . .
C13 C 0.32983(12) 0.1786(3) 0.7512(2) 0.0317(9) Uani 1 1 d . . . . .
C14 C 0.31473(12) 0.0821(3) 0.7353(2) 0.0331(9) Uani 1 1 d . . . . .
C15 C 0.17796(13) 0.1553(3) 0.7195(2) 0.0363(9) Uani 1 1 d . . . . .
C16 C 0.15570(12) 0.1552(3) 0.7964(2) 0.0340(9) Uani 1 1 d . . . . .
C17 C 0.11765(12) 0.1071(3) 0.7937(3) 0.0384(10) Uani 1 1 d . . . . .
H17 H 0.1056 0.0770 0.7434 0.046 Uiso 1 1 calc R U . . .
C18 C 0.09711(13) 0.1031(3) 0.8650(3) 0.0413(10) Uani 1 1 d . . . . .
C19 C 0.05819(14) 0.0419(4) 0.8602(3) 0.0508(12) Uani 1 1 d . . . . .
C20 C 0.11407(14) 0.1518(3) 0.9388(3) 0.0446(11) Uani 1 1 d . . . . .
H20 H 0.1004 0.1510 0.9865 0.053 Uiso 1 1 calc R U . . .
C21 C 0.15119(13) 0.2011(3) 0.9402(2) 0.0385(10) Uani 1 1 d . . . . .
C22 C 0.17242(12) 0.2032(3) 0.8710(2) 0.0356(9) Uani 1 1 d . . . . .
H22 H 0.1978 0.2366 0.8741 0.043 Uiso 1 1 calc R U . . .
C23 C 0.18008(13) 0.3410(3) 1.0143(2) 0.0337(9) Uani 1 1 d . . . . .
C24 C 0.21429(13) 0.3698(3) 1.0735(2) 0.0368(9) Uani 1 1 d . . . . .
H24 H 0.2293 0.3253 1.1099 0.044 Uiso 1 1 calc R U . . .
C25 C 0.22587(12) 0.4646(3) 1.0781(2) 0.0338(9) Uani 1 1 d . . . . .
H25 H 0.2486 0.4839 1.1183 0.041 Uiso 1 1 calc R U . . .
C26 C 0.20413(11) 0.5320(3) 1.0236(2) 0.0274(8) Uani 1 1 d . . . . .
C27 C 0.21556(11) 0.6360(3) 1.0284(2) 0.0283(8) Uani 1 1 d . . . . .
C28 C 0.17041(11) 0.5010(3) 0.9639(2) 0.0333(9) Uani 1 1 d . . . . .
H28 H 0.1560 0.5448 0.9259 0.040 Uiso 1 1 calc R U . . .
C29 C 0.15783(12) 0.4058(3) 0.9596(2) 0.0367(9) Uani 1 1 d . . . . .
H29 H 0.1347 0.3863 0.9204 0.044 Uiso 1 1 calc R U . . .
C30 C -0.07248(13) -0.2080(4) 0.6419(3) 0.0498(12) Uani 1 1 d . . . . .
H30 H -0.0848 -0.1493 0.6259 0.060 Uiso 1 1 calc R U . . .
C31 C -0.09193(15) -0.2908(4) 0.6061(3) 0.0627(14) Uani 1 1 d . . . . .
H31 H -0.1165 -0.2870 0.5664 0.075 Uiso 1 1 calc R U . . .
C32 C -0.07464(16) -0.3769(4) 0.6297(3) 0.0653(15) Uani 1 1 d . . . . .
H32 H -0.0874 -0.4325 0.6061 0.078 Uiso 1 1 calc R U . . .
C33 C -0.03799(15) -0.3822(3) 0.6888(3) 0.0532(12) Uani 1 1 d . . . . .
C34 C -0.01810(16) -0.4714(4) 0.7198(4) 0.0663(14) Uani 1 1 d . . . . .
C35 C -0.0179(3) -0.6347(5) 0.7195(6) 0.131(3) Uani 1 1 d . . . . .
H35 H -0.0292 -0.6931 0.6995 0.158 Uiso 1 1 calc R U . . .
C36 C -0.01952(12) -0.2959(3) 0.7206(3) 0.0412(10) 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
Ni1 O5 2.026(2) 6_565 ?
Ni1 N2 2.042(3) . ?
Ni1 O1W 2.060(2) . ?
Ni1 N1 2.068(3) . ?
Ni1 O1 2.104(2) . ?
Ni1 O6 2.188(2) 4_546 ?
Ni2 O3 2.015(3) 2_556 ?
Ni2 O3 2.015(3) . ?
Ni2 N5 2.102(3) 2_556 ?
Ni2 N5 2.102(3) . ?
Ni2 O2W 2.103(3) . ?
Ni2 O2W 2.103(3) 2_556 ?
O1W H1A 0.8547 . ?
O1W H1B 0.8608 . ?
O2W H2A 0.8416 . ?
O2W H2B 0.8503 . ?
O3W H3A 0.8790 . ?
O3W H3B 0.8664 . ?
O4W H4A 0.9904 . ?
O4W H4B 0.9688 . ?
O1 C15 1.249(4) . ?
O2 C15 1.263(5) . ?
O3 C19 1.240(5) . ?
O4 C19 1.239(5) . ?
O5 C27 1.261(4) . ?
O5 Ni1 2.026(2) 6_566 ?
O6 C27 1.270(4) . ?
O6 Ni1 2.188(2) 4_556 ?
O7 C23 1.387(4) . ?
O7 C21 1.404(5) . ?
N1 C12 1.322(5) . ?
N1 C13 1.357(5) . ?
N2 C1 1.338(5) . ?
N2 C14 1.355(5) . ?
N3 C6 1.307(9) . ?
N3 C5 1.360(6) . ?
N4 C7 1.324(9) . ?
N4 C8 1.353(6) . ?
N5 C30 1.328(5) . ?
N5 C36 1.358(5) . ?
N6 C35 1.325(8) . ?
N6 C34 1.377(6) . ?
C1 C2 1.394(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.353(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.399(6) . ?
C3 H3 0.9300 . ?
C4 C14 1.393(5) . ?
C4 C5 1.453(6) . ?
C5 C8 1.400(7) . ?
C6 C7 1.407(10) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.453(6) . ?
C9 C10 1.393(6) . ?
C9 C13 1.397(5) . ?
C10 C11 1.358(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.393(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.444(5) . ?
C15 C16 1.504(5) . ?
C16 C17 1.386(5) . ?
C16 C22 1.393(5) . ?
C17 C18 1.394(5) . ?
C17 H17 0.9300 . ?
C18 C20 1.389(5) . ?
C18 C19 1.504(6) . ?
C20 C21 1.371(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.377(5) . ?
C22 H22 0.9300 . ?
C23 C29 1.375(5) . ?
C23 C24 1.386(5) . ?
C24 C25 1.377(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.391(5) . ?
C25 H25 0.9300 . ?
C26 C28 1.390(5) . ?
C26 C27 1.499(5) . ?
C28 C29 1.390(5) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.395(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.354(7) . ?
C31 H31 0.9300 . ?
C32 C33 1.385(7) . ?
C32 H32 0.9300 . ?
C33 C36 1.403(6) . ?
C33 C34 1.453(7) . ?
C34 C34 1.384(10) 2_556 ?
C35 C35 1.377(15) 2_556 ?
C35 H35 0.9300 . ?
C36 C36 1.437(8) 2_556 ?

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
O5 Ni1 N2 169.80(11) 6_565 . ?
O5 Ni1 O1W 94.68(10) 6_565 . ?
N2 Ni1 O1W 95.40(12) . . ?
O5 Ni1 N1 89.94(11) 6_565 . ?
N2 Ni1 N1 80.30(12) . . ?
O1W Ni1 N1 170.60(11) . . ?
O5 Ni1 O1 91.62(10) 6_565 . ?
N2 Ni1 O1 86.34(11) . . ?
O1W Ni1 O1 93.15(10) . . ?
N1 Ni1 O1 94.90(10) . . ?
O5 Ni1 O6 93.39(9) 6_565 4_546 ?
N2 Ni1 O6 88.80(10) . 4_546 ?
O1W Ni1 O6 86.01(9) . 4_546 ?
N1 Ni1 O6 85.55(10) . 4_546 ?
O1 Ni1 O6 174.97(9) . 4_546 ?
O3 Ni2 O3 94.60(17) 2_556 . ?
O3 Ni2 N5 168.51(12) 2_556 2_556 ?
O3 Ni2 N5 93.91(12) . 2_556 ?
O3 Ni2 N5 93.90(12) 2_556 . ?
O3 Ni2 N5 168.51(12) . . ?
N5 Ni2 N5 78.81(18) 2_556 . ?
O3 Ni2 O2W 85.79(11) 2_556 . ?
O3 Ni2 O2W 91.86(11) . . ?
N5 Ni2 O2W 86.23(12) 2_556 . ?
N5 Ni2 O2W 96.47(12) . . ?
O3 Ni2 O2W 91.86(10) 2_556 2_556 ?
O3 Ni2 O2W 85.78(11) . 2_556 ?
N5 Ni2 O2W 96.46(12) 2_556 2_556 ?
N5 Ni2 O2W 86.23(12) . 2_556 ?
O2W Ni2 O2W 176.53(16) . 2_556 ?
Ni1 O1W H1A 101.4 . . ?
Ni1 O1W H1B 99.7 . . ?
H1A O1W H1B 108.8 . . ?
Ni2 O2W H2A 105.1 . . ?
Ni2 O2W H2B 108.4 . . ?
H2A O2W H2B 109.7 . . ?
H3A O3W H3B 106.1 . . ?
H4A O4W H4B 102.2 . . ?
C15 O1 Ni1 126.8(2) . . ?
C19 O3 Ni2 134.6(3) . . ?
C27 O5 Ni1 128.3(2) . 6_566 ?
C27 O6 Ni1 117.5(2) . 4_556 ?
C23 O7 C21 118.1(3) . . ?
C12 N1 C13 118.0(3) . . ?
C12 N1 Ni1 129.4(3) . . ?
C13 N1 Ni1 112.6(2) . . ?
C1 N2 C14 117.8(3) . . ?
C1 N2 Ni1 128.2(3) . . ?
C14 N2 Ni1 114.0(2) . . ?
C6 N3 C5 115.7(6) . . ?
C7 N4 C8 114.7(6) . . ?
C30 N5 C36 117.7(4) . . ?
C30 N5 Ni2 128.4(3) . . ?
C36 N5 Ni2 113.6(3) . . ?
C35 N6 C34 115.6(6) . . ?
N2 C1 C2 122.5(4) . . ?
N2 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 120.5(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C14 C4 C3 117.0(4) . . ?
C14 C4 C5 118.9(4) . . ?
C3 C4 C5 124.0(4) . . ?
N3 C5 C8 121.8(5) . . ?
N3 C5 C4 117.9(5) . . ?
C8 C5 C4 120.4(4) . . ?
N3 C6 C7 122.4(6) . . ?
N3 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
N4 C7 C6 123.4(7) . . ?
N4 C7 H7 118.3 . . ?
C6 C7 H7 118.3 . . ?
N4 C8 C5 122.1(5) . . ?
N4 C8 C9 117.5(5) . . ?
C5 C8 C9 120.4(4) . . ?
C10 C9 C13 117.7(4) . . ?
C10 C9 C8 123.3(4) . . ?
C13 C9 C8 118.9(4) . . ?
C11 C10 C9 119.5(4) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
N1 C12 C11 122.7(4) . . ?
N1 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
N1 C13 C9 122.6(4) . . ?
N1 C13 C14 116.8(3) . . ?
C9 C13 C14 120.6(4) . . ?
N2 C14 C4 123.1(4) . . ?
N2 C14 C13 116.0(3) . . ?
C4 C14 C13 120.9(4) . . ?
O1 C15 O2 124.7(4) . . ?
O1 C15 C16 118.6(3) . . ?
O2 C15 C16 116.7(3) . . ?
C17 C16 C22 118.8(3) . . ?
C17 C16 C15 119.9(3) . . ?
C22 C16 C15 121.3(3) . . ?
C16 C17 C18 121.1(4) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C20 C18 C17 119.4(4) . . ?
C20 C18 C19 122.3(4) . . ?
C17 C18 C19 118.2(4) . . ?
O4 C19 O3 123.8(4) . . ?
O4 C19 C18 118.9(4) . . ?
O3 C19 C18 117.0(4) . . ?
C21 C20 C18 119.1(4) . . ?
C21 C20 H20 120.5 . . ?
C18 C20 H20 120.5 . . ?
C20 C21 C22 122.1(4) . . ?
C20 C21 O7 117.7(3) . . ?
C22 C21 O7 120.2(3) . . ?
C21 C22 C16 119.6(4) . . ?
C21 C22 H22 120.2 . . ?
C16 C22 H22 120.2 . . ?
C29 C23 C24 120.8(4) . . ?
C29 C23 O7 122.8(4) . . ?
C24 C23 O7 116.3(4) . . ?
C25 C24 C23 119.6(4) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 121.2(4) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C28 C26 C25 118.1(3) . . ?
C28 C26 C27 119.7(3) . . ?
C25 C26 C27 122.2(3) . . ?
O5 C27 O6 124.2(3) . . ?
O5 C27 C26 117.0(3) . . ?
O6 C27 C26 118.8(3) . . ?
C26 C28 C29 121.4(4) . . ?
C26 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C23 C29 C28 119.0(3) . . ?
C23 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
N5 C30 C31 122.7(5) . . ?
N5 C30 H30 118.7 . . ?
C31 C30 H30 118.7 . . ?
C32 C31 C30 119.4(5) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C31 C32 C33 120.1(5) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C32 C33 C36 117.5(5) . . ?
C32 C33 C34 123.7(5) . . ?
C36 C33 C34 118.7(4) . . ?
N6 C34 C34 121.5(3) . 2_556 ?
N6 C34 C33 117.9(5) . . ?
C34 C34 C33 120.6(3) 2_556 . ?
N6 C35 C35 123.0(4) . 2_556 ?
N6 C35 H35 118.5 . . ?
C35 C35 H35 118.5 2_556 . ?
N5 C36 C33 122.6(4) . . ?
N5 C36 C36 116.9(2) . 2_556 ?
C33 C36 C36 120.5(3) . 2_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 N2 C1 C2 -0.3(5) . . . . ?
Ni1 N2 C1 C2 -179.8(3) . . . . ?
N2 C1 C2 C3 -1.8(6) . . . . ?
C1 C2 C3 C4 1.6(6) . . . . ?
C2 C3 C4 C14 0.6(6) . . . . ?
C2 C3 C4 C5 177.0(4) . . . . ?
C6 N3 C5 C8 0.0(7) . . . . ?
C6 N3 C5 C4 179.9(5) . . . . ?
C14 C4 C5 N3 -179.1(4) . . . . ?
C3 C4 C5 N3 4.5(6) . . . . ?
C14 C4 C5 C8 0.7(6) . . . . ?
C3 C4 C5 C8 -175.6(4) . . . . ?
C5 N3 C6 C7 1.5(10) . . . . ?
C8 N4 C7 C6 0.7(10) . . . . ?
N3 C6 C7 N4 -2.0(12) . . . . ?
C7 N4 C8 C5 0.8(7) . . . . ?
C7 N4 C8 C9 179.6(5) . . . . ?
N3 C5 C8 N4 -1.2(7) . . . . ?
C4 C5 C8 N4 178.9(4) . . . . ?
N3 C5 C8 C9 180.0(4) . . . . ?
C4 C5 C8 C9 0.1(6) . . . . ?
N4 C8 C9 C10 -0.6(6) . . . . ?
C5 C8 C9 C10 178.3(4) . . . . ?
N4 C8 C9 C13 -179.1(4) . . . . ?
C5 C8 C9 C13 -0.3(6) . . . . ?
C13 C9 C10 C11 0.3(6) . . . . ?
C8 C9 C10 C11 -178.3(4) . . . . ?
C9 C10 C11 C12 -0.4(7) . . . . ?
C13 N1 C12 C11 -0.2(6) . . . . ?
Ni1 N1 C12 C11 -175.7(3) . . . . ?
C10 C11 C12 N1 0.3(7) . . . . ?
C12 N1 C13 C9 0.1(5) . . . . ?
Ni1 N1 C13 C9 176.4(3) . . . . ?
C12 N1 C13 C14 179.0(3) . . . . ?
Ni1 N1 C13 C14 -4.7(4) . . . . ?
C10 C9 C13 N1 -0.2(6) . . . . ?
C8 C9 C13 N1 178.5(3) . . . . ?
C10 C9 C13 C14 -179.0(3) . . . . ?
C8 C9 C13 C14 -0.4(5) . . . . ?
C1 N2 C14 C4 2.7(5) . . . . ?
Ni1 N2 C14 C4 -177.8(3) . . . . ?
C1 N2 C14 C13 -175.4(3) . . . . ?
Ni1 N2 C14 C13 4.1(4) . . . . ?
C3 C4 C14 N2 -2.8(6) . . . . ?
C5 C4 C14 N2 -179.4(3) . . . . ?
C3 C4 C14 C13 175.2(3) . . . . ?
C5 C4 C14 C13 -1.4(5) . . . . ?
N1 C13 C14 N2 0.5(5) . . . . ?
C9 C13 C14 N2 179.4(3) . . . . ?
N1 C13 C14 C4 -177.7(3) . . . . ?
C9 C13 C14 C4 1.3(5) . . . . ?
Ni1 O1 C15 O2 -2.9(6) . . . . ?
Ni1 O1 C15 C16 175.4(2) . . . . ?
O1 C15 C16 C17 -176.8(4) . . . . ?
O2 C15 C16 C17 1.7(6) . . . . ?
O1 C15 C16 C22 3.6(6) . . . . ?
O2 C15 C16 C22 -177.9(4) . . . . ?
C22 C16 C17 C18 -2.6(6) . . . . ?
C15 C16 C17 C18 177.8(4) . . . . ?
C16 C17 C18 C20 3.0(7) . . . . ?
C16 C17 C18 C19 -174.2(4) . . . . ?
Ni2 O3 C19 O4 -1.4(8) . . . . ?
Ni2 O3 C19 C18 171.8(3) . . . . ?
C20 C18 C19 O4 -8.7(8) . . . . ?
C17 C18 C19 O4 168.4(5) . . . . ?
C20 C18 C19 O3 177.7(4) . . . . ?
C17 C18 C19 O3 -5.2(7) . . . . ?
C17 C18 C20 C21 -1.4(7) . . . . ?
C19 C18 C20 C21 175.7(4) . . . . ?
C18 C20 C21 C22 -0.5(7) . . . . ?
C18 C20 C21 O7 -176.9(4) . . . . ?
C23 O7 C21 C20 -129.6(4) . . . . ?
C23 O7 C21 C22 54.0(5) . . . . ?
C20 C21 C22 C16 0.9(6) . . . . ?
O7 C21 C22 C16 177.1(4) . . . . ?
C17 C16 C22 C21 0.7(6) . . . . ?
C15 C16 C22 C21 -179.7(4) . . . . ?
C21 O7 C23 C29 35.1(5) . . . . ?
C21 O7 C23 C24 -148.3(4) . . . . ?
C29 C23 C24 C25 0.6(6) . . . . ?
O7 C23 C24 C25 -176.1(3) . . . . ?
C23 C24 C25 C26 -0.7(6) . . . . ?
C24 C25 C26 C28 -0.4(5) . . . . ?
C24 C25 C26 C27 178.8(3) . . . . ?
Ni1 O5 C27 O6 3.3(5) 6_566 . . . ?
Ni1 O5 C27 C26 -175.7(2) 6_566 . . . ?
Ni1 O6 C27 O5 92.6(4) 4_556 . . . ?
Ni1 O6 C27 C26 -88.4(3) 4_556 . . . ?
C28 C26 C27 O5 157.0(3) . . . . ?
C25 C26 C27 O5 -22.2(5) . . . . ?
C28 C26 C27 O6 -22.0(5) . . . . ?
C25 C26 C27 O6 158.8(3) . . . . ?
C25 C26 C28 C29 1.7(5) . . . . ?
C27 C26 C28 C29 -177.5(3) . . . . ?
C24 C23 C29 C28 0.7(6) . . . . ?
O7 C23 C29 C28 177.1(3) . . . . ?
C26 C28 C29 C23 -1.9(6) . . . . ?
C36 N5 C30 C31 0.1(6) . . . . ?
Ni2 N5 C30 C31 173.6(3) . . . . ?
N5 C30 C31 C32 0.8(7) . . . . ?
C30 C31 C32 C33 0.0(8) . . . . ?
C31 C32 C33 C36 -1.6(7) . . . . ?
C31 C32 C33 C34 177.9(5) . . . . ?
C35 N6 C34 C34 0.0(11) . . . 2_556 ?
C35 N6 C34 C33 -178.9(7) . . . . ?
C32 C33 C34 N6 0.1(8) . . . . ?
C36 C33 C34 N6 179.6(5) . . . . ?
C32 C33 C34 C34 -178.7(6) . . . 2_556 ?
C36 C33 C34 C34 0.7(9) . . . 2_556 ?
C34 N6 C35 C35 0.9(17) . . . 2_556 ?
C30 N5 C36 C33 -1.7(6) . . . . ?
Ni2 N5 C36 C33 -176.2(3) . . . . ?
C30 N5 C36 C36 178.0(4) . . . 2_556 ?
Ni2 N5 C36 C36 3.6(6) . . . 2_556 ?
C32 C33 C36 N5 2.5(7) . . . . ?
C34 C33 C36 N5 -177.0(4) . . . . ?
C32 C33 C36 C36 -177.3(5) . . . 2_556 ?
C34 C33 C36 C36 3.2(8) . . . 2_556 ?

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
O1W H1A O2 0.85 1.77 2.582(4) 158 .
O1W H1B O6 0.86 1.92 2.732(4) 158 6_565
O2W H2A O4 0.84 1.99 2.723(4) 146 .
O2W H2B O3W 0.85 2.05 2.829(7) 151 .
O3W H3A O2 0.88 2.13 2.749(6) 127 2_556
O3W H3B O4 0.87 1.96 2.784(7) 159 5_557
O4W H4A O2W 0.99 2.31 3.162(8) 143 .

_refine_diff_density_max         0.983
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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 1964455'
loop_
_audit_author_name
_audit_author_address
'Liang Shuang'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-11-08 deposited with the CCDC.	2020-01-06 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         'C29 H18 N4 O8 Zn, H2 O'
_chemical_formula_sum            'C29 H20 N4 O9 Zn'
_chemical_formula_weight         633.88

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

_space_group_crystal_system      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                   9.7470(5)
_cell_length_b                   11.5054(6)
_cell_length_c                   12.5424(7)
_cell_angle_alpha                99.091(1)
_cell_angle_beta                 90.462(1)
_cell_angle_gamma                109.098(1)
_cell_volume                     1309.74(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2835
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      26.31

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_F_000             648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.004
_shelx_estimated_absorpt_T_min   0.832
_shelx_estimated_absorpt_T_max   0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 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  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8516
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.648
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5363
_reflns_number_gt                4294
_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       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0372P)²+0.2805P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5363
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0828
_refine_ls_wR_factor_gt          0.0768
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
Zn1 Zn -0.13529(3) 0.18381(3) 0.93048(2) 0.02880(9) Uani 1 1 d . . . . .
O1W O -0.18801(19) 0.05582(16) 1.03351(14) 0.0445(5) Uani 1 1 d . . . . .
H1A H -0.1595 -0.0077 1.0305 0.053 Uiso 1 1 d R U . . .
H1B H -0.2680 0.0424 1.0650 0.053 Uiso 1 1 d R U . . .
O2W O -0.4442(2) 0.00807(19) 1.12502(16) 0.0656(7) Uani 1 1 d . . . . .
H2A H -0.4351 0.0428 1.1913 0.079 Uiso 1 1 d R U . . .
H2B H -0.5145 -0.0603 1.1150 0.079 Uiso 1 1 d R U . . .
O1 O 0.04895(17) 0.30574(16) 1.01123(14) 0.0381(4) Uani 1 1 d . . . . .
O2 O 0.11145(17) 0.14470(16) 0.93839(14) 0.0390(4) Uani 1 1 d . . . . .
O3 O 0.67985(16) 0.22609(15) 0.95498(12) 0.0308(4) Uani 1 1 d . . . . .
O4 O 0.75338(17) 0.29531(17) 1.12828(13) 0.0399(4) Uani 1 1 d . . . . .
O5 O 0.3300(2) 0.66794(19) 1.67783(14) 0.0534(5) Uani 1 1 d . . . . .
H5A H 0.3040 0.6900 1.7490 0.064 Uiso 1 1 d R U . . .
O6 O 0.4091(2) 0.87038(18) 1.66426(14) 0.0521(5) Uani 1 1 d . . . . .
O7 O 0.50526(18) 0.62662(14) 1.19631(12) 0.0344(4) Uani 1 1 d . . . . .
N1 N -0.1899(2) 0.04267(18) 0.78785(15) 0.0297(4) Uani 1 1 d . . . . .
N2 N -0.0821(2) 0.28917(18) 0.79633(15) 0.0314(4) Uani 1 1 d . . . . .
N3 N -0.0563(2) 0.2356(2) 0.40806(18) 0.0506(6) Uani 1 1 d . . . . .
N4 N -0.1668(2) -0.0248(2) 0.39988(17) 0.0478(6) Uani 1 1 d . . . . .
C1 C -0.0306(3) 0.4122(2) 0.8033(2) 0.0407(6) Uani 1 1 d . . . . .
H1 H -0.0180 0.4618 0.8712 0.049 Uiso 1 1 calc R U . . .
C2 C 0.0051(3) 0.4698(3) 0.7138(2) 0.0528(8) Uani 1 1 d . . . . .
H2 H 0.0395 0.5564 0.7217 0.063 Uiso 1 1 calc R U . . .
C3 C -0.0107(3) 0.3983(3) 0.6140(2) 0.0504(7) Uani 1 1 d . . . . .
H3 H 0.0147 0.4360 0.5534 0.061 Uiso 1 1 calc R U . . .
C4 C -0.0651(3) 0.2683(2) 0.60285(19) 0.0356(6) Uani 1 1 d . . . . .
C5 C -0.0886(3) 0.1850(3) 0.49921(19) 0.0377(6) Uani 1 1 d . . . . .
C6 C -0.0821(3) 0.1556(4) 0.3166(2) 0.0579(9) Uani 1 1 d . . . . .
H6 H -0.0638 0.1865 0.2521 0.069 Uiso 1 1 calc R U . . .
C7 C -0.1354(3) 0.0271(3) 0.3123(2) 0.0558(8) Uani 1 1 d . . . . .
H7 H -0.1497 -0.0244 0.2453 0.067 Uiso 1 1 calc R U . . .
C8 C -0.1451(3) 0.0557(3) 0.49470(18) 0.0358(6) Uani 1 1 d . . . . .
C9 C -0.1817(2) 0.0033(2) 0.59346(19) 0.0320(5) Uani 1 1 d . . . . .
C10 C -0.2360(3) -0.1251(2) 0.5939(2) 0.0420(6) Uani 1 1 d . . . . .
H10 H -0.2516 -0.1817 0.5297 0.050 Uiso 1 1 calc R U . . .
C11 C -0.2657(3) -0.1659(2) 0.6904(2) 0.0456(7) Uani 1 1 d . . . . .
H11 H -0.3017 -0.2510 0.6925 0.055 Uiso 1 1 calc R U . . .
C12 C -0.2417(3) -0.0797(2) 0.7854(2) 0.0395(6) Uani 1 1 d . . . . .
H12 H -0.2630 -0.1092 0.8503 0.047 Uiso 1 1 calc R U . . .
C13 C -0.1595(2) 0.0841(2) 0.69270(18) 0.0280(5) Uani 1 1 d . . . . .
C14 C -0.1005(2) 0.2180(2) 0.69711(18) 0.0288(5) Uani 1 1 d . . . . .
C15 C 0.1425(2) 0.2516(2) 0.99269(17) 0.0294(5) Uani 1 1 d . . . . .
C16 C 0.2955(2) 0.3214(2) 1.03979(16) 0.0242(5) Uani 1 1 d . . . . .
C17 C 0.4065(2) 0.2710(2) 1.01799(16) 0.0236(5) Uani 1 1 d . . . . .
H17 H 0.3869 0.1948 0.9721 0.028 Uiso 1 1 calc R U . . .
C18 C 0.5461(2) 0.3341(2) 1.06454(16) 0.0237(5) Uani 1 1 d . . . . .
C19 C 0.6683(2) 0.2810(2) 1.04881(18) 0.0265(5) Uani 1 1 d . . . . .
C20 C 0.5761(2) 0.4513(2) 1.12911(17) 0.0274(5) Uani 1 1 d . . . . .
H20 H 0.6690 0.4940 1.1614 0.033 Uiso 1 1 calc R U . . .
C21 C 0.4679(2) 0.5027(2) 1.14456(17) 0.0270(5) Uani 1 1 d . . . . .
C22 C 0.3271(2) 0.4388(2) 1.10240(17) 0.0283(5) Uani 1 1 d . . . . .
H22 H 0.2543 0.4741 1.1158 0.034 Uiso 1 1 calc R U . . .
C23 C 0.4645(2) 0.6508(2) 1.29952(17) 0.0279(5) Uani 1 1 d . . . . .
C24 C 0.4781(3) 0.7740(2) 1.33729(19) 0.0342(6) Uani 1 1 d . . . . .
H24 H 0.5068 0.8334 1.2922 0.041 Uiso 1 1 calc R U . . .
C25 C 0.4486(3) 0.8071(2) 1.4424(2) 0.0370(6) Uani 1 1 d . . . . .
H25 H 0.4591 0.8900 1.4686 0.044 Uiso 1 1 calc R U . . .
C26 C 0.4038(2) 0.7199(2) 1.50986(18) 0.0334(6) Uani 1 1 d . . . . .
C27 C 0.3814(3) 0.7612(3) 1.6251(2) 0.0385(6) Uani 1 1 d . . . . .
C28 C 0.3879(3) 0.5972(2) 1.4703(2) 0.0440(7) Uani 1 1 d . . . . .
H28 H 0.3563 0.5374 1.5148 0.053 Uiso 1 1 calc R U . . .
C29 C 0.4185(3) 0.5619(2) 1.3651(2) 0.0452(7) Uani 1 1 d . . . . .
H29 H 0.4081 0.4791 1.3389 0.054 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
Zn1 O1 2.0228(16) . ?
Zn1 O3 2.0281(15) 1_455 ?
Zn1 O1W 2.0542(17) . ?
Zn1 N1 2.1498(19) . ?
Zn1 N2 2.1946(19) . ?
Zn1 O2 2.5912(17) . ?
O1W H1A 0.8584 . ?
O1W H1B 0.8560 . ?
O2W H2A 0.8546 . ?
O2W H2B 0.8474 . ?
O1 C15 1.266(3) . ?
O2 C15 1.247(3) . ?
O3 C19 1.269(3) . ?
O4 C19 1.246(3) . ?
O5 C27 1.310(3) . ?
O5 H5A 0.9487 . ?
O6 C27 1.214(3) . ?
O7 C23 1.371(2) . ?
O7 C21 1.396(3) . ?
N1 C12 1.326(3) . ?
N1 C13 1.354(3) . ?
N2 C1 1.327(3) . ?
N2 C14 1.353(3) . ?
N3 C6 1.317(4) . ?
N3 C5 1.357(3) . ?
N4 C7 1.323(4) . ?
N4 C8 1.355(3) . ?
C1 C2 1.381(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.397(4) . ?
C3 H3 0.9300 . ?
C4 C14 1.394(3) . ?
C4 C5 1.455(3) . ?
C5 C8 1.399(4) . ?
C6 C7 1.389(5) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.458(3) . ?
C9 C10 1.398(4) . ?
C9 C13 1.399(3) . ?
C10 C11 1.366(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.449(3) . ?
C15 C16 1.506(3) . ?
C16 C22 1.388(3) . ?
C16 C17 1.396(3) . ?
C17 C18 1.388(3) . ?
C17 H17 0.9300 . ?
C18 C20 1.397(3) . ?
C18 C19 1.508(3) . ?
C20 C21 1.370(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(3) . ?
C22 H22 0.9300 . ?
C23 C29 1.377(3) . ?
C23 C24 1.383(3) . ?
C24 C25 1.373(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(3) . ?
C25 H25 0.9300 . ?
C26 C28 1.378(3) . ?
C26 C27 1.489(3) . ?
C28 C29 1.382(3) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O3 116.59(6) . 1_455 ?
O1 Zn1 O1W 98.91(7) . . ?
O3 Zn1 O1W 92.58(7) 1_455 . ?
O1 Zn1 N1 136.63(7) . . ?
O3 Zn1 N1 104.09(7) 1_455 . ?
O1W Zn1 N1 93.41(7) . . ?
O1 Zn1 N2 87.73(7) . . ?
O3 Zn1 N2 92.38(7) 1_455 . ?
O1W Zn1 N2 168.89(7) . . ?
N1 Zn1 N2 75.73(7) . . ?
O1 Zn1 O2 55.39(6) . . ?
O3 Zn1 O2 169.08(6) 1_455 . ?
O1W Zn1 O2 82.13(6) . . ?
N1 Zn1 O2 85.83(6) . . ?
N2 Zn1 O2 94.54(6) . . ?
Zn1 O1W H1A 125.9 . . ?
Zn1 O1W H1B 119.7 . . ?
H1A O1W H1B 109.6 . . ?
H2A O2W H2B 110.4 . . ?
C15 O1 Zn1 104.07(15) . . ?
C15 O2 Zn1 78.13(13) . . ?
C19 O3 Zn1 116.74(14) . 1_655 ?
C27 O5 H5A 115.2 . . ?
C23 O7 C21 118.83(17) . . ?
C12 N1 C13 117.8(2) . . ?
C12 N1 Zn1 126.19(17) . . ?
C13 N1 Zn1 115.90(15) . . ?
C1 N2 C14 118.1(2) . . ?
C1 N2 Zn1 127.13(17) . . ?
C14 N2 Zn1 114.72(15) . . ?
C6 N3 C5 115.8(3) . . ?
C7 N4 C8 115.6(3) . . ?
N2 C1 C2 122.7(2) . . ?
N2 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C14 C4 C3 117.0(2) . . ?
C14 C4 C5 119.4(2) . . ?
C3 C4 C5 123.6(2) . . ?
N3 C5 C8 121.3(2) . . ?
N3 C5 C4 118.6(2) . . ?
C8 C5 C4 120.1(2) . . ?
N3 C6 C7 122.9(3) . . ?
N3 C6 H6 118.5 . . ?
C7 C6 H6 118.5 . . ?
N4 C7 C6 122.6(3) . . ?
N4 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
N4 C8 C5 121.8(2) . . ?
N4 C8 C9 117.9(2) . . ?
C5 C8 C9 120.4(2) . . ?
C10 C9 C13 118.0(2) . . ?
C10 C9 C8 122.8(2) . . ?
C13 C9 C8 119.2(2) . . ?
C11 C10 C9 118.9(2) . . ?
C11 C10 H10 120.6 . . ?
C9 C10 H10 120.6 . . ?
C10 C11 C12 119.6(2) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
N1 C12 C11 123.1(2) . . ?
N1 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
N1 C13 C9 122.6(2) . . ?
N1 C13 C14 117.03(19) . . ?
C9 C13 C14 120.3(2) . . ?
N2 C14 C4 122.9(2) . . ?
N2 C14 C13 116.5(2) . . ?
C4 C14 C13 120.6(2) . . ?
O2 C15 O1 122.4(2) . . ?
O2 C15 C16 120.4(2) . . ?
O1 C15 C16 117.2(2) . . ?
C22 C16 C17 119.8(2) . . ?
C22 C16 C15 119.6(2) . . ?
C17 C16 C15 120.65(19) . . ?
C18 C17 C16 120.22(19) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C20 119.5(2) . . ?
C17 C18 C19 122.55(19) . . ?
C20 C18 C19 118.00(19) . . ?
O4 C19 O3 123.9(2) . . ?
O4 C19 C18 118.10(19) . . ?
O3 C19 C18 118.0(2) . . ?
C21 C20 C18 119.6(2) . . ?
C21 C20 H20 120.2 . . ?
C18 C20 H20 120.2 . . ?
C20 C21 C22 121.6(2) . . ?
C20 C21 O7 118.3(2) . . ?
C22 C21 O7 119.9(2) . . ?
C21 C22 C16 119.2(2) . . ?
C21 C22 H22 120.4 . . ?
C16 C22 H22 120.4 . . ?
O7 C23 C29 123.7(2) . . ?
O7 C23 C24 115.5(2) . . ?
C29 C23 C24 120.7(2) . . ?
C25 C24 C23 118.9(2) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C24 C25 C26 121.3(2) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C28 C26 C25 119.1(2) . . ?
C28 C26 C27 121.4(2) . . ?
C25 C26 C27 119.4(2) . . ?
O6 C27 O5 124.6(2) . . ?
O6 C27 C26 122.4(3) . . ?
O5 C27 C26 112.9(2) . . ?
C26 C28 C29 120.7(2) . . ?
C26 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C23 C29 C28 119.3(2) . . ?
C23 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 N2 C1 C2 -0.2(4) . . . . ?
Zn1 N2 C1 C2 177.3(2) . . . . ?
N2 C1 C2 C3 -1.0(4) . . . . ?
C1 C2 C3 C4 1.2(5) . . . . ?
C2 C3 C4 C14 -0.2(4) . . . . ?
C2 C3 C4 C5 178.5(3) . . . . ?
C6 N3 C5 C8 0.3(4) . . . . ?
C6 N3 C5 C4 -178.9(2) . . . . ?
C14 C4 C5 N3 178.7(2) . . . . ?
C3 C4 C5 N3 -0.1(4) . . . . ?
C14 C4 C5 C8 -0.5(4) . . . . ?
C3 C4 C5 C8 -179.3(2) . . . . ?
C5 N3 C6 C7 -1.6(4) . . . . ?
C8 N4 C7 C6 0.7(4) . . . . ?
N3 C6 C7 N4 1.2(5) . . . . ?
C7 N4 C8 C5 -2.1(4) . . . . ?
C7 N4 C8 C9 178.4(2) . . . . ?
N3 C5 C8 N4 1.7(4) . . . . ?
C4 C5 C8 N4 -179.2(2) . . . . ?
N3 C5 C8 C9 -178.8(2) . . . . ?
C4 C5 C8 C9 0.4(4) . . . . ?
N4 C8 C9 C10 0.7(3) . . . . ?
C5 C8 C9 C10 -178.8(2) . . . . ?
N4 C8 C9 C13 179.6(2) . . . . ?
C5 C8 C9 C13 0.0(3) . . . . ?
C13 C9 C10 C11 0.4(4) . . . . ?
C8 C9 C10 C11 179.2(2) . . . . ?
C9 C10 C11 C12 0.1(4) . . . . ?
C13 N1 C12 C11 0.0(4) . . . . ?
Zn1 N1 C12 C11 -175.63(19) . . . . ?
C10 C11 C12 N1 -0.3(4) . . . . ?
C12 N1 C13 C9 0.5(3) . . . . ?
Zn1 N1 C13 C9 176.59(17) . . . . ?
C12 N1 C13 C14 -178.9(2) . . . . ?
Zn1 N1 C13 C14 -2.8(3) . . . . ?
C10 C9 C13 N1 -0.7(3) . . . . ?
C8 C9 C13 N1 -179.6(2) . . . . ?
C10 C9 C13 C14 178.7(2) . . . . ?
C8 C9 C13 C14 -0.2(3) . . . . ?
C1 N2 C14 C4 1.3(3) . . . . ?
Zn1 N2 C14 C4 -176.54(18) . . . . ?
C1 N2 C14 C13 -178.9(2) . . . . ?
Zn1 N2 C14 C13 3.2(3) . . . . ?
C3 C4 C14 N2 -1.1(4) . . . . ?
C5 C4 C14 N2 -179.9(2) . . . . ?
C3 C4 C14 C13 179.1(2) . . . . ?
C5 C4 C14 C13 0.3(3) . . . . ?
N1 C13 C14 N2 -0.4(3) . . . . ?
C9 C13 C14 N2 -179.8(2) . . . . ?
N1 C13 C14 C4 179.4(2) . . . . ?
C9 C13 C14 C4 0.0(3) . . . . ?
Zn1 O2 C15 O1 1.7(2) . . . . ?
Zn1 O2 C15 C16 -178.7(2) . . . . ?
Zn1 O1 C15 O2 -2.2(3) . . . . ?
Zn1 O1 C15 C16 178.14(15) . . . . ?
O2 C15 C16 C22 -178.3(2) . . . . ?
O1 C15 C16 C22 1.4(3) . . . . ?
O2 C15 C16 C17 3.9(3) . . . . ?
O1 C15 C16 C17 -176.4(2) . . . . ?
C22 C16 C17 C18 4.3(3) . . . . ?
C15 C16 C17 C18 -177.92(19) . . . . ?
C16 C17 C18 C20 -3.1(3) . . . . ?
C16 C17 C18 C19 176.60(19) . . . . ?
Zn1 O3 C19 O4 -9.5(3) 1_655 . . . ?
Zn1 O3 C19 C18 169.29(14) 1_655 . . . ?
C17 C18 C19 O4 -139.4(2) . . . . ?
C20 C18 C19 O4 40.3(3) . . . . ?
C17 C18 C19 O3 41.7(3) . . . . ?
C20 C18 C19 O3 -138.6(2) . . . . ?
C17 C18 C20 C21 -0.7(3) . . . . ?
C19 C18 C20 C21 179.6(2) . . . . ?
C18 C20 C21 C22 3.4(3) . . . . ?
C18 C20 C21 O7 -171.02(19) . . . . ?
C23 O7 C21 C20 -108.6(2) . . . . ?
C23 O7 C21 C22 76.9(3) . . . . ?
C20 C21 C22 C16 -2.2(3) . . . . ?
O7 C21 C22 C16 172.14(19) . . . . ?
C17 C16 C22 C21 -1.7(3) . . . . ?
C15 C16 C22 C21 -179.5(2) . . . . ?
C21 O7 C23 C29 15.5(3) . . . . ?
C21 O7 C23 C24 -167.2(2) . . . . ?
O7 C23 C24 C25 -175.7(2) . . . . ?
C29 C23 C24 C25 1.7(4) . . . . ?
C23 C24 C25 C26 -1.0(4) . . . . ?
C24 C25 C26 C28 -0.3(4) . . . . ?
C24 C25 C26 C27 176.5(2) . . . . ?
C28 C26 C27 O6 172.3(3) . . . . ?
C25 C26 C27 O6 -4.4(4) . . . . ?
C28 C26 C27 O5 -7.4(4) . . . . ?
C25 C26 C27 O5 175.9(2) . . . . ?
C25 C26 C28 C29 1.0(4) . . . . ?
C27 C26 C28 C29 -175.7(3) . . . . ?
O7 C23 C29 C28 176.2(2) . . . . ?
C24 C23 C29 C28 -1.0(4) . . . . ?
C26 C28 C29 C23 -0.4(4) . . . . ?

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
O1W H1A O2 0.86 1.88 2.717(3) 165 2_557
O1W H1B O2W 0.86 1.83 2.684(2) 177 .
O2W H2A O6 0.85 1.90 2.750(2) 176 2_568
O2W H2B O3 0.85 2.11 2.932(2) 164 2_557
O5 H5A O4 0.95 1.64 2.585(2) 171 2_668

_refine_diff_density_max         0.337
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.055

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1964452'
loop_
_audit_author_name
_audit_author_address
'Liang Shuang'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-11-08 deposited with the CCDC.	2020-01-06 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         'C29 H20 Cu N4 O9'
_chemical_formula_sum            'C29 H20 Cu N4 O9'
_chemical_formula_weight         632.04

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                   9.8670(5)
_cell_length_b                   13.5792(6)
_cell_length_c                   19.1123(9)
_cell_angle_alpha                90
_cell_angle_beta                 94.4950(10)
_cell_angle_gamma                90
_cell_volume                     2552.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5373
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      27.95

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_F_000             1292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.924
_shelx_estimated_absorpt_T_min   0.816
_shelx_estimated_absorpt_T_max   0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 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  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16146
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.842
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5210
_reflns_number_gt                4200
_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       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0491P)²+0.7826P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5210
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0878
_refine_ls_wR_factor_gt          0.0819
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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 0.89263(3) 0.05105(2) 0.64142(2) 0.03079(9) Uani 1 1 d . . . . .
O1W O 1.02947(14) -0.05130(10) 0.62213(8) 0.0361(3) Uani 1 1 d . . . . .
H1A H 1.1085 -0.0330 0.6380 0.043 Uiso 1 1 d R U . . .
H1B H 1.0037 -0.1006 0.6452 0.043 Uiso 1 1 d R U . . .
O2W O 0.74707(14) 0.00042(11) 0.55915(8) 0.0398(4) Uani 1 1 d . . . . .
H2A H 0.7233 0.0488 0.5330 0.048 Uiso 1 1 d R U . . .
H2B H 0.6778 -0.0289 0.5731 0.048 Uiso 1 1 d R U . . .
O1 O 0.80952(15) -0.02589(10) 0.71255(8) 0.0369(3) Uani 1 1 d . . . . .
O2 O 0.89421(16) -0.17514(10) 0.69535(9) 0.0447(4) Uani 1 1 d . . . . .
O3 O 0.72870(16) -0.45536(10) 0.83798(9) 0.0423(4) Uani 1 1 d . . . . .
O4 O 0.54870(18) -0.42889(11) 0.89804(11) 0.0604(6) Uani 1 1 d . . . . .
H4A H 0.5409 -0.4992 0.9036 0.072 Uiso 1 1 d R U . . .
O5 O 0.50137(17) 0.39323(11) 0.91034(10) 0.0531(4) Uani 1 1 d . . . . .
O6 O 0.6825(2) 0.34793(13) 0.97934(13) 0.0745(6) Uani 1 1 d . . . . .
O7 O 0.45553(15) -0.07140(10) 0.88412(9) 0.0422(4) Uani 1 1 d . . . . .
N1 N 0.82099(18) 0.17588(12) 0.68289(9) 0.0330(4) Uani 1 1 d . . . . .
N2 N 0.98873(17) 0.14966(12) 0.58400(9) 0.0302(4) Uani 1 1 d . . . . .
N3 N 1.08498(18) 0.49749(13) 0.57832(10) 0.0390(4) Uani 1 1 d . . . . .
N4 N 0.90655(18) 0.52526(13) 0.68441(11) 0.0403(4) Uani 1 1 d . . . . .
C1 C 1.0710(2) 0.13283(15) 0.53364(11) 0.0354(5) Uani 1 1 d . . . . .
H1 H 1.0840 0.0683 0.5194 0.042 Uiso 1 1 calc R U . . .
C2 C 1.1386(2) 0.20823(16) 0.50123(12) 0.0409(5) Uani 1 1 d . . . . .
H2 H 1.1943 0.1938 0.4655 0.049 Uiso 1 1 calc R U . . .
C3 C 1.1226(2) 0.30367(15) 0.52230(11) 0.0363(5) Uani 1 1 d . . . . .
H3 H 1.1686 0.3545 0.5017 0.044 Uiso 1 1 calc R U . . .
C4 C 1.0357(2) 0.32368(14) 0.57543(11) 0.0299(4) Uani 1 1 d . . . . .
C5 C 1.0144(2) 0.42174(14) 0.60335(11) 0.0308(4) Uani 1 1 d . . . . .
C6 C 1.0656(2) 0.58432(16) 0.60704(14) 0.0443(6) Uani 1 1 d . . . . .
H6 H 1.1130 0.6384 0.5918 0.053 Uiso 1 1 calc R U . . .
C7 C 0.9767(2) 0.59805(16) 0.65935(14) 0.0459(6) Uani 1 1 d . . . . .
H7 H 0.9665 0.6610 0.6773 0.055 Uiso 1 1 calc R U . . .
C8 C 0.9251(2) 0.43564(14) 0.65642(11) 0.0321(5) Uani 1 1 d . . . . .
C9 C 0.8529(2) 0.35229(14) 0.68360(11) 0.0305(4) Uani 1 1 d . . . . .
C10 C 0.7608(2) 0.36063(16) 0.73578(12) 0.0376(5) Uani 1 1 d . . . . .
H10 H 0.7405 0.4218 0.7541 0.045 Uiso 1 1 calc R U . . .
C11 C 0.7016(2) 0.27688(17) 0.75911(12) 0.0429(5) Uani 1 1 d . . . . .
H11 H 0.6394 0.2810 0.7931 0.052 Uiso 1 1 calc R U . . .
C12 C 0.7342(2) 0.18588(16) 0.73215(12) 0.0404(5) Uani 1 1 d . . . . .
H12 H 0.6938 0.1298 0.7492 0.048 Uiso 1 1 calc R U . . .
C13 C 0.8781(2) 0.25875(14) 0.65840(10) 0.0289(4) Uani 1 1 d . . . . .
C14 C 0.96985(19) 0.24430(14) 0.60390(10) 0.0280(4) Uani 1 1 d . . . . .
C15 C 0.8174(2) -0.11807(14) 0.72361(10) 0.0287(4) Uani 1 1 d . . . . .
C16 C 0.72571(19) -0.15754(14) 0.77652(10) 0.0276(4) Uani 1 1 d . . . . .
C17 C 0.72700(19) -0.25722(13) 0.79379(10) 0.0274(4) Uani 1 1 d . . . . .
H17 H 0.7860 -0.2999 0.7733 0.033 Uiso 1 1 calc R U . . .
C18 C 0.63983(19) -0.29277(13) 0.84173(10) 0.0267(4) Uani 1 1 d . . . . .
C19 C 0.6425(2) -0.40130(14) 0.85912(11) 0.0308(4) Uani 1 1 d . . . . .
C20 C 0.5514(2) -0.22977(14) 0.87288(11) 0.0306(4) Uani 1 1 d . . . . .
H20 H 0.4931 -0.2537 0.9048 0.037 Uiso 1 1 calc R U . . .
C21 C 0.5513(2) -0.13055(14) 0.85560(11) 0.0302(4) Uani 1 1 d . . . . .
C22 C 0.6368(2) -0.09451(14) 0.80768(11) 0.0315(4) Uani 1 1 d . . . . .
H22 H 0.6349 -0.0279 0.7962 0.038 Uiso 1 1 calc R U . . .
C23 C 0.4898(2) 0.02697(14) 0.89689(12) 0.0326(5) Uani 1 1 d . . . . .
C24 C 0.5975(2) 0.05135(15) 0.94380(12) 0.0380(5) Uani 1 1 d . . . . .
H24 H 0.6519 0.0023 0.9652 0.046 Uiso 1 1 calc R U . . .
C25 C 0.6243(2) 0.14957(15) 0.95883(12) 0.0361(5) Uani 1 1 d . . . . .
H25 H 0.6967 0.1663 0.9907 0.043 Uiso 1 1 calc R U . . .
C26 C 0.5439(2) 0.22331(14) 0.92671(11) 0.0302(4) Uani 1 1 d . . . . .
C27 C 0.5796(2) 0.32962(15) 0.94076(13) 0.0396(5) Uani 1 1 d . . . . .
C28 C 0.4354(2) 0.19669(15) 0.88062(12) 0.0375(5) Uani 1 1 d . . . . .
H28 H 0.3797 0.2453 0.8596 0.045 Uiso 1 1 calc R U . . .
C29 C 0.4081(2) 0.09856(16) 0.86515(12) 0.0390(5) Uani 1 1 d . . . . .
H29 H 0.3353 0.0814 0.8336 0.047 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 O1 1.9460(14) . ?
Cu1 O1W 1.9922(14) . ?
Cu1 N2 2.0148(16) . ?
Cu1 N1 2.0221(17) . ?
Cu1 O2W 2.1572(15) . ?
O1W H1A 0.8511 . ?
O1W H1B 0.8511 . ?
O2W H2A 0.8483 . ?
O2W H2B 0.8522 . ?
O1 C15 1.271(2) . ?
O2 C15 1.237(2) . ?
O3 C19 1.216(2) . ?
O4 C19 1.288(2) . ?
O4 H4A 0.9639 . ?
O5 C27 1.269(3) . ?
O6 C27 1.233(3) . ?
O7 C21 1.384(2) . ?
O7 C23 1.395(2) . ?
N1 C12 1.329(3) . ?
N1 C13 1.358(3) . ?
N2 C1 1.326(3) . ?
N2 C14 1.357(2) . ?
N3 C6 1.321(3) . ?
N3 C5 1.350(3) . ?
N4 C7 1.318(3) . ?
N4 C8 1.348(3) . ?
C1 C2 1.394(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.370(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.406(3) . ?
C3 H3 0.9300 . ?
C4 C14 1.391(3) . ?
C4 C5 1.456(3) . ?
C5 C8 1.408(3) . ?
C6 C7 1.393(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.455(3) . ?
C9 C13 1.388(3) . ?
C9 C10 1.405(3) . ?
C10 C11 1.369(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.446(3) . ?
C15 C16 1.507(3) . ?
C16 C22 1.392(3) . ?
C16 C17 1.393(3) . ?
C17 C18 1.391(3) . ?
C17 H17 0.9300 . ?
C18 C20 1.389(3) . ?
C18 C19 1.511(3) . ?
C20 C21 1.387(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(3) . ?
C22 H22 0.9300 . ?
C23 C29 1.373(3) . ?
C23 C24 1.376(3) . ?
C24 C25 1.385(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.390(3) . ?
C25 H25 0.9300 . ?
C26 C28 1.380(3) . ?
C26 C27 1.505(3) . ?
C28 C29 1.387(3) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1W 94.79(6) . . ?
O1 Cu1 N2 168.34(6) . . ?
O1W Cu1 N2 90.47(6) . . ?
O1 Cu1 N1 89.82(6) . . ?
O1W Cu1 N1 156.95(7) . . ?
N2 Cu1 N1 81.39(7) . . ?
O1 Cu1 O2W 92.59(6) . . ?
O1W Cu1 O2W 93.72(6) . . ?
N2 Cu1 O2W 97.45(6) . . ?
N1 Cu1 O2W 108.64(6) . . ?
Cu1 O1W H1A 110.2 . . ?
Cu1 O1W H1B 102.7 . . ?
H1A O1W H1B 110.3 . . ?
Cu1 O2W H2A 108.7 . . ?
Cu1 O2W H2B 115.1 . . ?
H2A O2W H2B 110.9 . . ?
C15 O1 Cu1 128.42(13) . . ?
C19 O4 H4A 114.8 . . ?
C21 O7 C23 117.44(15) . . ?
C12 N1 C13 117.87(18) . . ?
C12 N1 Cu1 128.91(14) . . ?
C13 N1 Cu1 113.10(13) . . ?
C1 N2 C14 118.14(17) . . ?
C1 N2 Cu1 128.42(14) . . ?
C14 N2 Cu1 113.32(13) . . ?
C6 N3 C5 115.9(2) . . ?
C7 N4 C8 116.2(2) . . ?
N2 C1 C2 122.51(19) . . ?
N2 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 119.6(2) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 119.07(19) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C14 C4 C3 117.56(18) . . ?
C14 C4 C5 118.69(18) . . ?
C3 C4 C5 123.72(18) . . ?
N3 C5 C8 121.49(19) . . ?
N3 C5 C4 118.27(19) . . ?
C8 C5 C4 120.21(18) . . ?
N3 C6 C7 122.5(2) . . ?
N3 C6 H6 118.7 . . ?
C7 C6 H6 118.7 . . ?
N4 C7 C6 122.6(2) . . ?
N4 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
N4 C8 C5 121.29(19) . . ?
N4 C8 C9 118.37(19) . . ?
C5 C8 C9 120.32(18) . . ?
C13 C9 C10 117.61(19) . . ?
C13 C9 C8 118.81(18) . . ?
C10 C9 C8 123.55(19) . . ?
C11 C10 C9 118.7(2) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
N1 C12 C11 122.4(2) . . ?
N1 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
N1 C13 C9 123.25(18) . . ?
N1 C13 C14 115.84(17) . . ?
C9 C13 C14 120.91(18) . . ?
N2 C14 C4 123.05(18) . . ?
N2 C14 C13 115.97(17) . . ?
C4 C14 C13 120.97(18) . . ?
O2 C15 O1 125.14(18) . . ?
O2 C15 C16 119.39(17) . . ?
O1 C15 C16 115.46(17) . . ?
C22 C16 C17 119.36(18) . . ?
C22 C16 C15 119.99(17) . . ?
C17 C16 C15 120.65(17) . . ?
C18 C17 C16 119.90(18) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C20 C18 C17 120.67(18) . . ?
C20 C18 C19 120.49(18) . . ?
C17 C18 C19 118.84(17) . . ?
O3 C19 O4 124.69(19) . . ?
O3 C19 C18 121.09(19) . . ?
O4 C19 C18 114.21(17) . . ?
C21 C20 C18 119.00(18) . . ?
C21 C20 H20 120.5 . . ?
C18 C20 H20 120.5 . . ?
C22 C21 O7 121.76(17) . . ?
C22 C21 C20 120.84(18) . . ?
O7 C21 C20 117.21(17) . . ?
C21 C22 C16 120.22(18) . . ?
C21 C22 H22 119.9 . . ?
C16 C22 H22 119.9 . . ?
C29 C23 C24 120.94(19) . . ?
C29 C23 O7 118.3(2) . . ?
C24 C23 O7 120.57(18) . . ?
C23 C24 C25 119.46(19) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C24 C25 C26 120.6(2) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C28 C26 C25 118.72(19) . . ?
C28 C26 C27 121.59(19) . . ?
C25 C26 C27 119.66(19) . . ?
O6 C27 O5 125.5(2) . . ?
O6 C27 C26 118.0(2) . . ?
O5 C27 C26 116.5(2) . . ?
C26 C28 C29 121.03(19) . . ?
C26 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C23 C29 C28 119.3(2) . . ?
C23 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 N2 C1 C2 0.5(3) . . . . ?
Cu1 N2 C1 C2 -175.40(16) . . . . ?
N2 C1 C2 C3 1.1(3) . . . . ?
C1 C2 C3 C4 -1.3(3) . . . . ?
C2 C3 C4 C14 -0.1(3) . . . . ?
C2 C3 C4 C5 178.0(2) . . . . ?
C6 N3 C5 C8 0.5(3) . . . . ?
C6 N3 C5 C4 -177.75(19) . . . . ?
C14 C4 C5 N3 176.12(18) . . . . ?
C3 C4 C5 N3 -2.0(3) . . . . ?
C14 C4 C5 C8 -2.2(3) . . . . ?
C3 C4 C5 C8 179.73(19) . . . . ?
C5 N3 C6 C7 -0.8(3) . . . . ?
C8 N4 C7 C6 -0.1(3) . . . . ?
N3 C6 C7 N4 0.7(4) . . . . ?
C7 N4 C8 C5 -0.1(3) . . . . ?
C7 N4 C8 C9 178.34(19) . . . . ?
N3 C5 C8 N4 -0.1(3) . . . . ?
C4 C5 C8 N4 178.18(19) . . . . ?
N3 C5 C8 C9 -178.50(19) . . . . ?
C4 C5 C8 C9 -0.3(3) . . . . ?
N4 C8 C9 C13 -175.81(19) . . . . ?
C5 C8 C9 C13 2.7(3) . . . . ?
N4 C8 C9 C10 2.4(3) . . . . ?
C5 C8 C9 C10 -179.09(19) . . . . ?
C13 C9 C10 C11 0.3(3) . . . . ?
C8 C9 C10 C11 -178.0(2) . . . . ?
C9 C10 C11 C12 0.9(3) . . . . ?
C13 N1 C12 C11 -0.5(3) . . . . ?
Cu1 N1 C12 C11 175.23(18) . . . . ?
C10 C11 C12 N1 -0.9(4) . . . . ?
C12 N1 C13 C9 1.8(3) . . . . ?
Cu1 N1 C13 C9 -174.59(16) . . . . ?
C12 N1 C13 C14 -178.86(19) . . . . ?
Cu1 N1 C13 C14 4.8(2) . . . . ?
C10 C9 C13 N1 -1.7(3) . . . . ?
C8 C9 C13 N1 176.66(18) . . . . ?
C10 C9 C13 C14 179.00(18) . . . . ?
C8 C9 C13 C14 -2.7(3) . . . . ?
C1 N2 C14 C4 -2.0(3) . . . . ?
Cu1 N2 C14 C4 174.53(15) . . . . ?
C1 N2 C14 C13 179.31(18) . . . . ?
Cu1 N2 C14 C13 -4.2(2) . . . . ?
C3 C4 C14 N2 1.8(3) . . . . ?
C5 C4 C14 N2 -176.45(18) . . . . ?
C3 C4 C14 C13 -179.57(18) . . . . ?
C5 C4 C14 C13 2.2(3) . . . . ?
N1 C13 C14 N2 -0.4(3) . . . . ?
C9 C13 C14 N2 178.98(18) . . . . ?
N1 C13 C14 C4 -179.16(18) . . . . ?
C9 C13 C14 C4 0.2(3) . . . . ?
Cu1 O1 C15 O2 9.0(3) . . . . ?
Cu1 O1 C15 C16 -171.98(13) . . . . ?
O2 C15 C16 C22 -178.72(19) . . . . ?
O1 C15 C16 C22 2.2(3) . . . . ?
O2 C15 C16 C17 0.1(3) . . . . ?
O1 C15 C16 C17 -178.98(18) . . . . ?
C22 C16 C17 C18 0.0(3) . . . . ?
C15 C16 C17 C18 -178.76(17) . . . . ?
C16 C17 C18 C20 -0.2(3) . . . . ?
C16 C17 C18 C19 179.54(18) . . . . ?
C20 C18 C19 O3 -172.3(2) . . . . ?
C17 C18 C19 O3 8.0(3) . . . . ?
C20 C18 C19 O4 6.8(3) . . . . ?
C17 C18 C19 O4 -172.97(19) . . . . ?
C17 C18 C20 C21 -0.1(3) . . . . ?
C19 C18 C20 C21 -179.84(18) . . . . ?
C23 O7 C21 C22 -35.0(3) . . . . ?
C23 O7 C21 C20 149.8(2) . . . . ?
C18 C20 C21 C22 0.6(3) . . . . ?
C18 C20 C21 O7 175.77(18) . . . . ?
O7 C21 C22 C16 -175.70(19) . . . . ?
C20 C21 C22 C16 -0.7(3) . . . . ?
C17 C16 C22 C21 0.4(3) . . . . ?
C15 C16 C22 C21 179.21(18) . . . . ?
C21 O7 C23 C29 121.9(2) . . . . ?
C21 O7 C23 C24 -62.3(3) . . . . ?
C29 C23 C24 C25 -0.4(3) . . . . ?
O7 C23 C24 C25 -176.02(19) . . . . ?
C23 C24 C25 C26 -0.3(3) . . . . ?
C24 C25 C26 C28 1.2(3) . . . . ?
C24 C25 C26 C27 -176.6(2) . . . . ?
C28 C26 C27 O6 -175.8(2) . . . . ?
C25 C26 C27 O6 2.0(3) . . . . ?
C28 C26 C27 O5 2.9(3) . . . . ?
C25 C26 C27 O5 -179.4(2) . . . . ?
C25 C26 C28 C29 -1.4(3) . . . . ?
C27 C26 C28 C29 176.4(2) . . . . ?
C24 C23 C29 C28 0.2(3) . . . . ?
O7 C23 C29 C28 175.9(2) . . . . ?
C26 C28 C29 C23 0.7(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
O1W H1A O3 0.85 1.95 2.773(2) 163 2_756
O1W H1B O2 0.85 1.81 2.619(2) 158 .
O2W H2A O6 0.85 1.76 2.612(2) 177 4_565
O2W H2B O5 0.85 2.10 2.948(2) 170 2_646
O4 H4A O5 0.96 1.52 2.475(2) 170 1_545

_refine_diff_density_max         0.316
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.050

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1964453'
loop_
_audit_author_name
_audit_author_address
'Liang Shuang'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-11-08 deposited with the CCDC.	2020-01-06 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         'C29 H18 Co N4 O8, H2 O'
_chemical_formula_sum            'C29 H20 Co N4 O9'
_chemical_formula_weight         627.42

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                   9.6652(6)
_cell_length_b                   11.5260(7)
_cell_length_c                   12.5516(8)
_cell_angle_alpha                80.708(1)
_cell_angle_beta                 89.602(1)
_cell_angle_gamma                70.774(1)
_cell_volume                     1301.35(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3786
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.19

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_F_000             642
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.726
_shelx_estimated_absorpt_T_min   0.822
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 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  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8413
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.646
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5310
_reflns_number_gt                4620
_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       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0340P)²+0.5505P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5310
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_ref         0.0777
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.62589(3) 0.67615(2) 0.56796(2) 0.02432(8) Uani 1 1 d . . . . .
O1W O 0.68378(15) 0.55254(13) 0.46280(11) 0.0384(3) Uani 1 1 d . . . . .
H1A H 0.6576 0.4887 0.4596 0.046 Uiso 1 1 d R U . . .
H1B H 0.7650 0.5439 0.4318 0.046 Uiso 1 1 d R U . . .
O2W O 0.94395(18) 0.50513(16) 0.37301(13) 0.0635(5) Uani 1 1 d . . . . .
H2A H 0.9401 0.5367 0.3065 0.076 Uiso 1 1 d R U . . .
H2B H 1.0224 0.4437 0.3895 0.076 Uiso 1 1 d R U . . .
O1 O 0.44635(14) 0.81670(12) 0.48715(11) 0.0336(3) Uani 1 1 d . . . . .
O2 O 0.39353(14) 0.65040(12) 0.55763(11) 0.0320(3) Uani 1 1 d . . . . .
O3 O -0.18335(13) 0.72047(12) 0.54575(10) 0.0279(3) Uani 1 1 d . . . . .
O4 O -0.25454(14) 0.78798(13) 0.37246(10) 0.0356(3) Uani 1 1 d . . . . .
O5 O 0.17040(19) 1.16960(15) -0.17883(11) 0.0493(4) Uani 1 1 d . . . . .
H5A H 0.1910 1.1982 -0.2484 0.059 Uiso 1 1 d R U . . .
O6 O 0.08737(18) 1.37183(15) -0.16373(12) 0.0493(4) Uani 1 1 d . . . . .
O7 O -0.01628(15) 1.12672(11) 0.30305(10) 0.0324(3) Uani 1 1 d . . . . .
N1 N 0.58057(16) 0.78480(14) 0.69837(12) 0.0270(3) Uani 1 1 d . . . . .
N2 N 0.68318(16) 0.53918(14) 0.71129(12) 0.0275(3) Uani 1 1 d . . . . .
N3 N 0.66483(19) 0.48187(18) 1.09967(14) 0.0437(4) Uani 1 1 d . . . . .
N4 N 0.5571(2) 0.74273(19) 1.08698(14) 0.0462(5) Uani 1 1 d . . . . .
C1 C 0.7349(2) 0.41629(18) 0.71568(17) 0.0362(4) Uani 1 1 d . . . . .
H1 H 0.7547 0.3851 0.6513 0.043 Uiso 1 1 calc R U . . .
C2 C 0.7607(2) 0.33251(19) 0.81192(18) 0.0420(5) Uani 1 1 d . . . . .
H2 H 0.7966 0.2472 0.8113 0.050 Uiso 1 1 calc R U . . .
C3 C 0.7333(2) 0.37578(19) 0.90765(17) 0.0385(5) Uani 1 1 d . . . . .
H3 H 0.7504 0.3205 0.9727 0.046 Uiso 1 1 calc R U . . .
C4 C 0.6791(2) 0.50464(18) 0.90638(15) 0.0296(4) Uani 1 1 d . . . . .
C5 C 0.6439(2) 0.5598(2) 1.00371(15) 0.0342(4) Uani 1 1 d . . . . .
C6 C 0.6336(3) 0.5361(3) 1.18612(17) 0.0522(6) Uani 1 1 d . . . . .
H6 H 0.6471 0.4861 1.2538 0.063 Uiso 1 1 calc R U . . .
C7 C 0.5817(3) 0.6646(3) 1.18000(18) 0.0523(6) Uani 1 1 d . . . . .
H7 H 0.5634 0.6972 1.2438 0.063 Uiso 1 1 calc R U . . .
C8 C 0.5893(2) 0.6894(2) 0.99714(15) 0.0350(4) Uani 1 1 d . . . . .
C9 C 0.5670(2) 0.77030(19) 0.89246(16) 0.0332(4) Uani 1 1 d . . . . .
C10 C 0.5157(3) 0.9005(2) 0.87857(19) 0.0466(5) Uani 1 1 d . . . . .
H10 H 0.4919 0.9403 0.9383 0.056 Uiso 1 1 calc R U . . .
C11 C 0.5006(3) 0.9692(2) 0.77699(19) 0.0472(6) Uani 1 1 d . . . . .
H11 H 0.4692 1.0558 0.7673 0.057 Uiso 1 1 calc R U . . .
C12 C 0.5328(2) 0.90797(18) 0.68864(17) 0.0364(4) Uani 1 1 d . . . . .
H12 H 0.5202 0.9553 0.6198 0.044 Uiso 1 1 calc R U . . .
C13 C 0.59921(19) 0.71691(17) 0.79897(14) 0.0263(4) Uani 1 1 d . . . . .
C14 C 0.65604(19) 0.58287(17) 0.80587(14) 0.0255(4) Uani 1 1 d . . . . .
C15 C 0.35534(19) 0.75954(16) 0.50448(14) 0.0256(4) Uani 1 1 d . . . . .
C16 C 0.20050(18) 0.82416(16) 0.45946(13) 0.0227(3) Uani 1 1 d . . . . .
C17 C 0.09089(18) 0.77075(15) 0.48160(13) 0.0215(3) Uani 1 1 d . . . . .
H17 H 0.1122 0.6944 0.5273 0.026 Uiso 1 1 calc R U . . .
C18 C -0.04991(18) 0.83128(15) 0.43562(13) 0.0215(3) Uani 1 1 d . . . . .
C19 C -0.17084(18) 0.77514(16) 0.45199(14) 0.0234(4) Uani 1 1 d . . . . .
C20 C -0.08289(19) 0.94823(16) 0.37124(14) 0.0252(4) Uani 1 1 d . . . . .
H20 H -0.1765 0.9889 0.3393 0.030 Uiso 1 1 calc R U . . .
C21 C 0.0239(2) 1.00329(16) 0.35523(13) 0.0252(4) Uani 1 1 d . . . . .
C22 C 0.16612(19) 0.94209(16) 0.39649(14) 0.0254(4) Uani 1 1 d . . . . .
H22 H 0.2380 0.9791 0.3824 0.030 Uiso 1 1 calc R U . . .
C23 C 0.0277(2) 1.15134(16) 0.20024(14) 0.0266(4) Uani 1 1 d . . . . .
C24 C 0.0761(3) 1.06256(18) 0.13450(16) 0.0416(5) Uani 1 1 d . . . . .
H24 H 0.0862 0.9798 0.1605 0.050 Uiso 1 1 calc R U . . .
C25 C 0.1094(3) 1.09749(19) 0.02973(16) 0.0417(5) Uani 1 1 d . . . . .
H25 H 0.1431 1.0377 -0.0146 0.050 Uiso 1 1 calc R U . . .
C26 C 0.0934(2) 1.22048(18) -0.00990(15) 0.0315(4) Uani 1 1 d . . . . .
C27 C 0.1171(2) 1.2622(2) -0.12489(16) 0.0364(5) Uani 1 1 d . . . . .
C28 C 0.0469(2) 1.30808(18) 0.05788(16) 0.0354(4) Uani 1 1 d . . . . .
H28 H 0.0370 1.3909 0.0320 0.042 Uiso 1 1 calc R U . . .
C29 C 0.0154(2) 1.27417(17) 0.16293(15) 0.0332(4) Uani 1 1 d . . . . .
H29 H -0.0139 1.3332 0.2084 0.040 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
Co1 O1W 2.0390(13) . ?
Co1 O1 2.0753(13) . ?
Co1 O3 2.0749(12) 1_655 ?
Co1 N2 2.1346(15) . ?
Co1 N1 2.1748(15) . ?
Co1 O2 2.3672(13) . ?
O1W H1A 0.8593 . ?
O1W H1B 0.8567 . ?
O2W H2A 0.8515 . ?
O2W H2B 0.8487 . ?
O1 C15 1.260(2) . ?
O2 C15 1.261(2) . ?
O3 C19 1.267(2) . ?
O3 Co1 2.0749(12) 1_455 ?
O4 C19 1.248(2) . ?
O5 C27 1.315(3) . ?
O5 H5A 0.9266 . ?
O6 C27 1.217(2) . ?
O7 C23 1.371(2) . ?
O7 C21 1.394(2) . ?
N1 C12 1.325(2) . ?
N1 C13 1.353(2) . ?
N2 C1 1.330(2) . ?
N2 C14 1.354(2) . ?
N3 C6 1.323(3) . ?
N3 C5 1.354(3) . ?
N4 C7 1.324(3) . ?
N4 C8 1.356(3) . ?
C1 C2 1.387(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.366(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.400(3) . ?
C3 H3 0.9300 . ?
C4 C14 1.399(3) . ?
C4 C5 1.454(3) . ?
C5 C8 1.400(3) . ?
C6 C7 1.388(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.455(3) . ?
C9 C13 1.398(3) . ?
C9 C10 1.398(3) . ?
C10 C11 1.369(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.388(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.447(3) . ?
C15 C16 1.502(2) . ?
C16 C22 1.394(2) . ?
C16 C17 1.396(2) . ?
C17 C18 1.388(2) . ?
C17 H17 0.9300 . ?
C18 C20 1.393(2) . ?
C18 C19 1.510(2) . ?
C20 C21 1.377(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.378(3) . ?
C23 C29 1.383(2) . ?
C24 C25 1.380(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(3) . ?
C25 H25 0.9300 . ?
C26 C28 1.385(3) . ?
C26 C27 1.487(3) . ?
C28 C29 1.375(3) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1W Co1 O1 102.66(6) . . ?
O1W Co1 O3 92.19(5) . 1_655 ?
O1 Co1 O3 111.29(5) . 1_655 ?
O1W Co1 N2 95.82(6) . . ?
O1 Co1 N2 140.99(5) . . ?
O3 Co1 N2 101.87(5) 1_655 . ?
O1W Co1 N1 171.58(6) . . ?
O1 Co1 N1 85.10(6) . . ?
O3 Co1 N1 87.93(5) 1_655 . ?
N2 Co1 N1 75.93(6) . . ?
O1W Co1 O2 84.66(5) . . ?
O1 Co1 O2 58.71(5) . . ?
O3 Co1 O2 168.24(5) 1_655 . ?
N2 Co1 O2 89.74(5) . . ?
N1 Co1 O2 96.84(5) . . ?
Co1 O1W H1A 129.3 . . ?
Co1 O1W H1B 117.7 . . ?
H1A O1W H1B 109.3 . . ?
H2A O2W H2B 110.7 . . ?
C15 O1 Co1 96.90(11) . . ?
C15 O2 Co1 83.55(10) . . ?
C19 O3 Co1 115.58(11) . 1_455 ?
C27 O5 H5A 111.1 . . ?
C23 O7 C21 118.84(14) . . ?
C12 N1 C13 118.09(16) . . ?
C12 N1 Co1 126.90(13) . . ?
C13 N1 Co1 114.96(12) . . ?
C1 N2 C14 117.69(16) . . ?
C1 N2 Co1 126.16(13) . . ?
C14 N2 Co1 116.04(12) . . ?
C6 N3 C5 115.8(2) . . ?
C7 N4 C8 115.8(2) . . ?
N2 C1 C2 122.96(19) . . ?
N2 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.72(19) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 119.01(19) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C14 C4 C3 117.72(18) . . ?
C14 C4 C5 119.13(18) . . ?
C3 C4 C5 123.15(18) . . ?
N3 C5 C8 121.64(19) . . ?
N3 C5 C4 117.88(19) . . ?
C8 C5 C4 120.48(17) . . ?
N3 C6 C7 122.7(2) . . ?
N3 C6 H6 118.6 . . ?
C7 C6 H6 118.6 . . ?
N4 C7 C6 122.6(2) . . ?
N4 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
N4 C8 C5 121.42(19) . . ?
N4 C8 C9 118.44(19) . . ?
C5 C8 C9 120.14(17) . . ?
C13 C9 C10 116.83(19) . . ?
C13 C9 C8 119.21(18) . . ?
C10 C9 C8 123.96(19) . . ?
C11 C10 C9 119.9(2) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 119.2(2) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
N1 C12 C11 122.7(2) . . ?
N1 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
N1 C13 C9 123.24(17) . . ?
N1 C13 C14 116.15(16) . . ?
C9 C13 C14 120.61(17) . . ?
N2 C14 C4 122.90(17) . . ?
N2 C14 C13 116.66(16) . . ?
C4 C14 C13 120.43(17) . . ?
O1 C15 O2 120.85(16) . . ?
O1 C15 C16 118.37(16) . . ?
O2 C15 C16 120.78(15) . . ?
C22 C16 C17 119.79(16) . . ?
C22 C16 C15 118.40(15) . . ?
C17 C16 C15 121.79(15) . . ?
C18 C17 C16 120.19(15) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C20 119.62(15) . . ?
C17 C18 C19 122.57(15) . . ?
C20 C18 C19 117.82(15) . . ?
O4 C19 O3 124.00(16) . . ?
O4 C19 C18 117.72(15) . . ?
O3 C19 C18 118.25(15) . . ?
C21 C20 C18 119.65(16) . . ?
C21 C20 H20 120.2 . . ?
C18 C20 H20 120.2 . . ?
C20 C21 C22 121.44(16) . . ?
C20 C21 O7 118.62(16) . . ?
C22 C21 O7 119.76(16) . . ?
C21 C22 C16 119.13(15) . . ?
C21 C22 H22 120.4 . . ?
C16 C22 H22 120.4 . . ?
O7 C23 C24 123.49(16) . . ?
O7 C23 C29 115.80(16) . . ?
C24 C23 C29 120.65(17) . . ?
C23 C24 C25 119.45(17) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C24 C25 C26 120.64(19) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C28 119.10(17) . . ?
C25 C26 C27 121.66(19) . . ?
C28 C26 C27 119.16(18) . . ?
O6 C27 O5 124.46(18) . . ?
O6 C27 C26 122.2(2) . . ?
O5 C27 C26 113.29(18) . . ?
C29 C28 C26 120.82(17) . . ?
C29 C28 H28 119.6 . . ?
C26 C28 H28 119.6 . . ?
C28 C29 C23 119.29(18) . . ?
C28 C29 H29 120.4 . . ?
C23 C29 H29 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 N2 C1 C2 0.5(3) . . . . ?
Co1 N2 C1 C2 -175.61(15) . . . . ?
N2 C1 C2 C3 -0.3(3) . . . . ?
C1 C2 C3 C4 0.2(3) . . . . ?
C2 C3 C4 C14 -0.2(3) . . . . ?
C2 C3 C4 C5 178.83(18) . . . . ?
C6 N3 C5 C8 -1.5(3) . . . . ?
C6 N3 C5 C4 178.95(17) . . . . ?
C14 C4 C5 N3 178.87(17) . . . . ?
C3 C4 C5 N3 -0.1(3) . . . . ?
C14 C4 C5 C8 -0.7(3) . . . . ?
C3 C4 C5 C8 -179.72(18) . . . . ?
C5 N3 C6 C7 0.5(3) . . . . ?
C8 N4 C7 C6 -1.6(3) . . . . ?
N3 C6 C7 N4 1.1(4) . . . . ?
C7 N4 C8 C5 0.5(3) . . . . ?
C7 N4 C8 C9 -179.02(19) . . . . ?
N3 C5 C8 N4 1.0(3) . . . . ?
C4 C5 C8 N4 -179.41(17) . . . . ?
N3 C5 C8 C9 -179.44(17) . . . . ?
C4 C5 C8 C9 0.1(3) . . . . ?
N4 C8 C9 C13 -179.79(17) . . . . ?
C5 C8 C9 C13 0.6(3) . . . . ?
N4 C8 C9 C10 0.8(3) . . . . ?
C5 C8 C9 C10 -178.72(19) . . . . ?
C13 C9 C10 C11 -0.6(3) . . . . ?
C8 C9 C10 C11 178.8(2) . . . . ?
C9 C10 C11 C12 1.8(3) . . . . ?
C13 N1 C12 C11 -0.4(3) . . . . ?
Co1 N1 C12 C11 177.03(16) . . . . ?
C10 C11 C12 N1 -1.4(3) . . . . ?
C12 N1 C13 C9 1.7(3) . . . . ?
Co1 N1 C13 C9 -176.03(14) . . . . ?
C12 N1 C13 C14 -178.08(16) . . . . ?
Co1 N1 C13 C14 4.20(19) . . . . ?
C10 C9 C13 N1 -1.2(3) . . . . ?
C8 C9 C13 N1 179.39(17) . . . . ?
C10 C9 C13 C14 178.57(18) . . . . ?
C8 C9 C13 C14 -0.8(3) . . . . ?
C1 N2 C14 C4 -0.5(3) . . . . ?
Co1 N2 C14 C4 175.99(13) . . . . ?
C1 N2 C14 C13 -179.75(16) . . . . ?
Co1 N2 C14 C13 -3.3(2) . . . . ?
C3 C4 C14 N2 0.3(3) . . . . ?
C5 C4 C14 N2 -178.70(16) . . . . ?
C3 C4 C14 C13 179.58(16) . . . . ?
C5 C4 C14 C13 0.5(3) . . . . ?
N1 C13 C14 N2 -0.7(2) . . . . ?
C9 C13 C14 N2 179.53(16) . . . . ?
N1 C13 C14 C4 -179.97(16) . . . . ?
C9 C13 C14 C4 0.3(3) . . . . ?
Co1 O1 C15 O2 -0.01(18) . . . . ?
Co1 O1 C15 C16 -179.49(13) . . . . ?
Co1 O2 C15 O1 0.01(16) . . . . ?
Co1 O2 C15 C16 179.48(15) . . . . ?
O1 C15 C16 C22 2.9(2) . . . . ?
O2 C15 C16 C22 -176.63(16) . . . . ?
O1 C15 C16 C17 -175.34(16) . . . . ?
O2 C15 C16 C17 5.2(3) . . . . ?
C22 C16 C17 C18 4.0(2) . . . . ?
C15 C16 C17 C18 -177.82(15) . . . . ?
C16 C17 C18 C20 -2.9(2) . . . . ?
C16 C17 C18 C19 176.80(15) . . . . ?
Co1 O3 C19 O4 -9.6(2) 1_455 . . . ?
Co1 O3 C19 C18 168.78(11) 1_455 . . . ?
C17 C18 C19 O4 -139.35(18) . . . . ?
C20 C18 C19 O4 40.4(2) . . . . ?
C17 C18 C19 O3 42.2(2) . . . . ?
C20 C18 C19 O3 -138.07(17) . . . . ?
C17 C18 C20 C21 -1.0(3) . . . . ?
C19 C18 C20 C21 179.31(15) . . . . ?
C18 C20 C21 C22 3.8(3) . . . . ?
C18 C20 C21 O7 -171.39(15) . . . . ?
C23 O7 C21 C20 -109.14(19) . . . . ?
C23 O7 C21 C22 75.6(2) . . . . ?
C20 C21 C22 C16 -2.7(3) . . . . ?
O7 C21 C22 C16 172.44(15) . . . . ?
C17 C16 C22 C21 -1.2(2) . . . . ?
C15 C16 C22 C21 -179.44(15) . . . . ?
C21 O7 C23 C24 17.3(3) . . . . ?
C21 O7 C23 C29 -165.21(17) . . . . ?
O7 C23 C24 C25 175.9(2) . . . . ?
C29 C23 C24 C25 -1.4(3) . . . . ?
C23 C24 C25 C26 -0.6(4) . . . . ?
C24 C25 C26 C28 1.7(3) . . . . ?
C24 C25 C26 C27 -175.0(2) . . . . ?
C25 C26 C27 O6 171.5(2) . . . . ?
C28 C26 C27 O6 -5.2(3) . . . . ?
C25 C26 C27 O5 -7.6(3) . . . . ?
C28 C26 C27 O5 175.67(18) . . . . ?
C25 C26 C28 C29 -0.8(3) . . . . ?
C27 C26 C28 C29 176.06(18) . . . . ?
C26 C28 C29 C23 -1.2(3) . . . . ?
O7 C23 C29 C28 -175.22(17) . . . . ?
C24 C23 C29 C28 2.3(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
O1W H1A O2 0.86 1.87 2.7282(18) 176 2_666
O1W H1B O2W 0.86 1.82 2.673(2) 173 .
O2W H2A O6 0.85 1.90 2.744(2) 172 2_675
O2W H2B O3 0.85 2.06 2.893(2) 167 2_666
O5 H5A O4 0.93 1.67 2.5803(19) 166 2_575

_refine_diff_density_max         0.319
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.048

####################################################################### 
# 
# 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 1963323'
loop_
_audit_author_name
_audit_author_address
'Liang Shuang'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-01-06 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         'C84 H50 N12 Ni3 O17'
_chemical_formula_sum            'C84 H50 N12 Ni3 O17'
_chemical_formula_weight         1675.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.7534(8)
_cell_length_b                   32.9347(16)
_cell_length_c                   15.7929(8)
_cell_angle_alpha                90
_cell_angle_beta                 111.776(1)
_cell_angle_gamma                90
_cell_volume                     7609.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3443
_cell_measurement_theta_min      2.3173
_cell_measurement_theta_max      21.5172

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_F_000             3432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.815
_shelx_estimated_absorpt_T_min   0.835
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 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  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44191
_diffrn_reflns_av_unetI/netI     0.1242
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.237
_diffrn_reflns_theta_max         25.142
_diffrn_reflns_theta_full        25.142
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             13572
_reflns_number_gt                7724
_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       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0519P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13572
_refine_ls_number_parameters     1045
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.1338
_refine_ls_wR_factor_gt          0.1140
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.01522(4) 0.51082(2) 0.33036(5) 0.02464(18) Uani 1 1 d . . . . .
Ni2 Ni 0.55451(4) 0.18770(2) 0.09652(5) 0.02424(17) Uani 1 1 d . . . . .
Ni3 Ni -0.51379(4) 0.36401(2) -0.15644(5) 0.02684(18) Uani 1 1 d . . . . .
O1W O 0.09068(19) 0.52516(9) 0.4664(2) 0.0329(9) Uani 1 1 d . . . . .
H1A H 0.0671 0.5307 0.5060 0.039 Uiso 1 1 d R U . . .
H1B H 0.1277 0.5050 0.4855 0.039 Uiso 1 1 d R U . . .
O2W O -0.60572(19) 0.36000(9) -0.2905(2) 0.0353(9) Uani 1 1 d . . . . .
H2A H -0.5819 0.3748 -0.3208 0.042 Uiso 1 1 d R U . . .
H2B H -0.6213 0.3371 -0.3184 0.042 Uiso 1 1 d R U . . .
O3W O -0.4318(2) 0.39605(9) -0.2112(2) 0.0366(9) Uani 1 1 d . . . . .
H3A H -0.3867 0.4055 -0.1655 0.044 Uiso 1 1 d R U . . .
H3B H -0.4130 0.3753 -0.2323 0.044 Uiso 1 1 d R U . . .
O1 O 0.1131(2) 0.47148(9) 0.3304(2) 0.0332(9) Uani 1 1 d . . . . .
O2 O 0.1953(3) 0.46408(14) 0.4787(3) 0.0758(16) Uani 1 1 d . . . . .
O3 O 0.4591(2) 0.36286(9) 0.5724(2) 0.0306(8) Uani 1 1 d . . . . .
O4 O 0.4672(2) 0.32421(9) 0.4628(2) 0.0332(9) Uani 1 1 d . . . . .
O5 O 0.2802(2) 0.39350(10) 0.1708(3) 0.0465(11) Uani 1 1 d . . . . .
O6 O 0.3572(3) 0.20956(11) 0.1222(4) 0.0717(15) Uani 1 1 d . . . . .
O7 O 0.4795(2) 0.23569(9) 0.1047(2) 0.0337(9) Uani 1 1 d . . . . .
O8 O -0.07004(19) 0.46703(9) 0.3555(2) 0.0279(8) Uani 1 1 d . . . . .
O9 O -0.08172(19) 0.48161(9) 0.2158(2) 0.0295(9) Uani 1 1 d . . . . .
O10 O -0.4235(2) 0.37405(9) -0.0233(2) 0.0314(9) Uani 1 1 d . . . . .
O11 O -0.3246(3) 0.41652(13) -0.0478(3) 0.0725(15) Uani 1 1 d . . . . .
O12 O -0.3260(2) 0.37031(9) 0.3199(2) 0.0354(9) Uani 1 1 d . . . . .
O13 O -0.45226(19) 0.19001(9) 0.3407(2) 0.0299(9) Uani 1 1 d . . . . .
O14 O -0.38775(19) 0.18080(9) 0.2379(2) 0.0285(8) Uani 1 1 d . . . . .
N1 N -0.0724(2) 0.55921(11) 0.3225(3) 0.0254(10) Uani 1 1 d . . . . .
N2 N 0.0699(2) 0.55471(11) 0.2707(3) 0.0280(10) Uani 1 1 d . . . . .
N3 N -0.0832(3) 0.70384(12) 0.2874(3) 0.0366(12) Uani 1 1 d . . . . .
N4 N 0.0731(2) 0.69939(12) 0.2397(3) 0.0355(12) Uani 1 1 d . . . . .
N5 N 0.6458(2) 0.22617(11) 0.0684(3) 0.0235(10) Uani 1 1 d . . . . .
N6 N 0.6471(2) 0.14556(11) 0.0814(3) 0.0289(11) Uani 1 1 d . . . . .
N7 N 0.9224(2) 0.22386(12) 0.0068(3) 0.0339(11) Uani 1 1 d . . . . .
N8 N 0.9078(3) 0.13830(12) -0.0064(3) 0.0353(11) Uani 1 1 d . . . . .
N9 N -0.6111(2) 0.33294(12) -0.1218(3) 0.0289(11) Uani 1 1 d . . . . .
N10 N -0.5901(3) 0.41225(12) -0.1351(3) 0.0389(12) Uani 1 1 d . . . . .
N11 N -0.8779(3) 0.35411(16) -0.0490(3) 0.0579(15) Uani 1 1 d . . . . .
N12 N -0.8375(4) 0.43814(16) -0.0331(4) 0.0695(17) Uani 1 1 d . . . . .
C1 C -0.1472(3) 0.55968(14) 0.3427(4) 0.0315(13) Uani 1 1 d . . . . .
H1 H -0.1672 0.5354 0.3590 0.038 Uiso 1 1 calc R U . . .
C2 C -0.1963(3) 0.59473(15) 0.3405(4) 0.0362(14) Uani 1 1 d . . . . .
H2 H -0.2493 0.5939 0.3535 0.043 Uiso 1 1 calc R U . . .
C3 C -0.1653(3) 0.63074(15) 0.3186(4) 0.0348(14) Uani 1 1 d . . . . .
H3 H -0.1974 0.6546 0.3168 0.042 Uiso 1 1 calc R U . . .
C4 C -0.0867(3) 0.63161(13) 0.2991(3) 0.0252(12) Uani 1 1 d . . . . .
C5 C -0.0431(3) 0.59453(13) 0.2993(3) 0.0243(12) Uani 1 1 d . . . . .
C6 C 0.0354(3) 0.59235(13) 0.2722(4) 0.0275(13) Uani 1 1 d . . . . .
C7 C 0.1364(3) 0.55088(15) 0.2394(4) 0.0366(14) Uani 1 1 d . . . . .
H7 H 0.1596 0.5251 0.2376 0.044 Uiso 1 1 calc R U . . .
C8 C 0.1732(3) 0.58348(15) 0.2092(4) 0.0433(16) Uani 1 1 d . . . . .
H8 H 0.2184 0.5795 0.1853 0.052 Uiso 1 1 calc R U . . .
C9 C 0.1417(3) 0.62175(15) 0.2153(4) 0.0388(15) Uani 1 1 d . . . . .
H9 H 0.1675 0.6442 0.1985 0.047 Uiso 1 1 calc R U . . .
C10 C 0.0706(3) 0.62673(14) 0.2469(4) 0.0286(13) Uani 1 1 d . . . . .
C11 C 0.0322(3) 0.66637(14) 0.2554(4) 0.0307(13) Uani 1 1 d . . . . .
C12 C -0.0457(3) 0.66865(13) 0.2791(4) 0.0276(13) Uani 1 1 d . . . . .
C13 C -0.0408(3) 0.73771(14) 0.2731(4) 0.0364(14) Uani 1 1 d . . . . .
C14 C 0.0362(3) 0.73554(14) 0.2507(4) 0.0370(15) Uani 1 1 d . . . . .
C15 C 0.0790(3) 0.77179(16) 0.2388(4) 0.0491(18) Uani 1 1 d . . . . .
H15 H 0.1295 0.7707 0.2217 0.059 Uiso 1 1 calc R U . . .
C16 C 0.0450(4) 0.80830(16) 0.2526(5) 0.0564(19) Uani 1 1 d . . . . .
H16 H 0.0746 0.8321 0.2480 0.068 Uiso 1 1 calc R U . . .
C17 C -0.0334(5) 0.81032(17) 0.2735(5) 0.0597(19) Uani 1 1 d . . . . .
H17 H -0.0564 0.8355 0.2807 0.072 Uiso 1 1 calc R U . . .
C18 C -0.0767(4) 0.77597(15) 0.2837(5) 0.0548(18) Uani 1 1 d . . . . .
H18 H -0.1291 0.7776 0.2974 0.066 Uiso 1 1 calc R U . . .
C19 C 0.6413(3) 0.26611(14) 0.0593(4) 0.0305(13) Uani 1 1 d . . . . .
H19 H 0.5929 0.2797 0.0669 0.037 Uiso 1 1 calc R U . . .
C20 C 0.7053(3) 0.28861(14) 0.0388(4) 0.0346(14) Uani 1 1 d . . . . .
H20 H 0.6995 0.3167 0.0331 0.042 Uiso 1 1 calc R U . . .
C21 C 0.7766(3) 0.26952(14) 0.0272(4) 0.0320(13) Uani 1 1 d . . . . .
H21 H 0.8207 0.2844 0.0147 0.038 Uiso 1 1 calc R U . . .
C22 C 0.7828(3) 0.22710(13) 0.0344(3) 0.0253(12) Uani 1 1 d . . . . .
C23 C 0.7151(3) 0.20658(13) 0.0550(3) 0.0229(12) Uani 1 1 d . . . . .
C24 C 0.7146(3) 0.16258(13) 0.0590(3) 0.0234(12) Uani 1 1 d . . . . .
C25 C 0.6425(3) 0.10533(15) 0.0819(4) 0.0378(14) Uani 1 1 d . . . . .
H25 H 0.5977 0.0933 0.0987 0.045 Uiso 1 1 calc R U . . .
C26 C 0.7016(3) 0.08041(15) 0.0586(4) 0.0398(15) Uani 1 1 d . . . . .
H26 H 0.6951 0.0523 0.0581 0.048 Uiso 1 1 calc R U . . .
C27 C 0.7687(3) 0.09760(14) 0.0368(4) 0.0363(14) Uani 1 1 d . . . . .
H27 H 0.8092 0.0812 0.0217 0.044 Uiso 1 1 calc R U . . .
C28 C 0.7777(3) 0.13985(13) 0.0367(3) 0.0253(12) Uani 1 1 d . . . . .
C29 C 0.8491(3) 0.16051(14) 0.0149(3) 0.0263(12) Uani 1 1 d . . . . .
C30 C 0.8538(3) 0.20381(14) 0.0186(3) 0.0270(12) Uani 1 1 d . . . . .
C31 C 0.9856(3) 0.20145(17) -0.0107(4) 0.0372(14) Uani 1 1 d . . . . .
C32 C 0.9770(3) 0.15855(17) -0.0206(4) 0.0386(15) Uani 1 1 d . . . . .
C33 C 1.0423(4) 0.13610(19) -0.0429(4) 0.0520(17) Uani 1 1 d . . . . .
H33 H 1.0349 0.1083 -0.0538 0.062 Uiso 1 1 calc R U . . .
C34 C 1.1158(4) 0.1557(2) -0.0484(5) 0.060(2) Uani 1 1 d . . . . .
H34 H 1.1591 0.1411 -0.0631 0.072 Uiso 1 1 calc R U . . .
C35 C 1.1274(4) 0.1975(2) -0.0320(5) 0.063(2) Uani 1 1 d . . . . .
H35 H 1.1804 0.2099 -0.0322 0.075 Uiso 1 1 calc R U . . .
C36 C 1.0637(3) 0.22049(18) -0.0159(4) 0.0515(17) Uani 1 1 d . . . . .
H36 H 1.0713 0.2484 -0.0084 0.062 Uiso 1 1 calc R U . . .
C37 C -0.6241(3) 0.29281(16) -0.1217(4) 0.0399(15) Uani 1 1 d . . . . .
H37 H -0.5812 0.2759 -0.1312 0.048 Uiso 1 1 calc R U . . .
C38 C -0.6975(3) 0.27511(17) -0.1085(4) 0.0470(16) Uani 1 1 d . . . . .
H38 H -0.7046 0.2471 -0.1108 0.056 Uiso 1 1 calc R U . . .
C39 C -0.7596(3) 0.29970(18) -0.0919(4) 0.0443(16) Uani 1 1 d . . . . .
H39 H -0.8092 0.2885 -0.0818 0.053 Uiso 1 1 calc R U . . .
C40 C -0.7482(3) 0.34126(16) -0.0902(4) 0.0359(14) Uani 1 1 d . . . . .
C41 C -0.6735(3) 0.35697(15) -0.1058(3) 0.0312(13) Uani 1 1 d . . . . .
C42 C -0.6598(3) 0.40021(16) -0.1097(4) 0.0371(14) Uani 1 1 d . . . . .
C43 C -0.5767(4) 0.45187(17) -0.1415(5) 0.0608(19) Uani 1 1 d . . . . .
H43 H -0.5303 0.4606 -0.1603 0.073 Uiso 1 1 calc R U . . .
C44 C -0.6316(5) 0.48092(19) -0.1202(6) 0.091(3) Uani 1 1 d . . . . .
H44 H -0.6204 0.5085 -0.1236 0.109 Uiso 1 1 calc R U . . .
C45 C -0.7006(5) 0.46853(19) -0.0950(5) 0.076(2) Uani 1 1 d . . . . .
H45 H -0.7374 0.4876 -0.0817 0.092 Uiso 1 1 calc R U . . .
C46 C -0.7168(4) 0.42722(17) -0.0887(4) 0.0473(16) Uani 1 1 d . . . . .
C47 C -0.7901(4) 0.4117(2) -0.0620(4) 0.0517(18) Uani 1 1 d . . . . .
C48 C -0.8091(4) 0.36942(19) -0.0673(4) 0.0455(16) Uani 1 1 d . . . . .
C49 C -0.9264(4) 0.3804(3) -0.0189(5) 0.068(2) Uani 1 1 d . . . . .
C50 C -0.9053(5) 0.4216(3) -0.0074(5) 0.074(2) Uani 1 1 d . . . . .
C51 C -0.9523(5) 0.4481(3) 0.0304(6) 0.094(3) Uani 1 1 d . . . . .
H51 H -0.9373 0.4755 0.0389 0.113 Uiso 1 1 calc R U . . .
C52 C -1.0198(6) 0.4325(3) 0.0538(7) 0.111(4) Uani 1 1 d . . . . .
H52 H -1.0516 0.4495 0.0785 0.133 Uiso 1 1 calc R U . . .
C53 C -1.0426(6) 0.3925(4) 0.0421(7) 0.115(4) Uani 1 1 d . . . . .
H53 H -1.0899 0.3831 0.0587 0.138 Uiso 1 1 calc R U . . .
C54 C -0.9979(4) 0.3658(3) 0.0067(6) 0.089(3) Uani 1 1 d . . . . .
H54 H -1.0143 0.3385 -0.0003 0.106 Uiso 1 1 calc R U . . .
C55 C 0.1788(3) 0.45697(14) 0.3968(4) 0.0347(14) Uani 1 1 d . . . . .
C56 C 0.2415(3) 0.42881(14) 0.3733(4) 0.0308(13) Uani 1 1 d . . . . .
C57 C 0.3082(3) 0.40707(13) 0.4417(4) 0.0273(12) Uani 1 1 d . . . . .
H57 H 0.3162 0.4112 0.5024 0.033 Uiso 1 1 calc R U . . .
C58 C 0.3626(3) 0.37931(14) 0.4191(4) 0.0274(13) Uani 1 1 d . . . . .
C59 C 0.3532(3) 0.37441(14) 0.3297(4) 0.0366(14) Uani 1 1 d . . . . .
H59 H 0.3902 0.3559 0.3149 0.044 Uiso 1 1 calc R U . . .
C60 C 0.2893(3) 0.39677(15) 0.2614(4) 0.0344(14) Uani 1 1 d . . . . .
C61 C 0.2321(3) 0.42332(14) 0.2828(4) 0.0322(14) Uani 1 1 d . . . . .
H61 H 0.1872 0.4375 0.2367 0.039 Uiso 1 1 calc R U . . .
C62 C 0.4331(3) 0.35410(15) 0.4891(4) 0.0282(13) Uani 1 1 d . . . . .
C63 C 0.3099(3) 0.35586(16) 0.1500(4) 0.0353(14) Uani 1 1 d . . . . .
C64 C 0.3894(3) 0.35300(15) 0.1344(4) 0.0347(14) Uani 1 1 d . . . . .
H64 H 0.4229 0.3761 0.1330 0.042 Uiso 1 1 calc R U . . .
C65 C 0.4186(3) 0.31472(15) 0.1209(4) 0.0363(14) Uani 1 1 d . . . . .
H65 H 0.4721 0.3122 0.1093 0.044 Uiso 1 1 calc R U . . .
C66 C 0.3703(3) 0.28030(14) 0.1242(4) 0.0285(13) Uani 1 1 d . . . . .
C67 C 0.2888(3) 0.28456(16) 0.1369(4) 0.0405(15) Uani 1 1 d . . . . .
H67 H 0.2542 0.2617 0.1369 0.049 Uiso 1 1 calc R U . . .
C68 C 0.2583(3) 0.32242(16) 0.1496(4) 0.0466(17) Uani 1 1 d . . . . .
H68 H 0.2032 0.3252 0.1579 0.056 Uiso 1 1 calc R U . . .
C69 C 0.4056(3) 0.23801(15) 0.1166(4) 0.0337(14) Uani 1 1 d . . . . .
C70 C -0.1079(3) 0.46192(13) 0.2692(4) 0.0262(13) Uani 1 1 d . . . . .
C71 C -0.1877(3) 0.43326(13) 0.2324(4) 0.0244(12) Uani 1 1 d . . . . .
C72 C -0.2304(3) 0.42783(13) 0.1391(4) 0.0266(12) Uani 1 1 d . . . . .
H72 H -0.2080 0.4409 0.0995 0.032 Uiso 1 1 calc R U . . .
C73 C -0.3072(3) 0.40274(13) 0.1046(4) 0.0264(12) Uani 1 1 d . . . . .
C74 C -0.3387(3) 0.38311(13) 0.1644(4) 0.0288(13) Uani 1 1 d . . . . .
H74 H -0.3900 0.3665 0.1420 0.035 Uiso 1 1 calc R U . . .
C75 C -0.2944(3) 0.38798(13) 0.2572(4) 0.0271(12) Uani 1 1 d . . . . .
C76 C -0.2178(3) 0.41297(13) 0.2928(4) 0.0283(13) Uani 1 1 d . . . . .
H76 H -0.1878 0.4159 0.3554 0.034 Uiso 1 1 calc R U . . .
C77 C -0.3554(3) 0.39761(14) 0.0035(4) 0.0327(13) Uani 1 1 d . . . . .
C78 C -0.3433(3) 0.32905(13) 0.3119(4) 0.0262(13) Uani 1 1 d . . . . .
C79 C -0.2939(3) 0.30205(14) 0.2818(4) 0.0321(13) Uani 1 1 d . . . . .
H79 H -0.2469 0.3113 0.2646 0.039 Uiso 1 1 calc R U . . .
C80 C -0.3145(3) 0.26130(13) 0.2773(4) 0.0289(13) Uani 1 1 d . . . . .
H80 H -0.2813 0.2432 0.2565 0.035 Uiso 1 1 calc R U . . .
C81 C -0.3836(3) 0.24692(13) 0.3031(3) 0.0232(12) Uani 1 1 d . . . . .
C82 C -0.4302(3) 0.27433(13) 0.3364(3) 0.0263(12) Uani 1 1 d . . . . .
H82 H -0.4753 0.2650 0.3563 0.032 Uiso 1 1 calc R U . . .
C83 C -0.4105(3) 0.31535(14) 0.3407(4) 0.0298(13) Uani 1 1 d . . . . .
H83 H -0.4424 0.3335 0.3629 0.036 Uiso 1 1 calc R U . . .
C84 C -0.4098(3) 0.20272(14) 0.2931(4) 0.0234(12) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.015(3) . ?
Ni1 N2 2.079(4) . ?
Ni1 N1 2.081(4) . ?
Ni1 O1W 2.087(3) . ?
Ni1 O8 2.107(3) . ?
Ni1 O9 2.117(3) . ?
Ni2 O7 2.006(3) . ?
Ni2 N5 2.084(4) . ?
Ni2 O14 2.087(3) 1_655 ?
Ni2 N6 2.090(4) . ?
Ni2 O4 2.086(3) 4_565 ?
Ni2 O3 2.180(3) 4_565 ?
Ni3 O13 2.034(3) 4_565 ?
Ni3 N9 2.078(4) . ?
Ni3 O2W 2.079(3) . ?
Ni3 O10 2.082(3) . ?
Ni3 O3W 2.088(3) . ?
Ni3 N10 2.094(4) . ?
O1W H1A 0.8583 . ?
O1W H1B 0.8606 . ?
O2W H2A 0.8610 . ?
O2W H2B 0.8626 . ?
O3W H3A 0.8624 . ?
O3W H3B 0.8607 . ?
O1 C55 1.263(6) . ?
O2 C55 1.243(7) . ?
O3 C62 1.256(6) . ?
O4 C62 1.263(6) . ?
O5 C60 1.388(6) . ?
O5 C63 1.406(6) . ?
O6 C69 1.232(6) . ?
O7 C69 1.247(6) . ?
O8 C70 1.280(6) . ?
O9 C70 1.248(6) . ?
O10 C77 1.263(5) . ?
O11 C77 1.252(6) . ?
O12 C78 1.383(5) . ?
O12 C75 1.390(6) . ?
O13 C84 1.250(6) . ?
O14 C84 1.275(6) . ?
N1 C1 1.330(6) . ?
N1 C5 1.351(6) . ?
N2 C7 1.319(6) . ?
N2 C6 1.357(5) . ?
N3 C12 1.329(6) . ?
N3 C13 1.362(6) . ?
N4 C11 1.334(6) . ?
N4 C14 1.364(6) . ?
N5 C19 1.322(5) . ?
N5 C23 1.352(5) . ?
N6 C25 1.327(6) . ?
N6 C24 1.359(6) . ?
N7 C30 1.336(6) . ?
N7 C31 1.348(6) . ?
N8 C29 1.317(6) . ?
N8 C32 1.365(6) . ?
N9 C37 1.338(6) . ?
N9 C41 1.356(6) . ?
N10 C43 1.332(6) . ?
N10 C42 1.360(7) . ?
N11 C48 1.321(7) . ?
N11 C49 1.351(8) . ?
N12 C47 1.334(7) . ?
N12 C50 1.386(9) . ?
C1 C2 1.383(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.375(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.383(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.401(6) . ?
C4 C12 1.468(6) . ?
C5 C6 1.452(6) . ?
C6 C10 1.384(6) . ?
C7 C8 1.387(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.371(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.395(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.466(6) . ?
C11 C12 1.412(7) . ?
C13 C14 1.386(7) . ?
C13 C18 1.417(7) . ?
C14 C15 1.417(7) . ?
C15 C16 1.366(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.393(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.362(7) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.382(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.357(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.402(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.399(6) . ?
C22 C30 1.452(6) . ?
C23 C24 1.451(6) . ?
C24 C28 1.391(6) . ?
C25 C26 1.390(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.352(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.399(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.460(7) . ?
C29 C30 1.428(6) . ?
C31 C36 1.410(7) . ?
C31 C32 1.422(7) . ?
C32 C33 1.414(7) . ?
C33 C34 1.355(8) . ?
C33 H33 0.9300 . ?
C34 C35 1.402(8) . ?
C34 H34 0.9300 . ?
C35 C36 1.353(8) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C38 1.377(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.369(7) . ?
C38 H38 0.9300 . ?
C39 C40 1.379(7) . ?
C39 H39 0.9300 . ?
C40 C41 1.389(7) . ?
C40 C48 1.473(7) . ?
C41 C42 1.445(7) . ?
C42 C46 1.388(7) . ?
C43 C44 1.411(8) . ?
C43 H43 0.9300 . ?
C44 C45 1.352(9) . ?
C44 H44 0.9300 . ?
C45 C46 1.394(8) . ?
C45 H45 0.9300 . ?
C46 C47 1.461(8) . ?
C47 C48 1.419(8) . ?
C49 C50 1.395(10) . ?
C49 C54 1.417(10) . ?
C50 C51 1.411(9) . ?
C51 C52 1.350(11) . ?
C51 H51 0.9300 . ?
C52 C53 1.358(12) . ?
C52 H52 0.9300 . ?
C53 C54 1.370(11) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 C56 1.498(7) . ?
C56 C61 1.392(7) . ?
C56 C57 1.393(6) . ?
C57 C58 1.387(6) . ?
C57 H57 0.9300 . ?
C58 C59 1.374(7) . ?
C58 C62 1.496(6) . ?
C59 C60 1.383(6) . ?
C59 H59 0.9300 . ?
C60 C61 1.386(7) . ?
C61 H61 0.9300 . ?
C63 C64 1.365(7) . ?
C63 C68 1.367(7) . ?
C64 C65 1.386(6) . ?
C64 H64 0.9300 . ?
C65 C66 1.377(6) . ?
C65 H65 0.9300 . ?
C66 C67 1.378(6) . ?
C66 C69 1.521(6) . ?
C67 C68 1.377(7) . ?
C67 H67 0.9300 . ?
C68 H68 0.9300 . ?
C70 C71 1.506(6) . ?
C71 C72 1.385(7) . ?
C71 C76 1.384(7) . ?
C72 C73 1.399(6) . ?
C72 H72 0.9300 . ?
C73 C74 1.379(7) . ?
C73 C77 1.503(7) . ?
C74 C75 1.379(7) . ?
C74 H74 0.9300 . ?
C75 C76 1.394(6) . ?
C76 H76 0.9300 . ?
C78 C83 1.374(6) . ?
C78 C79 1.377(7) . ?
C79 C80 1.376(6) . ?
C79 H79 0.9300 . ?
C80 C81 1.380(6) . ?
C80 H80 0.9300 . ?
C81 C82 1.385(6) . ?
C81 C84 1.505(6) . ?
C82 C83 1.382(6) . ?
C82 H82 0.9300 . ?
C83 H83 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N2 90.07(14) . . ?
O1 Ni1 N1 169.48(15) . . ?
N2 Ni1 N1 79.50(15) . . ?
O1 Ni1 O1W 90.09(13) . . ?
N2 Ni1 O1W 97.79(14) . . ?
N1 Ni1 O1W 90.00(14) . . ?
O1 Ni1 O8 95.82(12) . . ?
N2 Ni1 O8 164.14(14) . . ?
N1 Ni1 O8 94.61(13) . . ?
O1W Ni1 O8 96.92(13) . . ?
O1 Ni1 O9 91.01(13) . . ?
N2 Ni1 O9 102.58(15) . . ?
N1 Ni1 O9 92.57(13) . . ?
O1W Ni1 O9 159.60(13) . . ?
O8 Ni1 O9 62.71(13) . . ?
O7 Ni2 N5 90.25(14) . . ?
O7 Ni2 O14 92.90(14) . 1_655 ?
N5 Ni2 O14 103.45(14) . 1_655 ?
O7 Ni2 N6 169.48(15) . . ?
N5 Ni2 N6 79.25(14) . . ?
O14 Ni2 N6 90.27(15) 1_655 . ?
O7 Ni2 O4 91.72(13) . 4_565 ?
N5 Ni2 O4 98.45(14) . 4_565 ?
O14 Ni2 O4 157.58(12) 1_655 4_565 ?
N6 Ni2 O4 89.15(15) . 4_565 ?
O7 Ni2 O3 103.20(12) . 4_565 ?
N5 Ni2 O3 155.86(15) . 4_565 ?
O14 Ni2 O3 95.89(13) 1_655 4_565 ?
N6 Ni2 O3 86.44(13) . 4_565 ?
O4 Ni2 O3 61.71(13) 4_565 4_565 ?
O13 Ni3 N9 88.82(14) 4_565 . ?
O13 Ni3 O2W 94.57(13) 4_565 . ?
N9 Ni3 O2W 86.20(15) . . ?
O13 Ni3 O10 90.49(12) 4_565 . ?
N9 Ni3 O10 96.11(15) . . ?
O2W Ni3 O10 174.49(12) . . ?
O13 Ni3 O3W 93.44(13) 4_565 . ?
N9 Ni3 O3W 171.14(14) . . ?
O2W Ni3 O3W 85.08(13) . . ?
O10 Ni3 O3W 92.44(13) . . ?
O13 Ni3 N10 166.86(17) 4_565 . ?
N9 Ni3 N10 78.89(17) . . ?
O2W Ni3 N10 89.27(15) . . ?
O10 Ni3 N10 86.27(15) . . ?
O3W Ni3 N10 99.41(16) . . ?
Ni1 O1W H1A 124.3 . . ?
Ni1 O1W H1B 103.8 . . ?
H1A O1W H1B 109.3 . . ?
Ni3 O2W H2A 104.3 . . ?
Ni3 O2W H2B 122.4 . . ?
H2A O2W H2B 108.2 . . ?
Ni3 O3W H3A 106.3 . . ?
Ni3 O3W H3B 96.5 . . ?
H3A O3W H3B 108.5 . . ?
C55 O1 Ni1 129.4(4) . . ?
C62 O3 Ni2 86.7(3) . 4_566 ?
C62 O4 Ni2 90.8(3) . 4_566 ?
C60 O5 C63 113.1(4) . . ?
C69 O7 Ni2 131.5(3) . . ?
C70 O8 Ni1 88.1(3) . . ?
C70 O9 Ni1 88.5(3) . . ?
C77 O10 Ni3 127.8(3) . . ?
C78 O12 C75 117.2(4) . . ?
C84 O13 Ni3 132.2(3) . 4_566 ?
C84 O14 Ni2 123.3(3) . 1_455 ?
C1 N1 C5 118.5(4) . . ?
C1 N1 Ni1 128.4(3) . . ?
C5 N1 Ni1 112.9(3) . . ?
C7 N2 C6 118.2(4) . . ?
C7 N2 Ni1 128.5(3) . . ?
C6 N2 Ni1 113.0(3) . . ?
C12 N3 C13 115.8(4) . . ?
C11 N4 C14 115.4(4) . . ?
C19 N5 C23 118.1(4) . . ?
C19 N5 Ni2 128.0(3) . . ?
C23 N5 Ni2 113.9(3) . . ?
C25 N6 C24 117.6(4) . . ?
C25 N6 Ni2 128.3(3) . . ?
C24 N6 Ni2 113.7(3) . . ?
C30 N7 C31 117.0(4) . . ?
C29 N8 C32 116.7(4) . . ?
C37 N9 C41 117.0(4) . . ?
C37 N9 Ni3 127.9(3) . . ?
C41 N9 Ni3 114.7(3) . . ?
C43 N10 C42 118.4(5) . . ?
C43 N10 Ni3 127.9(4) . . ?
C42 N10 Ni3 113.6(3) . . ?
C48 N11 C49 116.7(6) . . ?
C47 N12 C50 115.7(6) . . ?
N1 C1 C2 122.8(5) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 118.6(5) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 120.3(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 117.4(4) . . ?
C3 C4 C12 124.5(4) . . ?
C5 C4 C12 118.0(4) . . ?
N1 C5 C4 122.3(4) . . ?
N1 C5 C6 116.8(4) . . ?
C4 C5 C6 120.9(4) . . ?
N2 C6 C10 122.4(5) . . ?
N2 C6 C5 116.1(4) . . ?
C10 C6 C5 121.4(4) . . ?
N2 C7 C8 123.1(5) . . ?
N2 C7 H7 118.4 . . ?
C8 C7 H7 118.4 . . ?
C9 C8 C7 118.6(5) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C8 C9 C10 119.5(5) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C6 C10 C9 117.9(4) . . ?
C6 C10 C11 118.6(5) . . ?
C9 C10 C11 123.4(4) . . ?
N4 C11 C12 122.3(4) . . ?
N4 C11 C10 117.7(5) . . ?
C12 C11 C10 120.0(4) . . ?
N3 C12 C11 122.3(4) . . ?
N3 C12 C4 117.2(5) . . ?
C11 C12 C4 120.5(4) . . ?
N3 C13 C14 122.0(5) . . ?
N3 C13 C18 117.8(5) . . ?
C14 C13 C18 120.1(5) . . ?
N4 C14 C13 122.2(4) . . ?
N4 C14 C15 118.2(5) . . ?
C13 C14 C15 119.6(5) . . ?
C16 C15 C14 119.1(6) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 120.9(5) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C18 C17 C16 121.1(5) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C17 C18 C13 119.0(6) . . ?
C17 C18 H18 120.5 . . ?
C13 C18 H18 120.5 . . ?
N5 C19 C20 123.0(4) . . ?
N5 C19 H19 118.5 . . ?
C20 C19 H19 118.5 . . ?
C21 C20 C19 119.6(5) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 119.2(5) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C23 C22 C21 117.6(4) . . ?
C23 C22 C30 119.1(4) . . ?
C21 C22 C30 123.2(4) . . ?
N5 C23 C22 122.4(4) . . ?
N5 C23 C24 116.8(4) . . ?
C22 C23 C24 120.7(4) . . ?
N6 C24 C28 123.1(4) . . ?
N6 C24 C23 116.2(4) . . ?
C28 C24 C23 120.7(4) . . ?
N6 C25 C26 123.0(5) . . ?
N6 C25 H25 118.5 . . ?
C26 C25 H25 118.5 . . ?
C27 C26 C25 119.0(5) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C26 C27 C28 120.4(5) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C28 C24 116.9(4) . . ?
C27 C28 C29 123.4(4) . . ?
C24 C28 C29 119.7(4) . . ?
N8 C29 C30 122.3(5) . . ?
N8 C29 C28 118.5(4) . . ?
C30 C29 C28 119.2(4) . . ?
N7 C30 C29 121.4(4) . . ?
N7 C30 C22 118.5(4) . . ?
C29 C30 C22 120.2(4) . . ?
N7 C31 C36 119.7(5) . . ?
N7 C31 C32 121.2(5) . . ?
C36 C31 C32 119.0(5) . . ?
N8 C32 C33 119.0(5) . . ?
N8 C32 C31 121.1(5) . . ?
C33 C32 C31 119.9(5) . . ?
C34 C33 C32 119.0(6) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 120.7(6) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C36 C35 C34 122.0(6) . . ?
C36 C35 H35 119.0 . . ?
C34 C35 H35 119.0 . . ?
C35 C36 C31 119.1(6) . . ?
C35 C36 H36 120.5 . . ?
C31 C36 H36 120.5 . . ?
N9 C37 C38 123.8(5) . . ?
N9 C37 H37 118.1 . . ?
C38 C37 H37 118.1 . . ?
C39 C38 C37 118.6(5) . . ?
C39 C38 H38 120.7 . . ?
C37 C38 H38 120.7 . . ?
C38 C39 C40 119.5(5) . . ?
C38 C39 H39 120.2 . . ?
C40 C39 H39 120.2 . . ?
C39 C40 C41 118.6(5) . . ?
C39 C40 C48 122.5(5) . . ?
C41 C40 C48 118.8(5) . . ?
N9 C41 C40 122.4(5) . . ?
N9 C41 C42 116.0(5) . . ?
C40 C41 C42 121.6(5) . . ?
N10 C42 C46 123.2(5) . . ?
N10 C42 C41 116.7(4) . . ?
C46 C42 C41 120.1(5) . . ?
N10 C43 C44 121.2(6) . . ?
N10 C43 H43 119.4 . . ?
C44 C43 H43 119.4 . . ?
C45 C44 C43 119.8(6) . . ?
C45 C44 H44 120.1 . . ?
C43 C44 H44 120.1 . . ?
C44 C45 C46 120.2(6) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C45 C46 C42 117.2(6) . . ?
C45 C46 C47 123.2(5) . . ?
C42 C46 C47 119.6(5) . . ?
N12 C47 C48 121.9(6) . . ?
N12 C47 C46 118.2(6) . . ?
C48 C47 C46 119.9(5) . . ?
N11 C48 C47 122.3(5) . . ?
N11 C48 C40 118.4(6) . . ?
C47 C48 C40 119.3(5) . . ?
N11 C49 C50 122.1(7) . . ?
N11 C49 C54 119.8(8) . . ?
C50 C49 C54 118.0(7) . . ?
N12 C50 C49 121.1(6) . . ?
N12 C50 C51 117.6(8) . . ?
C49 C50 C51 121.3(8) . . ?
C52 C51 C50 118.1(9) . . ?
C52 C51 H51 121.0 . . ?
C50 C51 H51 121.0 . . ?
C51 C52 C53 121.8(9) . . ?
C51 C52 H52 119.1 . . ?
C53 C52 H52 119.1 . . ?
C52 C53 C54 121.9(10) . . ?
C52 C53 H53 119.0 . . ?
C54 C53 H53 119.0 . . ?
C53 C54 C49 118.8(9) . . ?
C53 C54 H54 120.6 . . ?
C49 C54 H54 120.6 . . ?
O2 C55 O1 125.7(5) . . ?
O2 C55 C56 118.2(5) . . ?
O1 C55 C56 116.1(5) . . ?
C61 C56 C57 119.5(4) . . ?
C61 C56 C55 120.4(5) . . ?
C57 C56 C55 120.1(5) . . ?
C58 C57 C56 120.0(5) . . ?
C58 C57 H57 120.0 . . ?
C56 C57 H57 120.0 . . ?
C59 C58 C57 120.1(4) . . ?
C59 C58 C62 117.5(4) . . ?
C57 C58 C62 122.4(5) . . ?
C58 C59 C60 120.5(5) . . ?
C58 C59 H59 119.7 . . ?
C60 C59 H59 119.7 . . ?
C61 C60 C59 119.8(5) . . ?
C61 C60 O5 118.3(4) . . ?
C59 C60 O5 121.9(5) . . ?
C60 C61 C56 120.1(4) . . ?
C60 C61 H61 119.9 . . ?
C56 C61 H61 119.9 . . ?
O3 C62 O4 120.7(4) . . ?
O3 C62 C58 120.7(4) . . ?
O4 C62 C58 118.6(5) . . ?
C64 C63 C68 121.8(5) . . ?
C64 C63 O5 120.6(5) . . ?
C68 C63 O5 117.5(5) . . ?
C63 C64 C65 118.0(5) . . ?
C63 C64 H64 121.0 . . ?
C65 C64 H64 121.0 . . ?
C66 C65 C64 121.5(5) . . ?
C66 C65 H65 119.3 . . ?
C64 C65 H65 119.3 . . ?
C65 C66 C67 118.7(4) . . ?
C65 C66 C69 121.8(4) . . ?
C67 C66 C69 119.5(5) . . ?
C68 C67 C66 120.5(5) . . ?
C68 C67 H67 119.8 . . ?
C66 C67 H67 119.8 . . ?
C63 C68 C67 119.4(5) . . ?
C63 C68 H68 120.3 . . ?
C67 C68 H68 120.3 . . ?
O6 C69 O7 127.0(5) . . ?
O6 C69 C66 115.8(5) . . ?
O7 C69 C66 117.2(4) . . ?
O9 C70 O8 120.7(4) . . ?
O9 C70 C71 120.2(5) . . ?
O8 C70 C71 119.0(5) . . ?
C72 C71 C76 121.0(4) . . ?
C72 C71 C70 119.9(5) . . ?
C76 C71 C70 119.2(5) . . ?
C71 C72 C73 120.0(5) . . ?
C71 C72 H72 120.0 . . ?
C73 C72 H72 120.0 . . ?
C74 C73 C72 119.3(5) . . ?
C74 C73 C77 120.5(4) . . ?
C72 C73 C77 120.2(5) . . ?
C73 C74 C75 120.2(4) . . ?
C73 C74 H74 119.9 . . ?
C75 C74 H74 119.9 . . ?
C74 C75 O12 122.3(4) . . ?
C74 C75 C76 121.2(5) . . ?
O12 C75 C76 116.4(5) . . ?
C71 C76 C75 118.3(5) . . ?
C71 C76 H76 120.9 . . ?
C75 C76 H76 120.9 . . ?
O11 C77 O10 125.0(5) . . ?
O11 C77 C73 117.9(4) . . ?
O10 C77 C73 117.2(5) . . ?
C83 C78 C79 120.4(4) . . ?
C83 C78 O12 116.3(4) . . ?
C79 C78 O12 123.2(4) . . ?
C80 C79 C78 119.7(5) . . ?
C80 C79 H79 120.1 . . ?
C78 C79 H79 120.1 . . ?
C79 C80 C81 121.0(5) . . ?
C79 C80 H80 119.5 . . ?
C81 C80 H80 119.5 . . ?
C80 C81 C82 118.4(4) . . ?
C80 C81 C84 121.1(4) . . ?
C82 C81 C84 120.4(4) . . ?
C83 C82 C81 121.0(4) . . ?
C83 C82 H82 119.5 . . ?
C81 C82 H82 119.5 . . ?
C78 C83 C82 119.4(5) . . ?
C78 C83 H83 120.3 . . ?
C82 C83 H83 120.3 . . ?
O13 C84 O14 124.3(4) . . ?
O13 C84 C81 116.6(5) . . ?
O14 C84 C81 119.0(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 0.4(7) . . . . ?
Ni1 N1 C1 C2 175.4(4) . . . . ?
N1 C1 C2 C3 -1.6(8) . . . . ?
C1 C2 C3 C4 0.1(8) . . . . ?
C2 C3 C4 C5 2.4(8) . . . . ?
C2 C3 C4 C12 -177.1(5) . . . . ?
C1 N1 C5 C4 2.4(7) . . . . ?
Ni1 N1 C5 C4 -173.4(4) . . . . ?
C1 N1 C5 C6 -176.3(4) . . . . ?
Ni1 N1 C5 C6 7.9(5) . . . . ?
C3 C4 C5 N1 -3.8(7) . . . . ?
C12 C4 C5 N1 175.8(4) . . . . ?
C3 C4 C5 C6 174.8(5) . . . . ?
C12 C4 C5 C6 -5.6(7) . . . . ?
C7 N2 C6 C10 -3.5(7) . . . . ?
Ni1 N2 C6 C10 171.5(4) . . . . ?
C7 N2 C6 C5 174.6(5) . . . . ?
Ni1 N2 C6 C5 -10.4(5) . . . . ?
N1 C5 C6 N2 1.7(6) . . . . ?
C4 C5 C6 N2 -177.0(4) . . . . ?
N1 C5 C6 C10 179.8(5) . . . . ?
C4 C5 C6 C10 1.1(7) . . . . ?
C6 N2 C7 C8 0.8(8) . . . . ?
Ni1 N2 C7 C8 -173.3(4) . . . . ?
N2 C7 C8 C9 2.6(9) . . . . ?
C7 C8 C9 C10 -3.4(8) . . . . ?
N2 C6 C10 C9 2.7(8) . . . . ?
C5 C6 C10 C9 -175.3(5) . . . . ?
N2 C6 C10 C11 -176.7(4) . . . . ?
C5 C6 C10 C11 5.3(7) . . . . ?
C8 C9 C10 C6 0.9(8) . . . . ?
C8 C9 C10 C11 -179.8(5) . . . . ?
C14 N4 C11 C12 1.8(7) . . . . ?
C14 N4 C11 C10 -178.4(4) . . . . ?
C6 C10 C11 N4 173.2(5) . . . . ?
C9 C10 C11 N4 -6.1(8) . . . . ?
C6 C10 C11 C12 -7.1(7) . . . . ?
C9 C10 C11 C12 173.6(5) . . . . ?
C13 N3 C12 C11 -1.2(7) . . . . ?
C13 N3 C12 C4 176.6(4) . . . . ?
N4 C11 C12 N3 0.0(8) . . . . ?
C10 C11 C12 N3 -179.8(5) . . . . ?
N4 C11 C12 C4 -177.8(5) . . . . ?
C10 C11 C12 C4 2.5(7) . . . . ?
C3 C4 C12 N3 5.4(8) . . . . ?
C5 C4 C12 N3 -174.1(4) . . . . ?
C3 C4 C12 C11 -176.7(5) . . . . ?
C5 C4 C12 C11 3.8(7) . . . . ?
C12 N3 C13 C14 0.5(8) . . . . ?
C12 N3 C13 C18 -178.2(5) . . . . ?
C11 N4 C14 C13 -2.5(8) . . . . ?
C11 N4 C14 C15 177.4(5) . . . . ?
N3 C13 C14 N4 1.4(8) . . . . ?
C18 C13 C14 N4 -179.9(5) . . . . ?
N3 C13 C14 C15 -178.5(5) . . . . ?
C18 C13 C14 C15 0.2(8) . . . . ?
N4 C14 C15 C16 -177.7(5) . . . . ?
C13 C14 C15 C16 2.1(9) . . . . ?
C14 C15 C16 C17 -3.3(9) . . . . ?
C15 C16 C17 C18 2.1(10) . . . . ?
C16 C17 C18 C13 0.3(10) . . . . ?
N3 C13 C18 C17 177.3(6) . . . . ?
C14 C13 C18 C17 -1.4(9) . . . . ?
C23 N5 C19 C20 -1.6(7) . . . . ?
Ni2 N5 C19 C20 -178.8(4) . . . . ?
N5 C19 C20 C21 0.1(8) . . . . ?
C19 C20 C21 C22 1.3(8) . . . . ?
C20 C21 C22 C23 -1.2(7) . . . . ?
C20 C21 C22 C30 176.8(5) . . . . ?
C19 N5 C23 C22 1.7(7) . . . . ?
Ni2 N5 C23 C22 179.3(4) . . . . ?
C19 N5 C23 C24 -175.6(4) . . . . ?
Ni2 N5 C23 C24 1.9(5) . . . . ?
C21 C22 C23 N5 -0.4(7) . . . . ?
C30 C22 C23 N5 -178.4(4) . . . . ?
C21 C22 C23 C24 176.9(4) . . . . ?
C30 C22 C23 C24 -1.1(7) . . . . ?
C25 N6 C24 C28 0.3(7) . . . . ?
Ni2 N6 C24 C28 -173.3(4) . . . . ?
C25 N6 C24 C23 177.3(4) . . . . ?
Ni2 N6 C24 C23 3.7(5) . . . . ?
N5 C23 C24 N6 -3.8(6) . . . . ?
C22 C23 C24 N6 178.8(4) . . . . ?
N5 C23 C24 C28 173.3(4) . . . . ?
C22 C23 C24 C28 -4.1(7) . . . . ?
C24 N6 C25 C26 -1.7(8) . . . . ?
Ni2 N6 C25 C26 170.8(4) . . . . ?
N6 C25 C26 C27 1.9(9) . . . . ?
C25 C26 C27 C28 -0.7(8) . . . . ?
C26 C27 C28 C24 -0.6(7) . . . . ?
C26 C27 C28 C29 179.3(5) . . . . ?
N6 C24 C28 C27 0.8(7) . . . . ?
C23 C24 C28 C27 -176.1(4) . . . . ?
N6 C24 C28 C29 -179.0(4) . . . . ?
C23 C24 C28 C29 4.1(7) . . . . ?
C32 N8 C29 C30 3.2(7) . . . . ?
C32 N8 C29 C28 -175.8(4) . . . . ?
C27 C28 C29 N8 0.4(7) . . . . ?
C24 C28 C29 N8 -179.7(4) . . . . ?
C27 C28 C29 C30 -178.6(4) . . . . ?
C24 C28 C29 C30 1.2(7) . . . . ?
C31 N7 C30 C29 1.4(7) . . . . ?
C31 N7 C30 C22 -177.9(5) . . . . ?
N8 C29 C30 N7 -4.8(8) . . . . ?
C28 C29 C30 N7 174.2(5) . . . . ?
N8 C29 C30 C22 174.5(5) . . . . ?
C28 C29 C30 C22 -6.5(7) . . . . ?
C23 C22 C30 N7 -174.2(5) . . . . ?
C21 C22 C30 N7 7.8(7) . . . . ?
C23 C22 C30 C29 6.4(7) . . . . ?
C21 C22 C30 C29 -171.5(4) . . . . ?
C30 N7 C31 C36 -174.5(5) . . . . ?
C30 N7 C31 C32 3.0(7) . . . . ?
C29 N8 C32 C33 179.5(5) . . . . ?
C29 N8 C32 C31 1.2(7) . . . . ?
N7 C31 C32 N8 -4.5(8) . . . . ?
C36 C31 C32 N8 173.0(5) . . . . ?
N7 C31 C32 C33 177.2(5) . . . . ?
C36 C31 C32 C33 -5.3(8) . . . . ?
N8 C32 C33 C34 -173.7(5) . . . . ?
C31 C32 C33 C34 4.6(9) . . . . ?
C32 C33 C34 C35 0.1(10) . . . . ?
C33 C34 C35 C36 -4.2(10) . . . . ?
C34 C35 C36 C31 3.4(10) . . . . ?
N7 C31 C36 C35 178.9(6) . . . . ?
C32 C31 C36 C35 1.3(9) . . . . ?
C41 N9 C37 C38 1.4(8) . . . . ?
Ni3 N9 C37 C38 -171.7(4) . . . . ?
N9 C37 C38 C39 -1.8(9) . . . . ?
C37 C38 C39 C40 1.0(9) . . . . ?
C38 C39 C40 C41 0.2(8) . . . . ?
C38 C39 C40 C48 -176.2(5) . . . . ?
C37 N9 C41 C40 -0.1(7) . . . . ?
Ni3 N9 C41 C40 173.9(4) . . . . ?
C37 N9 C41 C42 -177.7(4) . . . . ?
Ni3 N9 C41 C42 -3.7(6) . . . . ?
C39 C40 C41 N9 -0.6(8) . . . . ?
C48 C40 C41 N9 175.9(5) . . . . ?
C39 C40 C41 C42 176.8(5) . . . . ?
C48 C40 C41 C42 -6.7(8) . . . . ?
C43 N10 C42 C46 -1.0(8) . . . . ?
Ni3 N10 C42 C46 177.5(4) . . . . ?
C43 N10 C42 C41 178.5(5) . . . . ?
Ni3 N10 C42 C41 -3.0(6) . . . . ?
N9 C41 C42 N10 4.5(7) . . . . ?
C40 C41 C42 N10 -173.1(5) . . . . ?
N9 C41 C42 C46 -176.0(5) . . . . ?
C40 C41 C42 C46 6.4(8) . . . . ?
C42 N10 C43 C44 1.6(9) . . . . ?
Ni3 N10 C43 C44 -176.6(5) . . . . ?
N10 C43 C44 C45 -1.6(12) . . . . ?
C43 C44 C45 C46 0.8(13) . . . . ?
C44 C45 C46 C42 -0.2(11) . . . . ?
C44 C45 C46 C47 -179.9(7) . . . . ?
N10 C42 C46 C45 0.3(9) . . . . ?
C41 C42 C46 C45 -179.2(5) . . . . ?
N10 C42 C46 C47 -180.0(5) . . . . ?
C41 C42 C46 C47 0.6(8) . . . . ?
C50 N12 C47 C48 1.0(9) . . . . ?
C50 N12 C47 C46 -179.1(6) . . . . ?
C45 C46 C47 N12 -7.2(9) . . . . ?
C42 C46 C47 N12 173.1(5) . . . . ?
C45 C46 C47 C48 172.7(6) . . . . ?
C42 C46 C47 C48 -7.0(9) . . . . ?
C49 N11 C48 C47 -4.2(8) . . . . ?
C49 N11 C48 C40 173.2(5) . . . . ?
N12 C47 C48 N11 3.9(9) . . . . ?
C46 C47 C48 N11 -176.0(5) . . . . ?
N12 C47 C48 C40 -173.5(5) . . . . ?
C46 C47 C48 C40 6.6(8) . . . . ?
C39 C40 C48 N11 -1.0(8) . . . . ?
C41 C40 C48 N11 -177.3(5) . . . . ?
C39 C40 C48 C47 176.5(5) . . . . ?
C41 C40 C48 C47 0.1(8) . . . . ?
C48 N11 C49 C50 -0.1(9) . . . . ?
C48 N11 C49 C54 -176.6(6) . . . . ?
C47 N12 C50 C49 -5.1(10) . . . . ?
C47 N12 C50 C51 175.1(6) . . . . ?
N11 C49 C50 N12 5.0(10) . . . . ?
C54 C49 C50 N12 -178.5(6) . . . . ?
N11 C49 C50 C51 -175.3(6) . . . . ?
C54 C49 C50 C51 1.3(11) . . . . ?
N12 C50 C51 C52 178.6(7) . . . . ?
C49 C50 C51 C52 -1.2(12) . . . . ?
C50 C51 C52 C53 0.2(15) . . . . ?
C51 C52 C53 C54 0.6(16) . . . . ?
C52 C53 C54 C49 -0.4(14) . . . . ?
N11 C49 C54 C53 176.2(7) . . . . ?
C50 C49 C54 C53 -0.5(11) . . . . ?
Ni1 O1 C55 O2 1.3(8) . . . . ?
Ni1 O1 C55 C56 -178.7(3) . . . . ?
O2 C55 C56 C61 -172.9(5) . . . . ?
O1 C55 C56 C61 7.1(7) . . . . ?
O2 C55 C56 C57 8.8(8) . . . . ?
O1 C55 C56 C57 -171.2(4) . . . . ?
C61 C56 C57 C58 -2.0(7) . . . . ?
C55 C56 C57 C58 176.3(4) . . . . ?
C56 C57 C58 C59 2.6(7) . . . . ?
C56 C57 C58 C62 -177.9(4) . . . . ?
C57 C58 C59 C60 -0.5(8) . . . . ?
C62 C58 C59 C60 180.0(4) . . . . ?
C58 C59 C60 C61 -2.2(8) . . . . ?
C58 C59 C60 O5 177.9(5) . . . . ?
C63 O5 C60 C61 -154.4(5) . . . . ?
C63 O5 C60 C59 25.5(7) . . . . ?
C59 C60 C61 C56 2.8(8) . . . . ?
O5 C60 C61 C56 -177.2(4) . . . . ?
C57 C56 C61 C60 -0.7(7) . . . . ?
C55 C56 C61 C60 -179.0(5) . . . . ?
Ni2 O3 C62 O4 1.7(5) 4_566 . . . ?
Ni2 O3 C62 C58 -177.1(4) 4_566 . . . ?
Ni2 O4 C62 O3 -1.8(5) 4_566 . . . ?
Ni2 O4 C62 C58 177.1(4) 4_566 . . . ?
C59 C58 C62 O3 164.6(5) . . . . ?
C57 C58 C62 O3 -14.9(7) . . . . ?
C59 C58 C62 O4 -14.2(7) . . . . ?
C57 C58 C62 O4 166.3(5) . . . . ?
C60 O5 C63 C64 -107.6(6) . . . . ?
C60 O5 C63 C68 69.8(6) . . . . ?
C68 C63 C64 C65 -2.0(8) . . . . ?
O5 C63 C64 C65 175.3(5) . . . . ?
C63 C64 C65 C66 -0.9(8) . . . . ?
C64 C65 C66 C67 3.2(8) . . . . ?
C64 C65 C66 C69 -175.3(5) . . . . ?
C65 C66 C67 C68 -2.5(8) . . . . ?
C69 C66 C67 C68 176.0(5) . . . . ?
C64 C63 C68 C67 2.7(9) . . . . ?
O5 C63 C68 C67 -174.8(5) . . . . ?
C66 C67 C68 C63 -0.3(9) . . . . ?
Ni2 O7 C69 O6 -3.8(9) . . . . ?
Ni2 O7 C69 C66 176.8(3) . . . . ?
C65 C66 C69 O6 178.7(5) . . . . ?
C67 C66 C69 O6 0.2(8) . . . . ?
C65 C66 C69 O7 -1.9(8) . . . . ?
C67 C66 C69 O7 179.6(5) . . . . ?
Ni1 O9 C70 O8 -0.5(4) . . . . ?
Ni1 O9 C70 C71 176.4(4) . . . . ?
Ni1 O8 C70 O9 0.6(4) . . . . ?
Ni1 O8 C70 C71 -176.5(3) . . . . ?
O9 C70 C71 C72 1.9(6) . . . . ?
O8 C70 C71 C72 179.0(4) . . . . ?
O9 C70 C71 C76 -177.4(4) . . . . ?
O8 C70 C71 C76 -0.4(6) . . . . ?
C76 C71 C72 C73 2.4(7) . . . . ?
C70 C71 C72 C73 -176.9(4) . . . . ?
C71 C72 C73 C74 -1.0(7) . . . . ?
C71 C72 C73 C77 178.3(4) . . . . ?
C72 C73 C74 C75 -0.5(7) . . . . ?
C77 C73 C74 C75 -179.9(4) . . . . ?
C73 C74 C75 O12 177.0(4) . . . . ?
C73 C74 C75 C76 0.7(7) . . . . ?
C78 O12 C75 C74 52.2(6) . . . . ?
C78 O12 C75 C76 -131.3(4) . . . . ?
C72 C71 C76 C75 -2.2(7) . . . . ?
C70 C71 C76 C75 177.1(4) . . . . ?
C74 C75 C76 C71 0.7(7) . . . . ?
O12 C75 C76 C71 -175.9(4) . . . . ?
Ni3 O10 C77 O11 -7.5(8) . . . . ?
Ni3 O10 C77 C73 173.4(3) . . . . ?
C74 C73 C77 O11 179.1(5) . . . . ?
C72 C73 C77 O11 -0.2(7) . . . . ?
C74 C73 C77 O10 -1.7(7) . . . . ?
C72 C73 C77 O10 178.9(4) . . . . ?
C75 O12 C78 C83 -150.5(4) . . . . ?
C75 O12 C78 C79 33.0(7) . . . . ?
C83 C78 C79 C80 2.5(8) . . . . ?
O12 C78 C79 C80 178.9(4) . . . . ?
C78 C79 C80 C81 -0.5(8) . . . . ?
C79 C80 C81 C82 -2.0(7) . . . . ?
C79 C80 C81 C84 176.5(4) . . . . ?
C80 C81 C82 C83 2.4(7) . . . . ?
C84 C81 C82 C83 -176.0(4) . . . . ?
C79 C78 C83 C82 -2.1(7) . . . . ?
O12 C78 C83 C82 -178.7(4) . . . . ?
C81 C82 C83 C78 -0.4(7) . . . . ?
Ni3 O13 C84 O14 -7.5(7) 4_566 . . . ?
Ni3 O13 C84 C81 172.6(3) 4_566 . . . ?
Ni2 O14 C84 O13 111.4(5) 1_455 . . . ?
Ni2 O14 C84 C81 -68.7(4) 1_455 . . . ?
C80 C81 C84 O13 159.8(4) . . . . ?
C82 C81 C84 O13 -21.8(6) . . . . ?
C80 C81 C84 O14 -20.1(6) . . . . ?
C82 C81 C84 O14 158.3(4) . . . . ?

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
O1W H1A O8 0.86 2.17 2.960(5) 153 3_566
O1W H1B O2 0.86 1.75 2.562(5) 157 .
O2W H2A O3 0.86 2.06 2.717(5) 133 1_454
O2W H2B O6 0.86 1.77 2.625(5) 174 4_465
O3W H3A O11 0.86 1.79 2.595(5) 155 .
O3W H3B O14 0.86 1.98 2.819(4) 164 4_565

_refine_diff_density_max         0.670
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.082




