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

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

data_www
_database_code_depnum_ccdc_archive 'CCDC 1434742'
_audit_update_record             
;
2016-01-29 deposited with the CCDC.
2016-02-09 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         'C67 H38 N11 O26 Zn4, 9(H2 O)'
_chemical_formula_sum            'C67 H56 N11 O35 Zn4'
_chemical_formula_weight         1836.70

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'
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'
H H 0.0000 0.0000 '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                   25.151(3)
_cell_length_b                   10.4057(13)
_cell_length_c                   30.589(5)
_cell_angle_alpha                90
_cell_angle_beta                 113.035(2)
_cell_angle_gamma                90
_cell_volume                     7367.2(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2176
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      22.01
_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_F_000             3740
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.390
_shelx_estimated_absorpt_T_min   0.681
_shelx_estimated_absorpt_T_max   0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27887
_diffrn_reflns_av_unetI/netI     0.1035
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.447
_diffrn_reflns_theta_max         25.678
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6995
_reflns_number_gt                3922
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.1510P)²+0.5363P] 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         6995
_refine_ls_number_parameters     651
_refine_ls_number_restraints     1210
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0849
_refine_ls_wR_factor_ref         0.2560
_refine_ls_wR_factor_gt          0.2300
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.021
_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 0.25698(4) 0.53664(9) -0.01051(3) 0.0332(3) Uani 1 1 d . U . . .
Zn2 Zn 0.19773(4) 0.29206(9) 0.01146(3) 0.0327(3) Uani 1 1 d . U . . .
O1 O 0.1841(3) 0.4768(6) 0.0377(2) 0.0499(15) Uani 1 1 d . U . . .
O2 O 0.2494(3) 0.6296(6) 0.04312(19) 0.0463(14) Uani 1 1 d . U . . .
O3 O 0.1225(6) 0.3953(14) 0.1636(4) 0.165(5) Uani 1 1 d D U . . .
O4 O 0.1751(8) 0.4502(13) 0.2362(4) 0.194(6) Uani 1 1 d D U . . .
O5 O 0.2306(2) 0.2291(6) 0.08078(19) 0.0428(13) Uani 1 1 d . U . . .
O6 O 0.3078(2) 0.3575(6) 0.11160(18) 0.0468(15) Uani 1 1 d . U . . .
O7 O 0.1437(9) 0.012(2) 0.1712(6) 0.272(10) Uani 1 1 d D U . . .
O8 O 0.1588(7) 0.0636(17) 0.2416(5) 0.208(7) Uani 1 1 d D U . . .
O9 O -0.0483(13) 0.273(3) -0.1630(7) 0.209(12) Uani 0.494(11) 1 d D U P . .
O9' O 0.0350(17) 0.705(4) -0.2826(13) 0.300(17) Uani 0.506(11) 1 d D U P . .
O10 O -0.0546(10) 0.213(2) -0.2301(8) 0.134(7) Uani 0.494(11) 1 d D U P . .
O10' O 0.1150(16) 0.708(4) -0.2327(14) 0.306(18) Uani 0.506(11) 1 d D U P . .
O11 O 0.1541(2) 0.3662(6) -0.05856(19) 0.0429(13) Uani 1 1 d . U . . .
O12 O 0.1950(2) 0.5439(6) -0.07321(18) 0.0418(13) Uani 1 1 d . U . . .
O13 O 0.27735(19) 0.3661(5) 0.01597(16) 0.0294(11) Uani 1 1 d . U . . .
H13 H 0.3034 0.3744 0.0503 0.035 Uiso 1 1 calc R U . . .
C1 C 0.2163(4) 0.5686(9) 0.0583(3) 0.049(2) Uani 1 1 d . U . . .
C2 C 0.2175(5) 0.6073(9) 0.1066(3) 0.059(2) Uani 1 1 d . U . . .
C3 C 0.2479(5) 0.7096(10) 0.1309(3) 0.068(3) Uani 1 1 d . U . . .
H3 H 0.2676 0.7636 0.1170 0.081 Uiso 1 1 calc R U . . .
C4 C 0.2503(6) 0.7360(12) 0.1765(4) 0.078(3) Uani 1 1 d . U . . .
H4 H 0.2718 0.8085 0.1929 0.093 Uiso 1 1 calc R U . . .
C5 C 0.2249(6) 0.6670(12) 0.1972(4) 0.084(3) Uani 1 1 d . U . . .
C6 C 0.1918(6) 0.5559(12) 0.1719(5) 0.093(4) Uani 1 1 d D U . . .
C7 C 0.1868(5) 0.5296(10) 0.1262(4) 0.076(3) Uani 1 1 d . U . . .
H7 H 0.1633 0.4609 0.1086 0.091 Uiso 1 1 calc R U . . .
C8 C 0.2701(4) 0.2829(8) 0.1145(3) 0.0391(19) Uani 1 1 d . U . . .
C9 C 0.2723(4) 0.2542(10) 0.1633(3) 0.053(2) Uani 1 1 d . U . . .
C10 C 0.3150(5) 0.2973(12) 0.2031(3) 0.076(3) Uani 1 1 d . U . . .
H10 H 0.3445 0.3497 0.2004 0.091 Uiso 1 1 calc R U . . .
C11 C 0.3171(6) 0.2667(12) 0.2483(4) 0.087(4) Uani 1 1 d . U . . .
H11 H 0.3485 0.2961 0.2757 0.105 Uiso 1 1 calc R U . . .
C12 C 0.2737(6) 0.1939(11) 0.2534(4) 0.080(3) Uani 1 1 d . U . . .
C13 C 0.2278(6) 0.1534(12) 0.2116(5) 0.090(3) Uani 1 1 d D U . . .
C14 C 0.2295(5) 0.1796(11) 0.1685(4) 0.073(3) Uani 1 1 d . U . . .
H14 H 0.2001 0.1452 0.1408 0.087 Uiso 1 1 calc R U . . .
C15 C 0.1572(3) 0.4558(9) -0.0837(3) 0.0401(18) Uani 1 1 d . U . . .
C16 C 0.1123(4) 0.4576(9) -0.1329(3) 0.053(2) Uani 1 1 d . U . . .
C17 C 0.1135(6) 0.5322(14) -0.1683(4) 0.100(4) Uani 1 1 d . U . . .
H17 H 0.1455 0.5881 -0.1617 0.120 Uiso 1 1 calc R U . . .
C18 C 0.0697(7) 0.5327(16) -0.2150(5) 0.118(5) Uani 1 1 d D U . . .
C19 C 0.0238(5) 0.4528(12) -0.2246(4) 0.083(3) Uani 1 1 d . U . . .
C20 C 0.0214(6) 0.3731(17) -0.1902(6) 0.133(5) Uani 1 1 d D U . . .
C21 C 0.0663(6) 0.3741(16) -0.1469(5) 0.129(5) Uani 1 1 d . U . . .
H21 H 0.0663 0.3120 -0.1241 0.155 Uiso 1 1 d R U . . .
C22 C -0.1333(12) 0.175(3) 0.0191(10) 0.037(5) Uani 0.5 1 d . U P A 1
H22A H -0.1424 0.2005 0.0455 0.044 Uiso 0.5 1 d R U P A 1
C23 C -0.1487(9) 0.057(2) -0.0480(7) 0.037(4) Uani 0.5 1 d D U P A 1
H23A H -0.1710 -0.0048 -0.0712 0.044 Uiso 0.5 1 d R U P A 1
C22' C 0.3541(13) 0.712(3) 0.0147(12) 0.047(6) Uani 0.5 1 d . U P B 2
H22B H 0.3442 0.7288 0.0414 0.056 Uiso 0.5 1 d R U P B 2
C23' C 0.3369(10) 0.604(2) -0.0536(8) 0.041(5) Uani 0.5 1 d . U P B 2
H23B H 0.3113 0.5504 -0.0783 0.049 Uiso 0.5 1 d R U P B 2
C27' C 0.4500(9) 0.855(2) -0.0416(9) 0.069(5) Uani 0.5 1 d . U P B 2
C28' C 0.4959(10) 0.907(2) -0.0066(9) 0.076(5) Uani 0.5 1 d . U P B 2
H28' H 0.5011 0.8897 0.0253 0.091 Uiso 0.5 1 d R U P B 2
C29' C 0.5331(10) 0.989(2) -0.0161(10) 0.082(6) Uani 0.5 1 d . U P B 2
H29' H 0.5651 1.0252 0.0092 0.099 Uiso 0.5 1 d R U P B 2
N1 N 0.1136(11) 0.2453(17) 0.0040(11) 0.046(4) Uani 0.5 1 d . U P A 1
C29 C 0.0971(8) 0.2603(15) 0.0396(8) 0.040(3) Uani 0.5 1 d . U P A 1
H29A H 0.1257 0.2933 0.0685 0.048 Uiso 0.5 1 d R U P A 1
C30 C 0.0731(8) 0.2024(15) -0.0376(7) 0.045(4) Uani 0.5 1 d . U P A 1
H30A H 0.0827 0.1934 -0.0649 0.054 Uiso 0.5 1 d R U P A 1
C30' C 0.4834(10) 0.953(2) -0.0976(10) 0.090(6) Uani 0.5 1 d . U P B 2
H30' H 0.4792 0.9646 -0.1296 0.108 Uiso 0.5 1 d R U P B 2
C31' C 0.4467(10) 0.869(2) -0.0874(9) 0.082(6) Uani 0.5 1 d . U P B 2
H31' H 0.4167 0.8286 -0.1133 0.098 Uiso 0.5 1 d R U P B 2
C24 C -0.0796(7) 0.2120(17) 0.0221(6) 0.036(3) Uani 0.5 1 d . U P A 1
H24A H -0.0567 0.2698 0.0467 0.043 Uiso 0.5 1 d R U P A 1
C25 C -0.0949(6) 0.0861(15) -0.0461(5) 0.030(3) Uani 0.5 1 d . U P A 1
H25A H -0.0830 0.0551 -0.0704 0.036 Uiso 0.5 1 d R U P A 1
C26 C -0.0587(6) 0.1615(14) -0.0099(5) 0.029(3) Uani 0.5 1 d . U P A 1
C27 C 0.0010(7) 0.1868(13) -0.0058(5) 0.036(3) Uani 0.5 1 d . U P A 1
C28 C 0.0439(6) 0.2326(13) 0.0375(5) 0.037(3) Uani 0.5 1 d . U P A 1
H28A H 0.0345 0.2439 0.0648 0.044 Uiso 0.5 1 d R U P A 1
C31 C 0.0190(7) 0.1742(13) -0.0416(5) 0.041(3) Uani 0.5 1 d . U P A 1
H31A H -0.0083 0.1458 -0.0720 0.050 Uiso 0.5 1 d R U P A 1
C24' C 0.3953(8) 0.7889(19) 0.0072(7) 0.055(4) Uani 0.5 1 d . U P B 2
H24B H 0.4150 0.8559 0.0292 0.066 Uiso 0.5 1 d R U P B 2
C25' C 0.3785(9) 0.666(2) -0.0619(8) 0.064(5) Uani 0.5 1 d . U P B 2
H25B H 0.3891 0.6405 -0.0875 0.077 Uiso 0.5 1 d R U P B 2
C26' C 0.4077(8) 0.7689(19) -0.0321(7) 0.056(4) Uani 0.5 1 d . U P B 2
N1A N 0.1173(11) 0.2062(17) 0.0047(10) 0.034(3) Uani 0.5 1 d . U P A 3
C29A C 0.0983(9) 0.1955(18) 0.0415(8) 0.049(4) Uani 0.5 1 d . U P A 3
H29B H 0.1170 0.2460 0.0692 0.059 Uiso 0.5 1 calc R U P A 3
C30A C 0.0870(7) 0.1344(15) -0.0332(7) 0.043(4) Uani 0.5 1 d . U P A 3
H30B H 0.0970 0.1391 -0.0601 0.051 Uiso 0.5 1 calc R U P A 3
C27A C 0.0229(6) 0.0401(15) 0.0009(6) 0.043(4) Uani 0.5 1 d . U P A 3
C28A C 0.0542(7) 0.1164(16) 0.0402(6) 0.052(4) Uani 0.5 1 d . U P A 3
H28B H 0.0445 0.1131 0.0673 0.063 Uiso 0.5 1 calc R U P A 3
C31A C 0.0404(6) 0.0510(16) -0.0361(6) 0.053(4) Uani 0.5 1 d . U P A 3
H31B H 0.0212 0.0023 -0.0642 0.063 Uiso 0.5 1 calc R U P A 3
N1' N 0.5258(9) 1.010(2) -0.0621(9) 0.090(5) Uani 0.5 1 d . U P . .
N2 N -0.1669(9) 0.111(3) -0.0150(9) 0.027(4) Uani 0.5 1 d D U P . .
N2' N 0.3200(11) 0.615(4) -0.0163(11) 0.040(5) Uani 0.5 1 d . U P . .
N3 N 0.1633(7) 0.4688(14) 0.1915(5) 0.144(5) Uani 1 1 d D U . . .
N4 N 0.1805(6) 0.0792(13) 0.2096(5) 0.125(4) Uani 1 1 d D U . . .
N5 N -0.0256(8) 0.287(2) -0.1943(8) 0.139(8) Uani 0.494(11) 1 d D U P . .
N5' N 0.0689(14) 0.642(2) -0.2448(9) 0.202(11) Uani 0.506(11) 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N2' 1.85(3) . ?
Zn1 O13 1.935(5) . ?
Zn1 O12 1.943(5) . ?
Zn1 O2 1.976(5) . ?
Zn1 N2 2.117(17) 3 ?
Zn2 O13 2.053(5) 7 ?
Zn2 O5 2.058(5) . ?
Zn2 N1 2.09(3) . ?
Zn2 O13 2.099(5) . ?
Zn2 O11 2.132(5) . ?
Zn2 N1A 2.14(3) . ?
Zn2 O1 2.162(6) . ?
Zn2 Zn2 3.1005(17) 7 ?
O1 C1 1.250(10) . ?
O2 C1 1.271(10) . ?
O3 N3 1.296(13) . ?
O4 N3 1.292(13) . ?
O5 C8 1.249(9) . ?
O6 C8 1.256(9) . ?
O7 N4 1.366(13) . ?
O8 N4 1.305(13) . ?
O9 N5 1.300(17) . ?
O9' N5' 1.319(18) . ?
O10 N5 1.306(17) . ?
O10' N5' 1.275(19) . ?
O11 C15 1.231(10) . ?
O12 C15 1.268(10) . ?
O13 Zn2 2.053(5) 7 ?
O13 H13 1.0000 . ?
C1 C2 1.519(11) . ?
C2 C3 1.352(14) . ?
C2 C7 1.404(13) . ?
C3 C4 1.400(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.282(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.456(16) . ?
C5 C12 1.522(14) 4 ?
C6 C7 1.382(14) . ?
C6 N3 1.425(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.504(10) . ?
C9 C10 1.346(13) . ?
C9 C14 1.384(13) . ?
C10 C11 1.401(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(16) . ?
C11 H11 0.9500 . ?
C12 C13 1.412(17) . ?
C12 C5 1.522(14) 4_545 ?
C13 C14 1.364(14) . ?
C13 N4 1.399(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.486(12) . ?
C16 C17 1.341(14) . ?
C16 C21 1.374(15) . ?
C17 C18 1.424(16) . ?
C17 H17 0.9500 . ?
C18 C19 1.358(17) . ?
C18 N5' 1.448(17) . ?
C19 C20 1.359(18) . ?
C19 C19 1.55(2) 2_554 ?
C20 C21 1.363(17) . ?
C20 N5 1.448(16) . ?
C21 H21 0.9501 . ?
C22 N2 1.25(4) . ?
C22 C24 1.37(3) . ?
C22 N2' 1.39(4) 3_445 ?
C22 H22A 0.9600 . ?
C23 C25 1.36(3) . ?
C23 N2 1.380(10) . ?
C23 N2' 1.59(4) 3_445 ?
C23 H23A 0.9600 . ?
C22' N2 1.36(4) 3 ?
C22' C24' 1.40(4) . ?
C22' N2' 1.42(4) . ?
C22' H22B 0.9602 . ?
C23' N2 1.22(4) 3 ?
C23' C25' 1.33(3) . ?
C23' N2' 1.37(3) . ?
C23' H23B 0.9599 . ?
C27' C28' 1.34(3) . ?
C27' C31' 1.38(3) . ?
C27' C26' 1.50(3) . ?
C28' C29' 1.38(3) . ?
C28' C29' 1.61(3) 5_675 ?
C28' C28' 1.98(5) 5_675 ?
C28' H28' 0.9499 . ?
C29' N1' 1.36(3) . ?
C29' C28' 1.61(3) 5_675 ?
C29' H29' 0.9500 . ?
N1 C29 1.32(4) . ?
N1 C30 1.36(3) . ?
C29 C28 1.35(2) . ?
C29 H29A 0.9597 . ?
C30 C31 1.35(2) . ?
C30 H30A 0.9600 . ?
C30' N1' 1.33(3) . ?
C30' C31' 1.39(3) . ?
C30' H30' 0.9503 . ?
C31' H31' 0.9500 . ?
C24 C26 1.38(2) . ?
C24 H24A 0.9600 . ?
C25 C26 1.37(2) . ?
C25 H25A 0.9597 . ?
C26 C27 1.48(2) . ?
C27 C31 1.35(2) . ?
C27 C28 1.42(2) . ?
C28 H28A 0.9598 . ?
C31 H31A 0.9600 . ?
C24' C26' 1.37(3) . ?
C24' H24B 0.9600 . ?
C25' C26' 1.41(3) . ?
C25' H25B 0.9602 . ?
N1A C30A 1.34(3) . ?
N1A C29A 1.39(4) . ?
C29A C28A 1.37(3) . ?
C29A H29B 0.9500 . ?
C30A C31A 1.43(2) . ?
C30A H30B 0.9500 . ?
C27A C31A 1.37(2) . ?
C27A C28A 1.40(2) . ?
C27A C27A 1.41(3) 5 ?
C28A H28B 0.9500 . ?
C31A H31B 0.9500 . ?
N2 N2' 0.32(4) 3_445 ?
N2 C23' 1.23(4) 3_445 ?
N2 C22' 1.36(4) 3_445 ?
N2 Zn1 2.117(17) 3_445 ?
N2' N2 0.32(4) 3 ?
N2' C22 1.39(4) 3 ?
N2' C23 1.59(4) 3 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2' Zn1 O13 110.3(13) . . ?
N2' Zn1 O12 106.0(11) . . ?
O13 Zn1 O12 115.3(2) . . ?
N2' Zn1 O2 103.2(8) . . ?
O13 Zn1 O2 101.4(2) . . ?
O12 Zn1 O2 120.0(2) . . ?
N2' Zn1 N2 5(2) . 3 ?
O13 Zn1 N2 105.2(10) . 3 ?
O12 Zn1 N2 108.6(7) . 3 ?
O2 Zn1 N2 105.0(6) . 3 ?
O13 Zn2 O5 95.9(2) 7 . ?
O13 Zn2 N1 103.1(7) 7 . ?
O5 Zn2 N1 91.1(8) . . ?
O13 Zn2 O13 83.4(2) 7 . ?
O5 Zn2 O13 93.51(19) . . ?
N1 Zn2 O13 171.6(5) . . ?
O13 Zn2 O11 89.9(2) 7 . ?
O5 Zn2 O11 172.4(2) . . ?
N1 Zn2 O11 82.7(8) . . ?
O13 Zn2 O11 92.03(19) . . ?
O13 Zn2 N1A 93.1(7) 7 . ?
O5 Zn2 N1A 87.1(7) . . ?
O13 Zn2 N1A 176.5(7) . . ?
O11 Zn2 N1A 87.7(7) . . ?
O13 Zn2 O1 169.3(2) 7 . ?
O5 Zn2 O1 87.6(2) . . ?
N1 Zn2 O1 87.0(6) . . ?
O13 Zn2 O1 86.3(2) . . ?
O11 Zn2 O1 87.6(2) . . ?
N1A Zn2 O1 97.2(6) . . ?
O13 Zn2 Zn2 42.27(13) 7 7 ?
O5 Zn2 Zn2 96.26(15) . 7 ?
N1 Zn2 Zn2 145.0(7) . 7 ?
O13 Zn2 Zn2 41.14(13) . 7 ?
O11 Zn2 Zn2 91.32(14) . 7 ?
N1A Zn2 Zn2 135.4(7) . 7 ?
O1 Zn2 Zn2 127.35(17) . 7 ?
C1 O1 Zn2 134.5(6) . . ?
C1 O2 Zn1 110.4(5) . . ?
C8 O5 Zn2 125.2(5) . . ?
C15 O11 Zn2 140.3(5) . . ?
C15 O12 Zn1 117.1(5) . . ?
Zn1 O13 Zn2 129.6(2) . 7 ?
Zn1 O13 Zn2 102.7(2) . . ?
Zn2 O13 Zn2 96.6(2) 7 . ?
Zn1 O13 H13 108.5 . . ?
Zn2 O13 H13 108.5 7 . ?
Zn2 O13 H13 108.5 . . ?
O1 C1 O2 125.8(8) . . ?
O1 C1 C2 117.0(8) . . ?
O2 C1 C2 117.1(8) . . ?
C3 C2 C7 120.4(9) . . ?
C3 C2 C1 122.4(9) . . ?
C7 C2 C1 117.3(9) . . ?
C2 C3 C4 119.8(10) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 123.2(11) . . ?
C5 C4 H4 118.4 . . ?
C3 C4 H4 118.4 . . ?
C4 C5 C6 118.3(10) . . ?
C4 C5 C12 124.3(12) . 4 ?
C6 C5 C12 117.4(11) . 4 ?
C7 C6 N3 116.0(11) . . ?
C7 C6 C5 120.0(10) . . ?
N3 C6 C5 124.0(11) . . ?
C6 C7 C2 118.2(10) . . ?
C6 C7 H7 120.9 . . ?
C2 C7 H7 120.9 . . ?
O5 C8 O6 126.8(7) . . ?
O5 C8 C9 116.1(7) . . ?
O6 C8 C9 117.2(7) . . ?
C10 C9 C14 117.7(9) . . ?
C10 C9 C8 122.5(8) . . ?
C14 C9 C8 119.7(8) . . ?
C9 C10 C11 121.6(11) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C12 C11 C10 120.6(12) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 117.5(10) . . ?
C11 C12 C5 119.8(12) . 4_545 ?
C13 C12 C5 122.6(11) . 4_545 ?
C14 C13 N4 114.7(13) . . ?
C14 C13 C12 119.5(11) . . ?
N4 C13 C12 125.7(11) . . ?
C13 C14 C9 122.9(11) . . ?
C13 C14 H14 118.6 . . ?
C9 C14 H14 118.6 . . ?
O11 C15 O12 127.8(7) . . ?
O11 C15 C16 115.7(8) . . ?
O12 C15 C16 116.5(8) . . ?
C17 C16 C21 113.4(11) . . ?
C17 C16 C15 125.1(10) . . ?
C21 C16 C15 121.4(10) . . ?
C16 C17 C18 124.0(12) . . ?
C16 C17 H17 118.0 . . ?
C18 C17 H17 118.0 . . ?
C19 C18 C17 118.2(12) . . ?
C19 C18 N5' 122.9(17) . . ?
C17 C18 N5' 116.6(17) . . ?
C18 C19 C20 119.9(12) . . ?
C18 C19 C19 118.3(12) . 2_554 ?
C20 C19 C19 121.8(12) . 2_554 ?
C19 C20 C21 118.5(13) . . ?
C19 C20 N5 126.2(14) . . ?
C21 C20 N5 115.2(15) . . ?
C20 C21 C16 125.7(14) . . ?
C20 C21 H21 118.1 . . ?
C16 C21 H21 116.2 . . ?
N2 C22 C24 122(2) . . ?
N2 C22 N2' 12.4(18) . 3_445 ?
C24 C22 N2' 133(3) . 3_445 ?
N2 C22 H22A 123.1 . . ?
C24 C22 H22A 114.6 . . ?
N2' C22 H22A 111.8 3_445 . ?
C25 C23 N2 119.1(17) . . ?
C25 C23 N2' 128(2) . 3_445 ?
N2 C23 N2' 9.4(18) . 3_445 ?
C25 C23 H23A 117.7 . . ?
N2 C23 H23A 123.1 . . ?
N2' C23 H23A 114.7 3_445 . ?
N2 C22' C24' 117(3) 3 . ?
N2 C22' N2' 13.0(18) 3 . ?
C24' C22' N2' 126(3) . . ?
N2 C22' H22B 123.4 3 . ?
C24' C22' H22B 119.4 . . ?
N2' C22' H22B 114.1 . . ?
N2 C23' C25' 121(2) 3 . ?
N2 C23' N2' 13(2) 3 . ?
C25' C23' N2' 130(2) . . ?
N2 C23' H23B 120.6 3 . ?
C25' C23' H23B 118.0 . . ?
N2' C23' H23B 111.7 . . ?
C28' C27' C31' 117(2) . . ?
C28' C27' C26' 123(2) . . ?
C31' C27' C26' 120(2) . . ?
C27' C28' C29' 122(2) . . ?
C27' C28' C29' 103(2) . 5_675 ?
C29' C28' C29' 97.4(19) . 5_675 ?
C27' C28' C28' 123(2) . 5_675 ?
C29' C28' C28' 53.8(15) . 5_675 ?
C29' C28' C28' 43.6(12) 5_675 5_675 ?
C27' C28' H28' 118.5 . . ?
C29' C28' H28' 119.8 . . ?
C29' C28' H28' 65.5 5_675 . ?
C28' C28' H28' 90.5 5_675 . ?
N1' C29' C28' 119(2) . . ?
N1' C29' C28' 116(2) . 5_675 ?
C28' C29' C28' 82.6(19) . 5_675 ?
N1' C29' H29' 120.2 . . ?
C28' C29' H29' 120.4 . . ?
C28' C29' H29' 76.1 5_675 . ?
C29 N1 C30 117(2) . . ?
C29 N1 Zn2 120.9(18) . . ?
C30 N1 Zn2 122(2) . . ?
N1 C29 C28 124(2) . . ?
N1 C29 H29A 116.1 . . ?
C28 C29 H29A 119.6 . . ?
C31 C30 N1 121(2) . . ?
C31 C30 H30A 119.1 . . ?
N1 C30 H30A 119.8 . . ?
N1' C30' C31' 119(2) . . ?
N1' C30' H30' 120.8 . . ?
C31' C30' H30' 119.8 . . ?
C27' C31' C30' 121(2) . . ?
C27' C31' H31' 120.7 . . ?
C30' C31' H31' 118.1 . . ?
C22 C24 C26 118.7(17) . . ?
C22 C24 H24A 120.2 . . ?
C26 C24 H24A 121.0 . . ?
C23 C25 C26 119.7(15) . . ?
C23 C25 H25A 119.9 . . ?
C26 C25 H25A 120.5 . . ?
C25 C26 C24 118.2(13) . . ?
C25 C26 C27 120.1(14) . . ?
C24 C26 C27 121.7(13) . . ?
C31 C27 C28 114.5(14) . . ?
C31 C27 C26 124.5(14) . . ?
C28 C27 C26 121.0(13) . . ?
C29 C28 C27 119.6(15) . . ?
C29 C28 H28A 120.8 . . ?
C27 C28 H28A 119.6 . . ?
C27 C31 C30 123.6(16) . . ?
C27 C31 H31A 118.5 . . ?
C30 C31 H31A 117.8 . . ?
C26' C24' C22' 120(2) . . ?
C26' C24' H24B 119.5 . . ?
C22' C24' H24B 120.9 . . ?
C23' C25' C26' 119.6(19) . . ?
C23' C25' H25B 120.4 . . ?
C26' C25' H25B 120.0 . . ?
C24' C26' C25' 116.2(18) . . ?
C24' C26' C27' 120.0(19) . . ?
C25' C26' C27' 123.8(19) . . ?
C30A N1A C29A 113(2) . . ?
C30A N1A Zn2 121(2) . . ?
C29A N1A Zn2 124.5(18) . . ?
C28A C29A N1A 124(2) . . ?
C28A C29A H29B 118.0 . . ?
N1A C29A H29B 118.0 . . ?
N1A C30A C31A 124(2) . . ?
N1A C30A H30B 117.8 . . ?
C31A C30A H30B 117.8 . . ?
C31A C27A C28A 114.2(15) . . ?
C31A C27A C27A 123(2) . 5 ?
C28A C27A C27A 123(2) . 5 ?
C29A C28A C27A 122.8(18) . . ?
C29A C28A H28B 118.6 . . ?
C27A C28A H28B 118.6 . . ?
C27A C31A C30A 121.3(17) . . ?
C27A C31A H31B 119.4 . . ?
C30A C31A H31B 119.4 . . ?
C30' N1' C29' 121(2) . . ?
N2' N2 C23' 111(10) 3_445 3_445 ?
N2' N2 C22 111(9) 3_445 . ?
N2' N2 C22' 95(10) 3_445 3_445 ?
C23' N2 C22' 122(3) 3_445 3_445 ?
N2' N2 C23 126(9) 3_445 . ?
C22 N2 C23 121(2) . . ?
N2' N2 Zn1 31(10) 3_445 3_445 ?
C23' N2 Zn1 117.2(18) 3_445 3_445 ?
C22 N2 Zn1 118.3(17) . 3_445 ?
C22' N2 Zn1 111.4(18) 3_445 3_445 ?
C23 N2 Zn1 117.9(18) . 3_445 ?
N2 N2' C23' 57(9) 3 . ?
N2 N2' C22 57(8) 3 3 ?
N2 N2' C22' 72(9) 3 . ?
C23' N2' C22' 108(3) . . ?
N2 N2' C23 45(8) 3 3 ?
C22 N2' C23 100(2) 3 3 ?
N2 N2' Zn1 144(10) 3 . ?
C23' N2' Zn1 127(2) . . ?
C22 N2' Zn1 128(2) 3 . ?
C22' N2' Zn1 124(2) . . ?
C23 N2' Zn1 123(2) 3 . ?
O4 N3 O3 113.8(12) . . ?
O4 N3 C6 126.4(14) . . ?
O3 N3 C6 119.8(12) . . ?
O8 N4 O7 103.9(13) . . ?
O8 N4 C13 129.4(14) . . ?
O7 N4 C13 126.6(14) . . ?
O9 N5 O10 106.8(19) . . ?
O9 N5 C20 126(2) . . ?
O10 N5 C20 127(2) . . ?
O10' N5' O9' 101(3) . . ?
O10' N5' C18 117(3) . . ?
O9' N5' C18 142(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
Zn2 O1 C1 O2 55.9(13) . . . . ?
Zn2 O1 C1 C2 -121.5(8) . . . . ?
Zn1 O2 C1 O1 -12.5(12) . . . . ?
Zn1 O2 C1 C2 164.9(7) . . . . ?
O1 C1 C2 C3 -176.0(10) . . . . ?
O2 C1 C2 C3 6.3(15) . . . . ?
O1 C1 C2 C7 5.8(14) . . . . ?
O2 C1 C2 C7 -171.9(9) . . . . ?
C7 C2 C3 C4 2.0(18) . . . . ?
C1 C2 C3 C4 -176.0(10) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C3 C4 C5 C12 -179.5(12) . . . 4 ?
C4 C5 C6 C7 -2(2) . . . . ?
C12 C5 C6 C7 177.3(12) 4 . . . ?
C4 C5 C6 N3 177.6(15) . . . . ?
C12 C5 C6 N3 -3(2) 4 . . . ?
N3 C6 C7 C2 -175.6(13) . . . . ?
C5 C6 C7 C2 4(2) . . . . ?
C3 C2 C7 C6 -4.1(18) . . . . ?
C1 C2 C7 C6 174.0(11) . . . . ?
Zn2 O5 C8 O6 -22.9(13) . . . . ?
Zn2 O5 C8 C9 157.4(6) . . . . ?
O5 C8 C9 C10 174.7(10) . . . . ?
O6 C8 C9 C10 -5.0(15) . . . . ?
O5 C8 C9 C14 -4.6(14) . . . . ?
O6 C8 C9 C14 175.7(9) . . . . ?
C14 C9 C10 C11 0.9(19) . . . . ?
C8 C9 C10 C11 -178.3(11) . . . . ?
C9 C10 C11 C12 -2(2) . . . . ?
C10 C11 C12 C13 0(2) . . . . ?
C10 C11 C12 C5 -177.1(12) . . . 4_545 ?
C11 C12 C13 C14 4(2) . . . . ?
C5 C12 C13 C14 -179.3(12) 4_545 . . . ?
C11 C12 C13 N4 179.6(13) . . . . ?
C5 C12 C13 N4 -4(2) 4_545 . . . ?
N4 C13 C14 C9 178.4(12) . . . . ?
C12 C13 C14 C9 -6(2) . . . . ?
C10 C9 C14 C13 3.0(18) . . . . ?
C8 C9 C14 C13 -177.7(11) . . . . ?
Zn2 O11 C15 O12 2.0(14) . . . . ?
Zn2 O11 C15 C16 179.5(6) . . . . ?
Zn1 O12 C15 O11 1.5(11) . . . . ?
Zn1 O12 C15 C16 -176.0(6) . . . . ?
O11 C15 C16 C17 -167.7(11) . . . . ?
O12 C15 C16 C17 10.1(15) . . . . ?
O11 C15 C16 C21 8.1(15) . . . . ?
O12 C15 C16 C21 -174.1(11) . . . . ?
C21 C16 C17 C18 4(2) . . . . ?
C15 C16 C17 C18 -179.6(13) . . . . ?
C16 C17 C18 C19 0(3) . . . . ?
C16 C17 C18 N5' 163.2(16) . . . . ?
C17 C18 C19 C20 -2(3) . . . . ?
N5' C18 C19 C20 -163.8(18) . . . . ?
C17 C18 C19 C19 -179.8(13) . . . 2_554 ?
N5' C18 C19 C19 18(2) . . . 2_554 ?
C18 C19 C20 C21 -1(3) . . . . ?
C19 C19 C20 C21 176.9(15) 2_554 . . . ?
C18 C19 C20 N5 176.9(18) . . . . ?
C19 C19 C20 N5 -5(3) 2_554 . . . ?
C19 C20 C21 C16 6(3) . . . . ?
N5 C20 C21 C16 -172.0(17) . . . . ?
C17 C16 C21 C20 -8(3) . . . . ?
C15 C16 C21 C20 176.1(16) . . . . ?
C31' C27' C28' C29' 11(4) . . . . ?
C26' C27' C28' C29' -178(2) . . . . ?
C31' C27' C28' C29' 118(2) . . . 5_675 ?
C26' C27' C28' C29' -71(3) . . . 5_675 ?
C31' C27' C28' C28' 76(4) . . . 5_675 ?
C26' C27' C28' C28' -113(3) . . . 5_675 ?
C27' C28' C29' N1' -5(4) . . . . ?
C29' C28' C29' N1' -115(3) 5_675 . . . ?
C28' C28' C29' N1' -115(3) 5_675 . . . ?
C27' C28' C29' C28' 110(3) . . . 5_675 ?
C29' C28' C29' C28' -0.005(2) 5_675 . . 5_675 ?
C30 N1 C29 C28 1.9(18) . . . . ?
Zn2 N1 C29 C28 179.9(12) . . . . ?
C29 N1 C30 C31 -1.2(13) . . . . ?
Zn2 N1 C30 C31 -179.3(10) . . . . ?
C28' C27' C31' C30' -12(4) . . . . ?
C26' C27' C31' C30' 177(2) . . . . ?
N1' C30' C31' C27' 7(4) . . . . ?
N2 C22 C24 C26 -9(4) . . . . ?
N2' C22 C24 C26 -16(4) 3_445 . . . ?
N2 C23 C25 C26 4(3) . . . . ?
N2' C23 C25 C26 9(3) 3_445 . . . ?
C23 C25 C26 C24 -4(2) . . . . ?
C23 C25 C26 C27 176.1(16) . . . . ?
C22 C24 C26 C25 6(3) . . . . ?
C22 C24 C26 C27 -173.7(18) . . . . ?
C25 C26 C27 C31 20.5(19) . . . . ?
C24 C26 C27 C31 -159.8(13) . . . . ?
C25 C26 C27 C28 -162.1(13) . . . . ?
C24 C26 C27 C28 18(2) . . . . ?
N1 C29 C28 C27 -1.6(18) . . . . ?
C31 C27 C28 C29 0.7(12) . . . . ?
C26 C27 C28 C29 -177.0(14) . . . . ?
C28 C27 C31 C30 -0.1(5) . . . . ?
C26 C27 C31 C30 177.4(13) . . . . ?
N1 C30 C31 C27 0.4(6) . . . . ?
N2 C22' C24' C26' 7(4) 3 . . . ?
N2' C22' C24' C26' -3(4) . . . . ?
N2 C23' C25' C26' -19(4) 3 . . . ?
N2' C23' C25' C26' -8(4) . . . . ?
C22' C24' C26' C25' -2(3) . . . . ?
C22' C24' C26' C27' 177.3(19) . . . . ?
C23' C25' C26' C24' 7(3) . . . . ?
C23' C25' C26' C27' -172(2) . . . . ?
C28' C27' C26' C24' 33(3) . . . . ?
C31' C27' C26' C24' -155(2) . . . . ?
C28' C27' C26' C25' -147(2) . . . . ?
C31' C27' C26' C25' 24(3) . . . . ?
C30A N1A C29A C28A 2.1(16) . . . . ?
Zn2 N1A C29A C28A -164.6(12) . . . . ?
C29A N1A C30A C31A -1.8(12) . . . . ?
Zn2 N1A C30A C31A 165.5(10) . . . . ?
N1A C29A C28A C27A -1.5(17) . . . . ?
C31A C27A C28A C29A 0.3(12) . . . . ?
C27A C27A C28A C29A -179.1(19) 5 . . . ?
C28A C27A C31A C30A 0.1(5) . . . . ?
C27A C27A C31A C30A 179.5(18) 5 . . . ?
N1A C30A C31A C27A 0.8(6) . . . . ?
C31' C30' N1' C29' -1(4) . . . . ?
C28' C29' N1' C30' 0(4) . . . . ?
C28' C29' N1' C30' -96(3) 5_675 . . . ?
C24 C22 N2 N2' -156(14) . . . 3_445 ?
C24 C22 N2 C23 10(5) . . . . ?
N2' C22 N2 C23 165(17) 3_445 . . . ?
C24 C22 N2 Zn1 171.2(19) . . . 3_445 ?
N2' C22 N2 Zn1 -33(13) 3_445 . . 3_445 ?
C25 C23 N2 N2' 156(17) . . . 3_445 ?
C25 C23 N2 C22 -7(4) . . . . ?
N2' C23 N2 C22 -163(20) 3_445 . . . ?
C25 C23 N2 Zn1 -168.5(16) . . . 3_445 ?
N2' C23 N2 Zn1 35(16) 3_445 . . 3_445 ?
C25' C23' N2' N2 -51(15) . . . 3 ?
N2 C23' N2' C22' 53(12) 3 . . . ?
C25' C23' N2' C22' 2(5) . . . . ?
N2 C23' N2' Zn1 -136(16) 3 . . . ?
C25' C23' N2' Zn1 173(2) . . . . ?
C24' C22' N2' N2 48(14) . . . 3 ?
N2 C22' N2' C23' -44(11) 3 . . . ?
C24' C22' N2' C23' 4(4) . . . . ?
N2 C22' N2' Zn1 144(15) 3 . . . ?
C24' C22' N2' Zn1 -168(2) . . . . ?
O13 Zn1 N2' N2 4(16) . . . 3 ?
O12 Zn1 N2' N2 -122(16) . . . 3 ?
O2 Zn1 N2' N2 111(15) . . . 3 ?
O13 Zn1 N2' C23' 86(3) . . . . ?
O12 Zn1 N2' C23' -39(4) . . . . ?
O2 Zn1 N2' C23' -166(3) . . . . ?
N2 Zn1 N2' C23' 82(15) 3 . . . ?
O13 Zn1 N2' C22 -80(3) . . . 3 ?
O12 Zn1 N2' C22 155(3) . . . 3 ?
O2 Zn1 N2' C22 28(4) . . . 3 ?
N2 Zn1 N2' C22 -83(16) 3 . . 3 ?
O13 Zn1 N2' C22' -104(3) . . . . ?
O12 Zn1 N2' C22' 131(3) . . . . ?
O2 Zn1 N2' C22' 4(3) . . . . ?
N2 Zn1 N2' C22' -108(17) 3 . . . ?
O13 Zn1 N2' C23 60(3) . . . 3 ?
O12 Zn1 N2' C23 -65(3) . . . 3 ?
O2 Zn1 N2' C23 168(2) . . . 3 ?
N2 Zn1 N2' C23 56(14) 3 . . 3 ?
C7 C6 N3 O4 158.0(18) . . . . ?
C5 C6 N3 O4 -22(3) . . . . ?
C7 C6 N3 O3 -19(2) . . . . ?
C5 C6 N3 O3 161.0(16) . . . . ?
C14 C13 N4 O8 -161.8(17) . . . . ?
C12 C13 N4 O8 23(3) . . . . ?
C14 C13 N4 O7 13(3) . . . . ?
C12 C13 N4 O7 -162.5(18) . . . . ?
C19 C20 N5 O9 -134(3) . . . . ?
C21 C20 N5 O9 44(3) . . . . ?
C19 C20 N5 O10 43(3) . . . . ?
C21 C20 N5 O10 -139(2) . . . . ?
C19 C18 N5' O10' -179(3) . . . . ?
C17 C18 N5' O10' 19(3) . . . . ?
C19 C18 N5' O9' 4(4) . . . . ?
C17 C18 N5' O9' -159(4) . . . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 1.000 0.088 0.250 252.9 92.7
2 1.000 -0.089 0.750 252.8 93.3
3 0.500 0.411 0.750 252.8 93.3
4 0.500 0.588 0.250 252.9 92.7
_platon_squeeze_details          
;
;


_refine_diff_density_max         1.467
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.251

####################################################################### 
# 
# 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_zzzz
_database_code_depnum_ccdc_archive 'CCDC 1434743'
_audit_update_record             
;
2016-01-29 deposited with the CCDC.
2016-02-09 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 O26, 2(H2 O)'
_chemical_formula_sum            'C72 H50 N12 Ni3 O28'
_chemical_formula_weight         1707.37

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                   21.687(3)
_cell_length_b                   18.249(2)
_cell_length_c                   22.474(4)
_cell_angle_alpha                90
_cell_angle_beta                 118.150(2)
_cell_angle_gamma                90
_cell_volume                     7842(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3711
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      21.05
_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_F_000             3496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.802
_shelx_estimated_absorpt_T_min   0.807
_shelx_estimated_absorpt_T_max   0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_process_details   sadabs
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19825
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.457
_diffrn_reflns_theta_max         21.205
_diffrn_reflns_theta_full        21.205
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             4283
_reflns_number_gt                3622
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.1261P)²+123.0352P] 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         4283
_refine_ls_number_parameters     619
_refine_ls_number_restraints     296
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0806
_refine_ls_wR_factor_ref         0.2215
_refine_ls_wR_factor_gt          0.2122
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.042
_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
C1 C 0.6571(4) 0.2565(4) 0.8476(3) 0.0189(18) Uani 1 1 d . . . . .
H1 H 0.6996 0.2652 0.8481 0.023 Uiso 1 1 calc R U . . .
C2 C 0.5976(4) 0.2555(4) 0.7864(4) 0.0203(18) Uani 1 1 d . . . . .
H2 H 0.6008 0.2634 0.7471 0.024 Uiso 1 1 calc R U . . .
C3 C 0.5325(4) 0.2428(4) 0.7826(4) 0.0148(17) Uani 1 1 d . . . . .
C4 C 0.5326(4) 0.2317(4) 0.8437(4) 0.0192(18) Uani 1 1 d . . . . .
H4 H 0.4908 0.2233 0.8446 0.023 Uiso 1 1 calc R U . . .
C5 C 0.5951(4) 0.2332(4) 0.9034(3) 0.0185(17) Uani 1 1 d . . . . .
H5 H 0.5936 0.2251 0.9435 0.022 Uiso 1 1 calc R U . . .
C6 C 0.8097(4) 0.3638(4) 0.9458(4) 0.0195(18) Uani 1 1 d . . . . .
C7 C 0.8322(4) 0.4429(4) 0.9484(4) 0.0188(17) Uani 1 1 d . . . . .
C8 C 0.8145(4) 0.4953(5) 0.9823(4) 0.034(2) Uani 1 1 d . . . . .
H8 H 0.7876 0.4825 1.0029 0.041 Uiso 1 1 calc R U . . .
C9 C 0.8370(5) 0.5668(5) 0.9852(5) 0.048(3) Uani 1 1 d . U . . .
H9 H 0.8242 0.6017 1.0076 0.058 Uiso 1 1 calc R U . . .
C10 C 0.8779(4) 0.5880(5) 0.9559(5) 0.037(2) Uani 1 1 d . U . . .
C11 C 0.8944(4) 0.5343(4) 0.9230(4) 0.031(2) Uani 1 1 d . . . . .
C12 C 0.8727(4) 0.4620(4) 0.9188(4) 0.0251(19) Uani 1 1 d . . . . .
H12 H 0.8853 0.4271 0.8964 0.030 Uiso 1 1 calc R U . . .
C13 C 0.9059(4) 0.6646(4) 0.9645(5) 0.039(2) Uani 1 1 d . . . . .
C16 C 0.9639(4) 0.8058(5) 0.9846(5) 0.040(2) Uani 1 1 d . . . . .
C17 C 1.0014(5) 0.7484(4) 1.0245(5) 0.035(2) Uani 1 1 d . . . . .
H17 H 1.0469 0.7557 1.0586 0.042 Uiso 1 1 calc R U . . .
C18 C 0.9714(5) 0.6792(5) 1.0139(5) 0.038(2) Uani 1 1 d . . . . .
H18 H 0.9976 0.6411 1.0420 0.045 Uiso 1 1 calc R U . . .
C19 C 0.9934(5) 0.8823(5) 0.9944(5) 0.042(2) Uani 1 1 d . . . . .
C20 C 0.7635(4) 1.0036(5) 0.8749(4) 0.029(2) Uani 1 1 d . . . . .
C21 C 0.6853(4) 0.9960(4) 0.8382(4) 0.028(2) Uani 1 1 d . . . . .
C24 C 0.5387(4) 0.9814(4) 0.7690(4) 0.0267(19) Uani 1 1 d . . . . .
C14 C 0.8745(7) 0.7218(10) 0.9088(7) 0.034(3) Uani 0.5 1 d D U P A 1
C15 C 0.9025(8) 0.7915(9) 0.9177(9) 0.026(4) Uani 0.5 1 d . U P A 1
H15 H 0.8842 0.8271 0.8842 0.031 Uiso 0.5 1 calc R U P A 1
C22 C 0.6546(8) 0.9350(9) 0.7919(8) 0.031(4) Uani 0.5 1 d . U P B 1
H22 H 0.6824 0.9008 0.7852 0.037 Uiso 0.5 1 calc R U P B 1
C23 C 0.5837(9) 0.9297(9) 0.7587(9) 0.048(2) Uani 0.5 1 d D U P B 1
C25 C 0.5710(9) 1.0363(9) 0.8115(9) 0.031(4) Uani 0.5 1 d . U P B 1
H25 H 0.5441 1.0706 0.8197 0.037 Uiso 0.5 1 calc R U P B 1
C26 C 0.6430(9) 1.0441(10) 0.8440(9) 0.033(4) Uani 0.5 1 d . U P B 1
H26 H 0.6625 1.0851 0.8711 0.039 Uiso 0.5 1 calc R U P B 1
C14' C 0.8652(6) 0.7236(10) 0.9457(10) 0.039(3) Uani 0.5 1 d D U P A 2
C15' C 0.8931(8) 0.7943(9) 0.9541(10) 0.029(4) Uani 0.5 1 d . U P A 2
H15' H 0.8630 0.8343 0.9385 0.035 Uiso 0.5 1 calc R U P A 2
C22' C 0.6542(8) 0.9357(9) 0.8482(8) 0.026(4) Uani 0.5 1 d . U P B 2
H22' H 0.6809 0.8988 0.8776 0.031 Uiso 0.5 1 calc R U P B 2
C23' C 0.5819(9) 0.9308(8) 0.8135(10) 0.045(2) Uani 0.5 1 d D U P B 2
C25' C 0.5719(8) 1.0453(9) 0.7637(9) 0.027(4) Uani 0.5 1 d . U P B 2
H25' H 0.5447 1.0833 0.7365 0.032 Uiso 0.5 1 calc R U P B 2
C26' C 0.6437(8) 1.0535(9) 0.7977(9) 0.032(4) Uani 0.5 1 d . U P B 2
H26' H 0.6642 1.0967 0.7939 0.038 Uiso 0.5 1 calc R U P B 2
N1 N 0.6573(3) 0.2457(3) 0.9067(3) 0.0158(14) Uani 1 1 d . . . . .
N3 N 0.9376(5) 0.5514(5) 0.8911(4) 0.053(2) Uani 1 1 d . . . . .
N5 N 0.8886(4) 1.0176(4) 0.8373(4) 0.041(2) Uani 1 1 d . . . . .
Ni1 Ni 0.7500 0.2500 1.0000 0.0136(4) Uani 1 2 d S . P . .
Ni2 Ni 0.89090(5) 1.01502(6) 0.93109(6) 0.0339(4) Uani 1 1 d . . . . .
O1 O 0.7748(2) 0.3493(3) 0.9761(2) 0.0187(12) Uani 1 1 d . . . . .
O2 O 0.8295(3) 0.3194(3) 0.9155(3) 0.0285(13) Uani 1 1 d . . . . .
O3 O 0.9285(5) 0.6111(4) 0.8623(4) 0.082(3) Uani 1 1 d . U . . .
O4 O 0.9810(4) 0.5056(5) 0.8957(4) 0.073(2) Uani 1 1 d . . . . .
O7 O 1.0536(3) 0.8918(3) 1.0442(3) 0.0374(15) Uani 1 1 d . . . . .
O8 O 0.9579(3) 0.9300(3) 0.9525(4) 0.060(2) Uani 1 1 d . . . . .
O9 O 0.8001(3) 0.9465(3) 0.8884(3) 0.0362(15) Uani 1 1 d . . . . .
O10 O 0.7903(3) 1.0664(3) 0.8906(3) 0.0287(13) Uani 1 1 d . . . . .
N2 N 0.8151(6) 0.7116(7) 0.8485(6) 0.055(3) Uani 0.5 1 d D U P A 1
N4 N 0.5587(6) 0.8691(8) 0.7176(8) 0.053(2) Uani 0.5 1 d D U P B 1
O5 O 0.7660(10) 0.6649(10) 0.8430(9) 0.080(6) Uani 0.5 1 d D U P A 1
O6 O 0.8064(8) 0.7562(8) 0.7969(6) 0.091(5) Uani 0.5 1 d D U P A 1
O11 O 0.4878(7) 0.8609(11) 0.6777(9) 0.048(3) Uani 0.5 1 d D U P B 1
O12 O 0.5945(7) 0.8386(9) 0.6868(7) 0.074(3) Uani 0.5 1 d D U P B 1
N2' N 0.7936(6) 0.7185(7) 0.9097(7) 0.048(3) Uani 0.5 1 d D U P A 2
N4' N 0.5542(6) 0.8709(7) 0.8299(8) 0.048(2) Uani 0.5 1 d D U P B 2
O11' O 0.4856(7) 0.8632(11) 0.8165(10) 0.045(3) Uani 0.5 1 d D U P B 2
O12' O 0.5921(6) 0.8083(7) 0.8584(7) 0.065(3) Uani 0.5 1 d D U P B 2
O5' O 0.7644(9) 0.6587(8) 0.8733(7) 0.052(4) Uani 0.5 1 d D U P A 2
O6' O 0.7508(6) 0.7721(6) 0.9089(7) 0.054(3) Uani 0.5 1 d D U P A 2
O13 O 0.8066(2) 0.1960(3) 0.9606(2) 0.0187(12) Uani 1 1 d . . . . .
H13A H 0.8200 0.2302 0.9363 0.022 Uiso 1 1 d R U . . .
H13B H 0.7782 0.1582 0.9305 0.022 Uiso 1 1 d R U . . .
C31 C 0.8877(4) 1.0120(5) 0.7115(5) 0.041(2) Uani 1 1 d . U . . .
C30 C 0.9089(6) 1.0731(6) 0.7522(6) 0.066(3) Uani 1 1 d . . . . .
H30 H 0.9238 1.1143 0.7381 0.079 Uiso 1 1 calc R U . . .
C28 C 0.9086(6) 1.0744(6) 0.8139(5) 0.061(3) Uani 1 1 d . . . . .
H28 H 0.9230 1.1168 0.8398 0.073 Uiso 1 1 calc R U . . .
C27 C 0.8680(7) 0.9595(7) 0.7990(7) 0.077(4) Uani 1 1 d . U . . .
H27 H 0.8532 0.9189 0.8139 0.092 Uiso 1 1 calc R U . . .
C29 C 0.8673(8) 0.9554(7) 0.7374(7) 0.084(4) Uani 1 1 d . U . . .
H29 H 0.8523 0.9122 0.7127 0.101 Uiso 1 1 calc R U . . .
C32 C 0.8888(4) 1.0072(5) 0.6469(5) 0.040(2) Uani 1 1 d . . . . .
C33 C 0.9007(5) 0.9407(5) 0.6233(5) 0.047(2) Uani 1 1 d . . . . .
H33 H 0.9088 0.8986 0.6493 0.056 Uiso 1 1 calc R U . . .
C34 C 0.8759(5) 1.0675(5) 0.6052(5) 0.051(3) Uani 1 1 d . U . . .
H34 H 0.8665 1.1131 0.6176 0.062 Uiso 1 1 calc R U . . .
C35 C 0.9006(5) 0.9366(5) 0.5631(5) 0.045(2) Uani 1 1 d . . . . .
H35 H 0.9081 0.8912 0.5489 0.054 Uiso 1 1 calc R U . . .
C36 C 0.8773(5) 1.0583(5) 0.5439(5) 0.053(3) Uani 1 1 d . U . . .
H36 H 0.8685 1.0991 0.5163 0.064 Uiso 1 1 calc R U . . .
N6 N 0.8903(4) 0.9947(4) 0.5227(4) 0.041(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.340(9) . ?
C1 C2 1.371(10) . ?
C1 H1 0.9300 . ?
C2 C3 1.392(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.387(10) . ?
C3 C3 1.478(14) 2_656 ?
C4 C5 1.387(10) . ?
C4 H4 0.9300 . ?
C5 N1 1.336(9) . ?
C5 H5 0.9300 . ?
C6 O2 1.257(9) . ?
C6 O1 1.262(9) . ?
C6 C7 1.516(11) . ?
C7 C12 1.372(11) . ?
C7 C8 1.385(11) . ?
C8 C9 1.384(13) . ?
C8 H8 0.9300 . ?
C9 C10 1.387(13) . ?
C9 H9 0.9300 . ?
C10 C11 1.374(12) . ?
C10 C13 1.501(12) . ?
C11 C12 1.389(11) . ?
C11 N3 1.455(11) . ?
C12 H12 0.9300 . ?
C13 C14' 1.328(19) . ?
C13 C18 1.354(12) . ?
C13 C14 1.521(19) . ?
C16 C17 1.370(12) . ?
C16 C15' 1.370(18) . ?
C16 C15 1.487(19) . ?
C16 C19 1.509(12) . ?
C17 C18 1.388(12) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 O8 1.245(11) . ?
C19 O7 1.268(11) . ?
C20 O9 1.256(10) . ?
C20 O10 1.258(10) . ?
C20 C21 1.503(12) . ?
C20 Ni2 2.445(8) . ?
C21 C26 1.321(19) . ?
C21 C22' 1.362(17) . ?
C21 C26' 1.403(19) . ?
C21 C22 1.452(18) . ?
C24 C25 1.332(19) . ?
C24 C23' 1.361(19) . ?
C24 C25' 1.403(18) . ?
C24 C23 1.451(19) . ?
C24 C24 1.480(16) 2_656 ?
C14 N2 1.373(10) . ?
C14 C15 1.38(2) . ?
C15 H15 0.9300 . ?
C22 C23 1.36(2) . ?
C22 H22 0.9300 . ?
C23 N4 1.379(3) . ?
C25 C26 1.39(2) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C14' N2' 1.375(10) . ?
C14' C15' 1.40(2) . ?
C15' H15' 0.9300 . ?
C22' C23' 1.39(2) . ?
C22' H22' 0.9300 . ?
C23' N4' 1.379(3) . ?
C25' C26' 1.38(2) . ?
C25' H25' 0.9300 . ?
C26' H26' 0.9300 . ?
N1 Ni1 2.113(6) . ?
N3 O4 1.227(11) . ?
N3 O3 1.236(11) . ?
N5 C27 1.305(13) . ?
N5 C28 1.325(12) . ?
N5 Ni2 2.085(8) . ?
Ni1 O1 2.033(5) 7_657 ?
Ni1 O1 2.033(5) . ?
Ni1 O13 2.071(5) 7_657 ?
Ni1 O13 2.071(5) . ?
Ni1 N1 2.113(6) 7_657 ?
Ni2 O7 2.004(5) 5_777 ?
Ni2 O8 2.022(6) . ?
Ni2 N6 2.072(8) 6_576 ?
Ni2 O9 2.140(5) . ?
Ni2 O10 2.142(5) . ?
O7 Ni2 2.004(5) 5_777 ?
N2 O5 1.324(9) . ?
N2 O6 1.355(9) . ?
N4 O11 1.376(3) . ?
N4 O12 1.377(3) . ?
N2' O5' 1.332(10) . ?
N2' O6' 1.342(9) . ?
N4' O12' 1.376(3) . ?
N4' O11' 1.378(3) . ?
O13 H13A 0.9600 . ?
O13 H13B 0.9599 . ?
C31 C29 1.359(15) . ?
C31 C30 1.375(14) . ?
C31 C32 1.466(14) . ?
C30 C28 1.391(15) . ?
C30 H30 0.9300 . ?
C28 H28 0.9300 . ?
C27 C29 1.378(17) . ?
C27 H27 0.9300 . ?
C29 H29 0.9300 . ?
C32 C34 1.386(14) . ?
C32 C33 1.395(13) . ?
C33 C35 1.356(14) . ?
C33 H33 0.9300 . ?
C34 C36 1.401(15) . ?
C34 H34 0.9300 . ?
C35 N6 1.343(12) . ?
C35 H35 0.9300 . ?
C36 N6 1.336(12) . ?
C36 H36 0.9300 . ?
N6 Ni2 2.072(8) 6_575 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.6(6) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 120.7(7) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 115.8(6) . . ?
C4 C3 C3 122.4(8) . 2_656 ?
C2 C3 C3 121.8(8) . 2_656 ?
C3 C4 C5 120.0(7) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 123.9(6) . . ?
N1 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
O2 C6 O1 127.0(7) . . ?
O2 C6 C7 116.7(6) . . ?
O1 C6 C7 116.3(7) . . ?
C12 C7 C8 119.9(7) . . ?
C12 C7 C6 119.4(7) . . ?
C8 C7 C6 120.7(7) . . ?
C9 C8 C7 119.6(8) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 122.0(8) . . ?
C8 C9 H9 119.0 . . ?
C10 C9 H9 119.0 . . ?
C11 C10 C9 116.5(8) . . ?
C11 C10 C13 122.8(8) . . ?
C9 C10 C13 120.6(8) . . ?
C10 C11 C12 123.1(8) . . ?
C10 C11 N3 120.3(7) . . ?
C12 C11 N3 116.6(8) . . ?
C7 C12 C11 118.9(7) . . ?
C7 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C14' C13 C18 112.6(10) . . ?
C14' C13 C10 123.1(9) . . ?
C18 C13 C10 119.5(8) . . ?
C18 C13 C14 115.4(9) . . ?
C10 C13 C14 122.4(9) . . ?
C17 C16 C15' 113.0(10) . . ?
C17 C16 C15 120.0(9) . . ?
C17 C16 C19 122.2(8) . . ?
C15' C16 C19 120.8(10) . . ?
C15 C16 C19 115.1(10) . . ?
C16 C17 C18 119.8(8) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C13 C18 C17 123.0(8) . . ?
C13 C18 H18 118.5 . . ?
C17 C18 H18 118.5 . . ?
O8 C19 O7 125.7(8) . . ?
O8 C19 C16 117.9(8) . . ?
O7 C19 C16 116.4(8) . . ?
O9 C20 O10 122.1(7) . . ?
O9 C20 C21 118.5(7) . . ?
O10 C20 C21 119.4(7) . . ?
O9 C20 Ni2 61.0(4) . . ?
O10 C20 Ni2 61.1(4) . . ?
C21 C20 Ni2 178.1(6) . . ?
C22' C21 C26' 119.6(11) . . ?
C26 C21 C22 118.4(11) . . ?
C26 C21 C20 122.7(10) . . ?
C22' C21 C20 120.2(9) . . ?
C26' C21 C20 120.1(10) . . ?
C22 C21 C20 118.8(9) . . ?
C23' C24 C25' 115.0(10) . . ?
C25 C24 C23 115.9(11) . . ?
C25 C24 C24 118.8(9) . 2_656 ?
C23' C24 C24 128.6(8) . 2_656 ?
C25' C24 C24 116.0(8) . 2_656 ?
C23 C24 C24 125.0(8) . 2_656 ?
N2 C14 C15 114.2(15) . . ?
N2 C14 C13 124.5(13) . . ?
C15 C14 C13 121.1(12) . . ?
C14 C15 C16 115.4(14) . . ?
C14 C15 H15 122.3 . . ?
C16 C15 H15 122.3 . . ?
C23 C22 C21 117.7(13) . . ?
C23 C22 H22 121.1 . . ?
C21 C22 H22 121.1 . . ?
C22 C23 N4 114.1(15) . . ?
C22 C23 C24 122.6(12) . . ?
N4 C23 C24 123.2(14) . . ?
C24 C25 C26 122.5(15) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C21 C26 C25 122.8(16) . . ?
C21 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
C13 C14' N2' 122.0(14) . . ?
C13 C14' C15' 121.6(12) . . ?
N2' C14' C15' 115.9(15) . . ?
C16 C15' C14' 121.2(14) . . ?
C16 C15' H15' 119.4 . . ?
C14' C15' H15' 119.4 . . ?
C21 C22' C23' 118.5(13) . . ?
C21 C22' H22' 120.8 . . ?
C23' C22' H22' 120.8 . . ?
C24 C23' N4' 119.9(14) . . ?
C24 C23' C22' 125.0(11) . . ?
N4' C23' C22' 115.0(15) . . ?
C26' C25' C24 122.2(14) . . ?
C26' C25' H25' 118.9 . . ?
C24 C25' H25' 118.9 . . ?
C25' C26' C21 119.3(15) . . ?
C25' C26' H26' 120.3 . . ?
C21 C26' H26' 120.3 . . ?
C5 N1 C1 116.0(6) . . ?
C5 N1 Ni1 121.6(4) . . ?
C1 N1 Ni1 122.4(4) . . ?
O4 N3 O3 124.8(9) . . ?
O4 N3 C11 117.3(8) . . ?
O3 N3 C11 117.9(9) . . ?
C27 N5 C28 116.6(9) . . ?
C27 N5 Ni2 119.1(7) . . ?
C28 N5 Ni2 124.2(6) . . ?
O1 Ni1 O1 180.0 7_657 . ?
O1 Ni1 O13 91.55(18) 7_657 7_657 ?
O1 Ni1 O13 88.46(18) . 7_657 ?
O1 Ni1 O13 88.45(18) 7_657 . ?
O1 Ni1 O13 91.54(18) . . ?
O13 Ni1 O13 180.0(2) 7_657 . ?
O1 Ni1 N1 91.0(2) 7_657 7_657 ?
O1 Ni1 N1 89.0(2) . 7_657 ?
O13 Ni1 N1 92.1(2) 7_657 7_657 ?
O13 Ni1 N1 87.9(2) . 7_657 ?
O1 Ni1 N1 89.0(2) 7_657 . ?
O1 Ni1 N1 91.0(2) . . ?
O13 Ni1 N1 87.9(2) 7_657 . ?
O13 Ni1 N1 92.1(2) . . ?
N1 Ni1 N1 180.0 7_657 . ?
O7 Ni2 O8 108.4(2) 5_777 . ?
O7 Ni2 N6 94.6(3) 5_777 6_576 ?
O8 Ni2 N6 92.2(3) . 6_576 ?
O7 Ni2 N5 89.2(3) 5_777 . ?
O8 Ni2 N5 86.0(3) . . ?
N6 Ni2 N5 176.1(3) 6_576 . ?
O7 Ni2 O9 157.7(2) 5_777 . ?
O8 Ni2 O9 93.7(2) . . ?
N6 Ni2 O9 87.7(3) 6_576 . ?
N5 Ni2 O9 88.9(3) . . ?
O7 Ni2 O10 96.0(2) 5_777 . ?
O8 Ni2 O10 155.5(2) . . ?
N6 Ni2 O10 88.7(2) 6_576 . ?
N5 Ni2 O10 91.5(2) . . ?
O9 Ni2 O10 61.9(2) . . ?
O7 Ni2 C20 126.9(3) 5_777 . ?
O8 Ni2 C20 124.5(3) . . ?
N6 Ni2 C20 88.3(3) 6_576 . ?
N5 Ni2 C20 89.8(3) . . ?
O9 Ni2 C20 30.9(2) . . ?
O10 Ni2 C20 31.0(2) . . ?
C6 O1 Ni1 129.1(5) . . ?
C19 O7 Ni2 126.5(6) . 5_777 ?
C19 O8 Ni2 146.7(7) . . ?
C20 O9 Ni2 88.1(5) . . ?
C20 O10 Ni2 87.9(5) . . ?
O5 N2 O6 121.8(10) . . ?
O5 N2 C14 121.2(13) . . ?
O6 N2 C14 116.8(12) . . ?
O11 N4 O12 110.5(14) . . ?
O11 N4 C23 119.3(14) . . ?
O12 N4 C23 121.7(14) . . ?
O5' N2' O6' 117.6(13) . . ?
O5' N2' C14' 119.6(14) . . ?
O6' N2' C14' 122.7(13) . . ?
O12' N4' O11' 111.4(14) . . ?
O12' N4' C23' 122.8(13) . . ?
O11' N4' C23' 125.7(14) . . ?
Ni1 O13 H13A 109.4 . . ?
Ni1 O13 H13B 109.3 . . ?
H13A O13 H13B 109.5 . . ?
C29 C31 C30 114.0(10) . . ?
C29 C31 C32 122.6(9) . . ?
C30 C31 C32 123.4(9) . . ?
C31 C30 C28 121.2(10) . . ?
C31 C30 H30 119.4 . . ?
C28 C30 H30 119.4 . . ?
N5 C28 C30 122.7(9) . . ?
N5 C28 H28 118.7 . . ?
C30 C28 H28 118.7 . . ?
N5 C27 C29 123.0(11) . . ?
N5 C27 H27 118.5 . . ?
C29 C27 H27 118.5 . . ?
C31 C29 C27 122.5(11) . . ?
C31 C29 H29 118.7 . . ?
C27 C29 H29 118.7 . . ?
C34 C32 C33 116.7(9) . . ?
C34 C32 C31 121.9(8) . . ?
C33 C32 C31 121.4(9) . . ?
C35 C33 C32 120.9(9) . . ?
C35 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C32 C34 C36 118.6(9) . . ?
C32 C34 H34 120.7 . . ?
C36 C34 H34 120.7 . . ?
N6 C35 C33 123.6(9) . . ?
N6 C35 H35 118.2 . . ?
C33 C35 H35 118.2 . . ?
N6 C36 C34 124.1(10) . . ?
N6 C36 H36 117.9 . . ?
C34 C36 H36 117.9 . . ?
C36 N6 C35 116.1(9) . . ?
C36 N6 Ni2 122.1(7) . 6_575 ?
C35 N6 Ni2 121.8(6) . 6_575 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.0(11) . . . . ?
C1 C2 C3 C4 0.1(10) . . . . ?
C1 C2 C3 C3 178.8(5) . . . 2_656 ?
C2 C3 C4 C5 -0.5(10) . . . . ?
C3 C3 C4 C5 -179.2(5) 2_656 . . . ?
C3 C4 C5 N1 0.7(11) . . . . ?
O2 C6 C7 C12 -0.5(10) . . . . ?
O1 C6 C7 C12 177.5(7) . . . . ?
O2 C6 C7 C8 -178.2(7) . . . . ?
O1 C6 C7 C8 -0.3(10) . . . . ?
C12 C7 C8 C9 0.8(12) . . . . ?
C6 C7 C8 C9 178.5(8) . . . . ?
C7 C8 C9 C10 -0.9(14) . . . . ?
C8 C9 C10 C11 0.7(14) . . . . ?
C8 C9 C10 C13 -175.3(9) . . . . ?
C9 C10 C11 C12 -0.6(13) . . . . ?
C13 C10 C11 C12 175.4(8) . . . . ?
C9 C10 C11 N3 -179.6(9) . . . . ?
C13 C10 C11 N3 -3.6(14) . . . . ?
C8 C7 C12 C11 -0.7(11) . . . . ?
C6 C7 C12 C11 -178.4(7) . . . . ?
C10 C11 C12 C7 0.6(13) . . . . ?
N3 C11 C12 C7 179.6(8) . . . . ?
C11 C10 C13 C14' 126.0(14) . . . . ?
C9 C10 C13 C14' -58.2(17) . . . . ?
C11 C10 C13 C18 -80.2(13) . . . . ?
C9 C10 C13 C18 95.6(11) . . . . ?
C11 C10 C13 C14 80.6(13) . . . . ?
C9 C10 C13 C14 -103.6(13) . . . . ?
C15' C16 C17 C18 21.5(15) . . . . ?
C15 C16 C17 C18 -20.2(15) . . . . ?
C19 C16 C17 C18 179.3(9) . . . . ?
C14' C13 C18 C17 -24.5(16) . . . . ?
C10 C13 C18 C17 179.1(8) . . . . ?
C14 C13 C18 C17 17.0(15) . . . . ?
C16 C17 C18 C13 1.0(14) . . . . ?
C17 C16 C19 O8 174.4(9) . . . . ?
C15' C16 C19 O8 -29.5(17) . . . . ?
C15 C16 C19 O8 13.0(14) . . . . ?
C17 C16 C19 O7 -4.1(14) . . . . ?
C15' C16 C19 O7 152.0(13) . . . . ?
C15 C16 C19 O7 -165.5(10) . . . . ?
O9 C20 C21 C26 153.0(12) . . . . ?
O10 C20 C21 C26 -27.6(15) . . . . ?
O9 C20 C21 C22' 32.2(13) . . . . ?
O10 C20 C21 C22' -148.3(10) . . . . ?
O9 C20 C21 C26' -153.0(11) . . . . ?
O10 C20 C21 C26' 26.5(14) . . . . ?
O9 C20 C21 C22 -30.0(13) . . . . ?
O10 C20 C21 C22 149.4(10) . . . . ?
C18 C13 C14 N2 167.3(14) . . . . ?
C10 C13 C14 N2 6(2) . . . . ?
C18 C13 C14 C15 -17(2) . . . . ?
C10 C13 C14 C15 -178.5(14) . . . . ?
N2 C14 C15 C16 175.8(13) . . . . ?
C13 C14 C15 C16 0(2) . . . . ?
C17 C16 C15 C14 19(2) . . . . ?
C19 C16 C15 C14 -179.1(13) . . . . ?
C26 C21 C22 C23 -2(2) . . . . ?
C20 C21 C22 C23 -179.3(14) . . . . ?
C21 C22 C23 N4 -177.9(15) . . . . ?
C21 C22 C23 C24 -1(3) . . . . ?
C25 C24 C23 C22 2(2) . . . . ?
C24 C24 C23 C22 175.7(14) 2_656 . . . ?
C25 C24 C23 N4 178.5(17) . . . . ?
C24 C24 C23 N4 -8(2) 2_656 . . . ?
C23 C24 C25 C26 0(2) . . . . ?
C24 C24 C25 C26 -173.7(14) 2_656 . . . ?
C22 C21 C26 C25 5(2) . . . . ?
C20 C21 C26 C25 -178.4(13) . . . . ?
C24 C25 C26 C21 -4(3) . . . . ?
C18 C13 C14' N2' -163.1(15) . . . . ?
C10 C13 C14' N2' -8(3) . . . . ?
C18 C13 C14' C15' 25(2) . . . . ?
C10 C13 C14' C15' -179.5(15) . . . . ?
C17 C16 C15' C14' -21(2) . . . . ?
C19 C16 C15' C14' -179.0(16) . . . . ?
C13 C14' C15' C16 -3(3) . . . . ?
N2' C14' C15' C16 -175.1(17) . . . . ?
C26' C21 C22' C23' 5(2) . . . . ?
C20 C21 C22' C23' 179.8(12) . . . . ?
C25' C24 C23' N4' 170.8(15) . . . . ?
C24 C24 C23' N4' -2(2) 2_656 . . . ?
C25' C24 C23' C22' -6(2) . . . . ?
C24 C24 C23' C22' -178.5(14) 2_656 . . . ?
C21 C22' C23' C24 1(3) . . . . ?
C21 C22' C23' N4' -175.6(14) . . . . ?
C23' C24 C25' C26' 5(2) . . . . ?
C24 C24 C25' C26' 178.4(14) 2_656 . . . ?
C24 C25' C26' C21 1(2) . . . . ?
C22' C21 C26' C25' -6(2) . . . . ?
C20 C21 C26' C25' 179.3(13) . . . . ?
C4 C5 N1 C1 -0.6(10) . . . . ?
C4 C5 N1 Ni1 178.3(5) . . . . ?
C2 C1 N1 C5 0.2(10) . . . . ?
C2 C1 N1 Ni1 -178.7(6) . . . . ?
C10 C11 N3 O4 140.7(9) . . . . ?
C12 C11 N3 O4 -38.3(12) . . . . ?
C10 C11 N3 O3 -38.2(13) . . . . ?
C12 C11 N3 O3 142.7(9) . . . . ?
O2 C6 O1 Ni1 10.2(11) . . . . ?
C7 C6 O1 Ni1 -167.5(4) . . . . ?
O8 C19 O7 Ni2 -1.0(14) . . . 5_777 ?
C16 C19 O7 Ni2 177.3(6) . . . 5_777 ?
O7 C19 O8 Ni2 -82.6(14) . . . . ?
C16 C19 O8 Ni2 99.1(12) . . . . ?
O10 C20 O9 Ni2 -1.5(8) . . . . ?
C21 C20 O9 Ni2 177.9(6) . . . . ?
O9 C20 O10 Ni2 1.5(8) . . . . ?
C21 C20 O10 Ni2 -177.9(7) . . . . ?
C15 C14 N2 O5 -149.4(19) . . . . ?
C13 C14 N2 O5 27(2) . . . . ?
C15 C14 N2 O6 25(2) . . . . ?
C13 C14 N2 O6 -159.3(15) . . . . ?
C22 C23 N4 O11 -175.2(18) . . . . ?
C24 C23 N4 O11 8(3) . . . . ?
C22 C23 N4 O12 -30(3) . . . . ?
C24 C23 N4 O12 153.0(17) . . . . ?
C13 C14' N2' O5' -23(3) . . . . ?
C15' C14' N2' O5' 149.2(18) . . . . ?
C13 C14' N2' O6' 157.7(16) . . . . ?
C15' C14' N2' O6' -30(3) . . . . ?
C24 C23' N4' O12' 161.1(16) . . . . ?
C22' C23' N4' O12' -22(3) . . . . ?
C24 C23' N4' O11' -14(3) . . . . ?
C22' C23' N4' O11' 162.3(19) . . . . ?
C29 C31 C30 C28 -0.1(16) . . . . ?
C32 C31 C30 C28 -178.3(10) . . . . ?
C27 N5 C28 C30 -0.7(17) . . . . ?
Ni2 N5 C28 C30 177.4(9) . . . . ?
C31 C30 C28 N5 0.4(18) . . . . ?
C28 N5 C27 C29 0.7(18) . . . . ?
Ni2 N5 C27 C29 -177.5(11) . . . . ?
C30 C31 C29 C27 0.1(18) . . . . ?
C32 C31 C29 C27 178.3(11) . . . . ?
N5 C27 C29 C31 0(2) . . . . ?
C29 C31 C32 C34 148.0(11) . . . . ?
C30 C31 C32 C34 -33.9(14) . . . . ?
C29 C31 C32 C33 -29.9(15) . . . . ?
C30 C31 C32 C33 148.2(10) . . . . ?
C34 C32 C33 C35 1.1(13) . . . . ?
C31 C32 C33 C35 179.1(8) . . . . ?
C33 C32 C34 C36 -1.5(13) . . . . ?
C31 C32 C34 C36 -179.5(8) . . . . ?
C32 C33 C35 N6 0.9(15) . . . . ?
C32 C34 C36 N6 0.0(15) . . . . ?
C34 C36 N6 C35 1.9(14) . . . . ?
C34 C36 N6 Ni2 179.6(7) . . . 6_575 ?
C33 C35 N6 C36 -2.3(13) . . . . ?
C33 C35 N6 Ni2 179.9(7) . . . 6_575 ?

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.269 0.032 0.774 13.1 0.3
2 0.731 0.032 0.726 13.0 0.3
3 0.264 0.125 0.287 8.1 0.8
4 0.736 0.125 0.213 8.1 1.0
5 0.184 0.199 0.685 16.0 5.4
6 0.816 0.199 0.815 16.0 5.7
7 0.009 0.187 0.824 7.1 2.1
8 0.991 0.187 0.676 6.8 1.7
9 0.000 0.229 0.750 6.9 2.0
10 0.500 0.279 0.250 9.0 3.7
11 0.316 0.301 0.315 16.1 6.1
12 0.684 0.301 0.185 16.1 5.7
13 0.490 0.316 0.168 5.8 1.2
14 0.510 0.316 0.332 6.0 1.6
15 0.236 0.375 0.713 8.1 1.0
16 0.764 0.375 0.787 8.0 0.8
17 0.231 0.468 0.226 13.0 0.2
18 0.769 0.468 0.274 13.0 0.2
19 0.231 0.532 0.726 13.0 0.3
20 0.769 0.532 0.774 13.1 0.3
21 0.236 0.625 0.213 8.1 1.0
22 0.764 0.625 0.287 8.1 0.8
23 0.316 0.699 0.815 16.0 5.7
24 0.684 0.699 0.685 16.0 5.4
25 0.491 0.687 0.676 6.8 1.7
26 0.509 0.687 0.824 7.1 2.1
27 0.500 0.729 0.750 6.9 2.0
28 0.000 0.779 0.250 9.0 3.7
29 0.184 0.801 0.185 16.1 5.7
30 0.816 0.801 0.315 16.1 6.1
31 0.010 0.816 0.332 6.0 1.6
32 0.990 0.816 0.168 5.8 1.2
33 0.264 0.875 0.787 8.0 0.8
34 0.736 0.875 0.713 8.1 1.0
35 0.269 0.968 0.274 13.0 0.2
36 0.731 0.968 0.226 13.0 0.2
_platon_squeeze_details          
;
The contributions of 68/4 electrons per formula were assigned to be two water molecules in the CIF. 
;


_refine_diff_density_max         1.952
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.112

####################################################################### 
# 
# 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_112
_database_code_depnum_ccdc_archive 'CCDC 1434744'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;
_audit_creation_date             2015-04-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.25(C96 H56 N16 Ni4 O32)'
_chemical_formula_sum            'C24 H14 N4 Ni O8.02'
_chemical_formula_weight         545.34
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.5739(15)
_cell_length_b                   19.361(2)
_cell_length_c                   8.7636(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.1510(10)
_cell_angle_gamma                90.00
_cell_volume                     2289.9(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1617
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.794
_cell_measurement_theta_min      2.845
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.9476
_exptl_absorpt_correction_T_min  0.9147
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9041
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.84
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                1854
_reflns_number_total             2253
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         2.061
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2253
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0692
_refine_ls_restrained_S_all      1.216
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1083P)²+17.0554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.2003
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 O1, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 O2, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 N1, C9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O1 \\sim N1: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.02
O2 \\sim N1: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.02
N1 \\sim C9: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.01
Uanis(N1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C14(H14), C16(H16), C18(H18), C22(H22), C19(H19), C15(H15)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 0.5000 0.94242(5) 0.2500 0.0148(3) Uani 1 d . . 2 S T P
O0AA O 0.6103(3) 0.9371(2) 0.4305(4) 0.0240(9) Uani 1 d . . 1 . . .
O1AA O 0.5782(3) 1.0211(2) 0.1577(5) 0.0265(9) Uani 1 d . . 1 . . .
N1 N 0.9540(5) 0.8388(3) 0.5274(7) 0.0476(11) Uani 1 d . . 1 . U .
N2 N 0.5833(3) 0.8680(2) 0.1478(5) 0.0216(10) Uani 1 d . . 1 . . .
C1 C 0.7418(4) 0.9445(3) 0.6254(6) 0.0201(11) Uani 1 d . . 1 . . .
C3 C 0.6331(4) 0.9550(2) 0.5661(6) 0.0165(10) Uani 1 d . . 1 . . .
C5 C 0.7988(4) 0.8968(3) 0.5564(6) 0.0221(11) Uani 1 d . . 1 . . .
H5 H 0.7700 0.8694 0.4765 0.027 Uiso 1 calc . . 1 R . .
C9 C 0.8987(5) 0.8898(4) 0.6059(8) 0.0386(12) Uani 1 d . . 1 . U .
C10 C 0.9455(4) 0.9315(3) 0.7243(7) 0.0307(14) Uani 1 d . . 1 . . .
C14 C 0.6027(5) 0.8713(3) 0.0020(7) 0.0333(14) Uani 1 d . . 1 . . .
H14 H 0.5717 0.9052 -0.0612 0.040 Uiso 1 calc . . 1 R . .
C16 C 0.6284(5) 0.8178(3) 0.2348(7) 0.0281(13) Uani 1 d . . 1 . . .
H16 H 0.6150 0.8141 0.3363 0.034 Uiso 1 calc . . 1 R . .
C18 C 0.7862(4) 0.9845(4) 0.7435(8) 0.0394(17) Uani 1 d . . 1 . . .
H18 H 0.7484 1.0162 0.7921 0.047 Uiso 1 calc . . 1 R . .
C22 C 0.8863(5) 0.9780(4) 0.7901(9) 0.049(2) Uani 1 d . . 1 . . .
H22 H 0.9147 1.0062 0.8688 0.058 Uiso 1 calc . . 1 R . .
C13 C 0.7151(4) 0.7746(3) 0.0311(6) 0.0247(12) Uani 1 d . . 1 . . .
C19 C 0.6938(5) 0.7713(3) 0.1810(7) 0.0300(13) Uani 1 d . . 1 . . .
H19 H 0.7234 0.7376 0.2463 0.036 Uiso 1 calc . . 1 R . .
C15 C 0.6673(5) 0.8259(3) -0.0586(7) 0.0392(16) Uani 1 d . . 1 . . .
H15 H 0.6786 0.8300 -0.1610 0.047 Uiso 1 calc . . 1 R . .
O1 O 0.9104(5) 0.7887(3) 0.4724(8) 0.0720(16) Uani 1 d . . 1 . U .
O2 O 1.0413(5) 0.8481(4) 0.5173(9) 0.0847(17) Uani 1 d . . 1 . U .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O0AA 2.061(4) 2_655 ?
Ni1 O0AA 2.061(4) . ?
Ni1 O1AA 2.071(4) . ?
Ni1 O1AA 2.071(4) 2_655 ?
Ni1 N2 2.092(4) 2_655 ?
Ni1 N2 2.092(4) . ?
O0AA C3 1.244(6) . ?
O1AA C3 1.241(6) 6_575 ?
N1 C9 1.457(9) . ?
N1 O1 1.209(8) . ?
N1 O2 1.211(9) . ?
N2 C14 1.333(8) . ?
N2 C16 1.342(7) . ?
C1 C3 1.524(7) . ?
C1 C5 1.385(8) . ?
C1 C18 1.379(8) . ?
C3 O1AA 1.241(6) 6_576 ?
C5 H5 0.9300 . ?
C5 C9 1.386(8) . ?
C9 C10 1.410(9) . ?
C10 C10 1.500(10) 2_756 ?
C10 C22 1.375(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.387(8) . ?
C16 H16 0.9300 . ?
C16 C19 1.382(8) . ?
C18 H18 0.9300 . ?
C18 C22 1.383(9) . ?
C22 H22 0.9300 . ?
C13 C13 1.488(10) 7_665 ?
C13 C19 1.377(8) . ?
C13 C15 1.384(8) . ?
C19 H19 0.9300 . ?
C15 H15 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
O0AA Ni1 O0AA 174.3(2) 2_655 . ?
O0AA Ni1 O1AA 88.62(16) . . ?
O0AA Ni1 O1AA 95.61(15) . 2_655 ?
O0AA Ni1 O1AA 95.61(15) 2_655 . ?
O0AA Ni1 O1AA 88.62(16) 2_655 2_655 ?
O0AA Ni1 N2 91.08(17) . 2_655 ?
O0AA Ni1 N2 84.97(16) . . ?
O0AA Ni1 N2 91.08(17) 2_655 . ?
O0AA Ni1 N2 84.97(16) 2_655 2_655 ?
O1AA Ni1 O1AA 85.2(2) . 2_655 ?
O1AA Ni1 N2 176.11(16) 2_655 . ?
O1AA Ni1 N2 90.93(17) . . ?
O1AA Ni1 N2 90.93(17) 2_655 2_655 ?
O1AA Ni1 N2 176.11(16) . 2_655 ?
N2 Ni1 N2 92.9(3) 2_655 . ?
C3 O0AA Ni1 143.6(3) . . ?
C3 O1AA Ni1 153.5(4) 6_575 . ?
O1 N1 C9 118.5(7) . . ?
O1 N1 O2 122.1(7) . . ?
O2 N1 C9 119.4(7) . . ?
C14 N2 Ni1 123.2(4) . . ?
C14 N2 C16 117.1(5) . . ?
C16 N2 Ni1 119.4(4) . . ?
C5 C1 C3 120.4(5) . . ?
C18 C1 C3 120.6(5) . . ?
C18 C1 C5 118.9(5) . . ?
O0AA C3 C1 114.9(4) . . ?
O1AA C3 O0AA 128.0(5) 6_576 . ?
O1AA C3 C1 117.1(5) 6_576 . ?
C1 C5 H5 119.9 . . ?
C1 C5 C9 120.2(5) . . ?
C9 C5 H5 119.9 . . ?
C5 C9 N1 117.0(6) . . ?
C5 C9 C10 121.5(6) . . ?
C10 C9 N1 121.4(6) . . ?
C9 C10 C10 125.0(6) . 2_756 ?
C22 C10 C9 116.5(5) . . ?
C22 C10 C10 118.4(5) . 2_756 ?
N2 C14 H14 118.9 . . ?
N2 C14 C15 122.3(5) . . ?
C15 C14 H14 118.9 . . ?
N2 C16 H16 118.4 . . ?
N2 C16 C19 123.3(5) . . ?
C19 C16 H16 118.4 . . ?
C1 C18 H18 119.8 . . ?
C1 C18 C22 120.5(6) . . ?
C22 C18 H18 119.8 . . ?
C10 C22 C18 122.4(6) . . ?
C10 C22 H22 118.8 . . ?
C18 C22 H22 118.8 . . ?
C19 C13 C13 121.8(6) . 7_665 ?
C19 C13 C15 116.2(5) . . ?
C15 C13 C13 122.0(6) . 7_665 ?
C16 C19 H19 119.9 . . ?
C13 C19 C16 120.2(5) . . ?
C13 C19 H19 119.9 . . ?
C14 C15 H15 119.5 . . ?
C13 C15 C14 121.0(6) . . ?
C13 C15 H15 119.5 . . ?

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
Ni1 O0AA C3 O1AA 13.3(10) . . . 6_576 ?
Ni1 O0AA C3 C1 -168.0(4) . . . . ?
Ni1 N2 C14 C15 172.4(5) . . . . ?
Ni1 N2 C16 C19 -172.4(5) . . . . ?
O0AA Ni1 O0AA C3 -122.5(6) 2_655 . . . ?
O0AA Ni1 O1AA C3 -73.2(8) 2_655 . . 6_575 ?
O0AA Ni1 O1AA C3 102.9(8) . . . 6_575 ?
O0AA Ni1 N2 C14 49.6(5) 2_655 . . . ?
O0AA Ni1 N2 C14 -134.6(5) . . . . ?
O0AA Ni1 N2 C16 38.6(4) . . . . ?
O0AA Ni1 N2 C16 -137.3(4) 2_655 . . . ?
O1AA Ni1 O0AA C3 14.9(6) 2_655 . . . ?
O1AA Ni1 O0AA C3 99.9(6) . . . . ?
O1AA Ni1 O1AA C3 -161.4(9) 2_655 . . 6_575 ?
O1AA Ni1 N2 C14 -46.0(5) . . . . ?
O1AA Ni1 N2 C14 -36(3) 2_655 . . . ?
O1AA Ni1 N2 C16 127.1(4) . . . . ?
O1AA Ni1 N2 C16 137(2) 2_655 . . . ?
N1 C9 C10 C10 3.7(10) . . . 2_756 ?
N1 C9 C10 C22 179.8(7) . . . . ?
N2 Ni1 O0AA C3 -169.0(6) . . . . ?
N2 Ni1 O0AA C3 -76.2(6) 2_655 . . . ?
N2 Ni1 O1AA C3 -172(2) 2_655 . . 6_575 ?
N2 Ni1 O1AA C3 17.9(8) . . . 6_575 ?
N2 Ni1 N2 C14 134.6(5) 2_655 . . . ?
N2 Ni1 N2 C16 -52.3(4) 2_655 . . . ?
N2 C14 C15 C13 0.0(11) . . . . ?
N2 C16 C19 C13 -0.5(10) . . . . ?
C1 C5 C9 N1 -179.8(5) . . . . ?
C1 C5 C9 C10 -1.5(10) . . . . ?
C1 C18 C22 C10 -1.0(13) . . . . ?
C3 C1 C5 C9 176.9(5) . . . . ?
C3 C1 C18 C22 -175.6(7) . . . . ?
C5 C1 C3 O0AA -22.6(7) . . . . ?
C5 C1 C3 O1AA 156.2(5) . . . 6_576 ?
C5 C1 C18 C22 1.2(11) . . . . ?
C5 C9 C10 C10 -174.6(6) . . . 2_756 ?
C5 C9 C10 C22 1.5(10) . . . . ?
C9 C10 C22 C18 -0.3(12) . . . . ?
C10 C10 C22 C18 176.1(7) 2_756 . . . ?
C14 N2 C16 C19 1.1(9) . . . . ?
C16 N2 C14 C15 -0.8(10) . . . . ?
C18 C1 C3 O0AA 154.1(6) . . . . ?
C18 C1 C3 O1AA -27.0(8) . . . 6_576 ?
C18 C1 C5 C9 0.1(9) . . . . ?
C13 C13 C19 C16 -179.9(7) 7_665 . . . ?
C13 C13 C15 C14 -179.9(7) 7_665 . . . ?
C19 C13 C15 C14 0.7(10) . . . . ?
C15 C13 C19 C16 -0.5(9) . . . . ?
O1 N1 C9 C5 -29.1(10) . . . . ?
O1 N1 C9 C10 152.6(7) . . . . ?
O2 N1 C9 C5 149.9(8) . . . . ?
O2 N1 C9 C10 -28.4(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_11
_database_code_depnum_ccdc_archive 'CCDC 1434748'
_audit_update_record             
;
2016-01-29 deposited with the CCDC.
2016-02-09 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         'C24 H14 Mn N4 O8'
_chemical_formula_sum            'C24 H14 Mn N4 O8'
_chemical_formula_weight         541.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.827(3)
_cell_length_b                   19.685(4)
_cell_length_c                   8.9064(17)
_cell_angle_alpha                90
_cell_angle_beta                 97.320(3)
_cell_angle_gamma                90
_cell_volume                     2404.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1042
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      19.65
_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.606
_shelx_estimated_absorpt_T_min   0.942
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_process_details   sadabs
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8581
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.779
_diffrn_reflns_theta_max         24.785
_diffrn_reflns_theta_full        24.785
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2058
_reflns_number_gt                1462
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0485P)²+0.8039P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2058
_refine_ls_number_parameters     187
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1149
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.218
_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
Mn1 Mn 0.5000 1.05335(3) 0.2500 0.0256(2) Uani 1 2 d S T P . .
O1 O 0.41440(16) 0.97640(13) 0.3366(3) 0.0414(6) Uani 1 1 d . . . . .
O2 O 0.38826(15) 0.93408(12) 0.5596(3) 0.0388(6) Uani 1 1 d . . . . .
O3 O -0.0366(4) 0.8505(3) 0.4833(8) 0.1015(17) Uani 0.713(5) 1 d . U P A 1
O4 O 0.0941(3) 0.7886(3) 0.5194(6) 0.0769(15) Uani 0.713(5) 1 d . U P A 1
O3A O 0.0702(10) 0.8317(8) 0.6012(18) 0.100(2) Uani 0.287(5) 1 d . U P A 2
O4A O -0.0210(8) 0.8120(7) 0.3903(15) 0.073(2) Uani 0.287(5) 1 d . U P A 2
N1 N 0.0480(3) 0.8393(2) 0.4658(5) 0.0731(11) Uani 1 1 d . U . . .
N2 N 0.4131(2) 1.13485(14) 0.3564(3) 0.0373(7) Uani 1 1 d . . . . .
C1 C 0.3619(2) 0.95198(16) 0.4269(4) 0.0275(8) Uani 1 1 d . . . . .
C2 C 0.2550(2) 0.94321(17) 0.3702(4) 0.0299(8) Uani 1 1 d . . . . .
C3 C 0.2105(2) 0.9822(2) 0.2542(5) 0.0568(12) Uani 1 1 d . . . . .
H3 H 0.2470 1.0129 0.2055 0.068 Uiso 1 1 calc R U . . .
C4 C 0.1998(2) 0.89727(17) 0.4386(4) 0.0340(8) Uani 1 1 d . . . . .
H4 H 0.2290 0.8705 0.5177 0.041 Uiso 1 1 calc R U . . .
C5 C 0.1010(2) 0.89067(18) 0.3902(4) 0.0371(9) Uani 1 1 d . . . . .
C6 C 0.0539(2) 0.9305(2) 0.2749(4) 0.0412(10) Uani 1 1 d . . . . .
C7 C 0.1108(3) 0.9760(2) 0.2089(5) 0.0654(14) Uani 1 1 d . . . . .
H7 H 0.0817 1.0037 0.1313 0.079 Uiso 1 1 calc R U . . .
C8 C 0.3673(3) 1.18357(19) 0.2716(4) 0.0453(10) Uani 1 1 d . . . . .
H8 H 0.3795 1.1873 0.1716 0.054 Uiso 1 1 calc R U . . .
C9 C 0.3951(3) 1.1321(2) 0.4989(5) 0.0622(13) Uani 1 1 d . . . . .
H9 H 0.4263 1.0990 0.5620 0.075 Uiso 1 1 calc R U . . .
C10 C 0.3035(3) 1.22861(18) 0.3224(4) 0.0434(10) Uani 1 1 d . . . . .
H10 H 0.2733 1.2613 0.2572 0.052 Uiso 1 1 calc R U . . .
C11 C 0.3324(3) 1.1759(2) 0.5573(5) 0.0712(15) Uani 1 1 d . . . . .
H11 H 0.3227 1.1718 0.6584 0.085 Uiso 1 1 calc R U . . .
C12 C 0.2837(2) 1.22562(17) 0.4704(4) 0.0383(9) 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
Mn1 O1 2.127(2) . ?
Mn1 O1 2.127(2) 2_655 ?
Mn1 O2 2.158(2) 5_676 ?
Mn1 O2 2.158(2) 6_575 ?
Mn1 N2 2.282(3) . ?
Mn1 N2 2.282(3) 2_655 ?
O1 C1 1.247(4) . ?
O2 C1 1.242(4) . ?
O2 Mn1 2.158(2) 5_676 ?
O3 N1 1.220(6) . ?
O4 N1 1.245(6) . ?
O3A N1 1.215(15) . ?
O4A N1 1.220(11) . ?
N1 C5 1.463(5) . ?
N2 C9 1.324(4) . ?
N2 C8 1.330(4) . ?
C1 C2 1.510(4) . ?
C2 C3 1.368(5) . ?
C2 C4 1.374(4) . ?
C3 C7 1.392(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(5) . ?
C6 C7 1.373(5) . ?
C6 C6 1.499(6) 2 ?
C7 H7 0.9300 . ?
C8 C10 1.368(5) . ?
C8 H8 0.9300 . ?
C9 C11 1.373(5) . ?
C9 H9 0.9300 . ?
C10 C12 1.381(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.370(5) . ?
C11 H11 0.9300 . ?
C12 C12 1.481(6) 7_576 ?

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 Mn1 O1 89.15(14) . 2_655 ?
O1 Mn1 O2 99.94(9) . 5_676 ?
O1 Mn1 O2 89.48(9) 2_655 5_676 ?
O1 Mn1 O2 89.48(9) . 6_575 ?
O1 Mn1 O2 99.94(9) 2_655 6_575 ?
O2 Mn1 O2 166.83(13) 5_676 6_575 ?
O1 Mn1 N2 90.19(10) . . ?
O1 Mn1 N2 176.68(10) 2_655 . ?
O2 Mn1 N2 87.43(10) 5_676 . ?
O2 Mn1 N2 83.31(9) 6_575 . ?
O1 Mn1 N2 176.68(10) . 2_655 ?
O1 Mn1 N2 90.19(10) 2_655 2_655 ?
O2 Mn1 N2 83.31(9) 5_676 2_655 ?
O2 Mn1 N2 87.43(10) 6_575 2_655 ?
N2 Mn1 N2 90.65(15) . 2_655 ?
C1 O1 Mn1 154.9(2) . . ?
C1 O2 Mn1 144.0(2) . 5_676 ?
O3A N1 O4A 125.1(9) . . ?
O3 N1 O4 123.3(5) . . ?
O3A N1 C5 117.6(7) . . ?
O4A N1 C5 116.9(7) . . ?
O3 N1 C5 118.5(5) . . ?
O4 N1 C5 117.9(4) . . ?
C9 N2 C8 116.1(3) . . ?
C9 N2 Mn1 122.8(2) . . ?
C8 N2 Mn1 120.6(2) . . ?
O2 C1 O1 126.8(3) . . ?
O2 C1 C2 116.2(3) . . ?
O1 C1 C2 117.0(3) . . ?
C3 C2 C4 118.8(3) . . ?
C3 C2 C1 121.0(3) . . ?
C4 C2 C1 120.1(3) . . ?
C2 C3 C7 120.2(4) . . ?
C2 C3 H3 119.9 . . ?
C7 C3 H3 119.9 . . ?
C2 C4 C5 120.3(3) . . ?
C2 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 121.9(3) . . ?
C4 C5 N1 117.0(3) . . ?
C6 C5 N1 121.1(3) . . ?
C7 C6 C5 116.4(3) . . ?
C7 C6 C6 118.4(3) . 2 ?
C5 C6 C6 125.0(3) . 2 ?
C6 C7 C3 122.3(4) . . ?
C6 C7 H7 118.9 . . ?
C3 C7 H7 118.9 . . ?
N2 C8 C10 124.0(3) . . ?
N2 C8 H8 118.0 . . ?
C10 C8 H8 118.0 . . ?
N2 C9 C11 122.8(4) . . ?
N2 C9 H9 118.6 . . ?
C11 C9 H9 118.6 . . ?
C8 C10 C12 120.2(3) . . ?
C8 C10 H10 119.9 . . ?
C12 C10 H10 119.9 . . ?
C12 C11 C9 121.6(4) . . ?
C12 C11 H11 119.2 . . ?
C9 C11 H11 119.2 . . ?
C11 C12 C10 115.3(3) . . ?
C11 C12 C12 123.2(4) . 7_576 ?
C10 C12 C12 121.5(4) . 7_576 ?

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
Mn1 O2 C1 O1 21.3(6) 5_676 . . . ?
Mn1 O2 C1 C2 -158.5(3) 5_676 . . . ?
Mn1 O1 C1 O2 -72.1(7) . . . . ?
Mn1 O1 C1 C2 107.8(5) . . . . ?
O2 C1 C2 C3 155.3(4) . . . . ?
O1 C1 C2 C3 -24.5(5) . . . . ?
O2 C1 C2 C4 -22.3(5) . . . . ?
O1 C1 C2 C4 157.8(3) . . . . ?
C4 C2 C3 C7 1.2(6) . . . . ?
C1 C2 C3 C7 -176.5(4) . . . . ?
C3 C2 C4 C5 0.1(5) . . . . ?
C1 C2 C4 C5 177.9(3) . . . . ?
C2 C4 C5 C6 -1.4(6) . . . . ?
C2 C4 C5 N1 178.3(3) . . . . ?
O3A N1 C5 C4 38.0(12) . . . . ?
O4A N1 C5 C4 -148.6(9) . . . . ?
O3 N1 C5 C4 146.1(6) . . . . ?
O4 N1 C5 C4 -28.3(7) . . . . ?
O3A N1 C5 C6 -142.3(10) . . . . ?
O4A N1 C5 C6 31.1(10) . . . . ?
O3 N1 C5 C6 -34.1(7) . . . . ?
O4 N1 C5 C6 151.4(5) . . . . ?
C4 C5 C6 C7 1.3(6) . . . . ?
N1 C5 C6 C7 -178.4(4) . . . . ?
C4 C5 C6 C6 -174.6(3) . . . 2 ?
N1 C5 C6 C6 5.7(6) . . . 2 ?
C5 C6 C7 C3 0.1(7) . . . . ?
C6 C6 C7 C3 176.3(4) 2 . . . ?
C2 C3 C7 C6 -1.4(8) . . . . ?
C9 N2 C8 C10 -1.1(6) . . . . ?
Mn1 N2 C8 C10 170.9(3) . . . . ?
C8 N2 C9 C11 0.7(7) . . . . ?
Mn1 N2 C9 C11 -171.1(4) . . . . ?
N2 C8 C10 C12 0.6(6) . . . . ?
N2 C9 C11 C12 0.3(8) . . . . ?
C9 C11 C12 C10 -0.9(7) . . . . ?
C9 C11 C12 C12 -179.3(5) . . . 7_576 ?
C8 C10 C12 C11 0.5(6) . . . . ?
C8 C10 C12 C12 178.9(4) . . . 7_576 ?

_refine_diff_density_max         0.352
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_2222
_database_code_depnum_ccdc_archive 'CCDC 1434749'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;
_audit_creation_date             2015-04-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C12 H7 Co0.5 N2 O4.18'
_chemical_formula_sum            'C12 H7 Co0.50 N2 O4.18'
_chemical_formula_weight         275.54
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.641(4)
_cell_length_b                   19.536(5)
_cell_length_c                   8.806(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.639(3)
_cell_angle_gamma                90.00
_cell_volume                     2331.0(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.82
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_correction_T_min  0.9765
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9086
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.82
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                1997
_reflns_number_total             2281
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.856
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2281
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.237
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0671P)²+8.7857P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1344
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 O28, N15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N15, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
O28 \\sim N15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N15) \\sim Ueq, Uanis(O5C) \\sim Ueq, Uanis(O5D) \\sim Ueq, Uanis(O28)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(O5D)=1-FVAR(1)
 Sof(O5C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C18(H18), C20(H20), C23(H23), C33(H33)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.0000 -0.05667(3) 1.2500 0.0178(2) Uani 1 d . . 2 S T P
O1 O 0.07981(18) 0.02150(14) 1.1586(3) 0.0305(6) Uani 1 d . . 1 . . .
O2 O -0.10988(17) -0.06371(14) 1.0666(3) 0.0283(6) Uani 1 d . . 1 . . .
H8 H 0.272(5) 0.128(3) 0.981(7) 0.08(3) Uiso 1.00(14) d A 1 1 . U .
O28 O 0.4086(3) 0.2109(3) 0.9757(6) 0.0797(11) Uani 1 d . . 1 . U .
N3 N 0.0847(2) -0.13316(15) 1.1466(3) 0.0258(6) Uani 1 d . . 1 . . .
N15 N 0.4535(3) 0.1603(2) 1.0306(5) 0.0521(9) Uani 1 d B . 1 . U .
C1 C 0.1341(2) 0.04559(16) 1.0684(4) 0.0199(7) Uani 1 d . . 1 . . .
C2 C 0.2869(3) 0.0155(3) 1.2443(5) 0.0444(12) Uani 1 d B . 1 . . .
H2 H 0.2496 -0.0158 1.2929 0.053 Uiso 1 calc . . 1 R . .
C3 C 0.1679(4) -0.1741(2) 0.9412(5) 0.0486(13) Uani 1 d . . 1 . . .
H3 H 0.1790 -0.1696 0.8395 0.058 Uiso 1 calc . . 1 R . .
C5 C 0.2424(2) 0.05534(18) 1.1264(4) 0.0241(7) Uani 1 d . . 1 . . .
C8 C 0.2987(3) 0.1025(2) 1.0583(4) 0.0262(8) Uani 1 d B . 1 . . .
C9 C 0.4456(3) 0.0687(2) 1.2245(5) 0.0344(9) Uani 1 d . . 1 . . .
C10 C 0.2154(3) -0.22543(19) 1.0303(4) 0.0299(8) Uani 1 d . . 1 . . .
C14 C 0.3984(3) 0.1094(2) 1.1079(4) 0.0313(8) Uani 1 d . . 1 . U .
C18 C 0.1042(3) -0.1297(2) 1.0022(5) 0.0407(10) Uani 1 d . . 1 . . .
H18 H 0.0735 -0.0958 0.9395 0.049 Uiso 1 calc . . 1 R . .
C20 C 0.1945(3) -0.2287(2) 1.1806(5) 0.0358(9) Uani 1 d . . 1 . . .
H20 H 0.2245 -0.2618 1.2462 0.043 Uiso 1 calc . . 1 R . .
C23 C 0.1292(3) -0.1828(2) 1.2326(4) 0.0334(9) Uani 1 d . . 1 . . .
H23 H 0.1155 -0.1867 1.3333 0.040 Uiso 1 calc . . 1 R . .
C33 C 0.3872(3) 0.0222(3) 1.2905(6) 0.0520(13) Uani 1 d . . 1 . . .
H33 H 0.4162 -0.0057 1.3688 0.062 Uiso 1 calc B . 1 R . .
O5B O 0.431(2) 0.1674(14) 0.889(3) 0.082(12) Uiso 0.180(16) d B 3 1 . U .
O5C O 0.5407(4) 0.1470(4) 1.0106(8) 0.068(2) Uani 0.641(14) d B 4 1 . U .
O5D O 0.5279(9) 0.1842(6) 1.0931(15) 0.066(4) Uani 0.359(14) d B 5 1 . 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 2.090(3) . ?
Co1 O1 2.090(3) 2_557 ?
Co1 O2 2.077(2) 2_557 ?
Co1 O2 2.077(2) . ?
Co1 N3 2.154(3) . ?
Co1 N3 2.154(3) 2_557 ?
O1 C1 1.240(4) . ?
O2 C1 1.247(4) 5_557 ?
O28 N15 1.232(6) . ?
O28 O5B 1.20(3) . ?
N3 C18 1.331(5) . ?
N3 C23 1.333(5) . ?
N15 C14 1.461(6) . ?
N15 O5B 1.25(3) . ?
N15 O5C 1.250(7) . ?
N15 O5D 1.192(12) . ?
C1 O2 1.247(4) 5_557 ?
C1 C5 1.518(4) . ?
C2 H2 0.9300 . ?
C2 C5 1.381(5) . ?
C2 C33 1.388(6) . ?
C3 H3 0.9300 . ?
C3 C10 1.387(5) . ?
C3 C18 1.380(6) . ?
C5 C8 1.381(5) . ?
C8 H8 0.89(6) . ?
C8 C14 1.386(5) . ?
C9 C9 1.500(7) 2_657 ?
C9 C14 1.396(6) . ?
C9 C33 1.380(6) . ?
C10 C10 1.487(7) 7_547 ?
C10 C20 1.387(5) . ?
C18 H18 0.9300 . ?
C20 H20 0.9300 . ?
C20 C23 1.380(5) . ?
C23 H23 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 O1 86.10(15) . 2_557 ?
O1 Co1 N3 90.89(11) . . ?
O1 Co1 N3 176.77(11) 2_557 . ?
O1 Co1 N3 176.77(11) . 2_557 ?
O1 Co1 N3 90.89(11) 2_557 2_557 ?
O2 Co1 O1 96.33(10) . . ?
O2 Co1 O1 89.23(10) 2_557 . ?
O2 Co1 O1 89.23(10) . 2_557 ?
O2 Co1 O1 96.33(10) 2_557 2_557 ?
O2 Co1 O2 172.41(15) 2_557 . ?
O2 Co1 N3 84.77(11) 2_557 . ?
O2 Co1 N3 89.96(11) . . ?
O2 Co1 N3 89.96(11) 2_557 2_557 ?
O2 Co1 N3 84.77(11) . 2_557 ?
N3 Co1 N3 92.15(17) 2_557 . ?
C1 O1 Co1 154.2(2) . . ?
C1 O2 Co1 144.1(2) 5_557 . ?
O5B O28 N15 62.0(13) . . ?
C18 N3 Co1 123.0(3) . . ?
C18 N3 C23 116.9(3) . . ?
C23 N3 Co1 119.7(2) . . ?
O28 N15 C14 118.0(4) . . ?
O28 N15 O5B 57.8(13) . . ?
O28 N15 O5C 123.3(5) . . ?
O5B N15 C14 117.1(13) . . ?
O5C N15 C14 118.3(5) . . ?
O5C N15 O5B 90.8(13) . . ?
O5D N15 O28 103.0(7) . . ?
O5D N15 C14 120.5(7) . . ?
O5D N15 O5B 120.9(14) . . ?
O5D N15 O5C 51.1(7) . . ?
O1 C1 O2 127.3(3) . 5_557 ?
O1 C1 C5 117.5(3) . . ?
O2 C1 C5 115.2(3) 5_557 . ?
C5 C2 H2 120.0 . . ?
C5 C2 C33 120.0(4) . . ?
C33 C2 H2 120.0 . . ?
C10 C3 H3 119.7 . . ?
C18 C3 H3 119.7 . . ?
C18 C3 C10 120.6(4) . . ?
C2 C5 C1 120.6(3) . . ?
C8 C5 C1 120.4(3) . . ?
C8 C5 C2 119.0(3) . . ?
C5 C8 H8 121(4) . . ?
C5 C8 C14 120.2(4) . . ?
C14 C8 H8 119(4) . . ?
C14 C9 C9 125.2(4) . 2_657 ?
C33 C9 C9 118.2(3) . 2_657 ?
C33 C9 C14 116.5(3) . . ?
C3 C10 C10 122.6(4) . 7_547 ?
C3 C10 C20 116.0(3) . . ?
C20 C10 C10 121.4(4) . 7_547 ?
C8 C14 N15 117.2(4) . . ?
C8 C14 C9 121.9(4) . . ?
C9 C14 N15 120.8(3) . . ?
N3 C18 C3 123.0(4) . . ?
N3 C18 H18 118.5 . . ?
C3 C18 H18 118.5 . . ?
C10 C20 H20 120.1 . . ?
C23 C20 C10 119.9(4) . . ?
C23 C20 H20 120.1 . . ?
N3 C23 C20 123.6(4) . . ?
N3 C23 H23 118.2 . . ?
C20 C23 H23 118.2 . . ?
C2 C33 H33 118.8 . . ?
C9 C33 C2 122.4(4) . . ?
C9 C33 H33 118.8 . . ?
O28 O5B N15 60.2(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O1 C1 O2 79.3(7) . . . 5_557 ?
Co1 O1 C1 C5 -101.4(5) . . . . ?
Co1 N3 C18 C3 172.1(4) . . . . ?
Co1 N3 C23 C20 -171.7(3) . . . . ?
O1 Co1 O1 C1 -159.7(6) 2_557 . . . ?
O1 Co1 O2 C1 11.6(4) . . . 5_557 ?
O1 Co1 O2 C1 97.6(4) 2_557 . . 5_557 ?
O1 Co1 N3 C18 -45.8(3) . . . . ?
O1 Co1 N3 C18 -25(2) 2_557 . . . ?
O1 Co1 N3 C23 126.7(3) . . . . ?
O1 Co1 N3 C23 147.7(18) 2_557 . . . ?
O1 C1 C5 C2 25.8(5) . . . . ?
O1 C1 C5 C8 -156.5(3) . . . . ?
O2 Co1 O1 C1 -70.9(5) . . . . ?
O2 Co1 O1 C1 104.0(5) 2_557 . . . ?
O2 Co1 O2 C1 -125.2(4) 2_557 . . 5_557 ?
O2 Co1 N3 C18 -135.0(3) 2_557 . . . ?
O2 Co1 N3 C18 50.5(3) . . . . ?
O2 Co1 N3 C23 37.6(3) 2_557 . . . ?
O2 Co1 N3 C23 -136.9(3) . . . . ?
O2 C1 C5 C2 -154.8(4) 5_557 . . . ?
O2 C1 C5 C8 22.9(5) 5_557 . . . ?
O28 N15 C14 C8 29.0(6) . . . . ?
O28 N15 C14 C9 -152.3(5) . . . . ?
N3 Co1 O1 C1 19.2(5) . . . . ?
N3 Co1 O1 C1 179(100) 2_557 . . . ?
N3 Co1 O2 C1 -171.4(4) 2_557 . . 5_557 ?
N3 Co1 O2 C1 -79.3(4) . . . 5_557 ?
N3 Co1 N3 C18 135.3(4) 2_557 . . . ?
N3 Co1 N3 C23 -52.2(3) 2_557 . . . ?
C1 C5 C8 C14 -177.5(3) . . . . ?
C2 C5 C8 C14 0.2(6) . . . . ?
C3 C10 C20 C23 0.5(7) . . . . ?
C5 C2 C33 C9 1.3(8) . . . . ?
C5 C8 C14 N15 179.9(4) . . . . ?
C5 C8 C14 C9 1.3(6) . . . . ?
C9 C9 C14 N15 -4.2(6) 2_657 . . . ?
C9 C9 C14 C8 174.5(4) 2_657 . . . ?
C9 C9 C33 C2 -176.0(5) 2_657 . . . ?
C10 C3 C18 N3 -0.1(8) . . . . ?
C10 C10 C20 C23 -179.3(5) 7_547 . . . ?
C10 C20 C23 N3 -1.3(7) . . . . ?
C14 N15 O5B O28 107.5(10) . . . . ?
C14 C9 C33 C2 0.1(8) . . . . ?
C18 N3 C23 C20 1.3(6) . . . . ?
C18 C3 C10 C10 179.9(5) . . . 7_547 ?
C18 C3 C10 C20 0.2(7) . . . . ?
C23 N3 C18 C3 -0.7(7) . . . . ?
C33 C2 C5 C1 176.3(4) . . . . ?
C33 C2 C5 C8 -1.4(7) . . . . ?
C33 C9 C14 N15 180.0(4) . . . . ?
C33 C9 C14 C8 -1.4(6) . . . . ?
O5B O28 N15 C14 -106.0(15) . . . . ?
O5B O28 N15 O5C 66.8(16) . . . . ?
O5B O28 N15 O5D 118.6(17) . . . . ?
O5B N15 C14 C8 -37.0(16) . . . . ?
O5B N15 C14 C9 141.7(15) . . . . ?
O5C N15 C14 C8 -144.1(6) . . . . ?
O5C N15 C14 C9 34.6(7) . . . . ?
O5C N15 O5B O28 -129.8(9) . . . . ?
O5D N15 C14 C8 156.5(9) . . . . ?
O5D N15 C14 C9 -24.8(10) . . . . ?
O5D N15 O5B O28 -86.1(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pqj_zhou_nicl2_0m
_database_code_depnum_ccdc_archive 'CCDC 1434751'
_audit_update_record             
;
2016-01-29 deposited with the CCDC.
2016-02-09 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 O26, 2(H2 O)'
_chemical_formula_sum            'C24 H32 N4 Ni O17'
_chemical_formula_weight         707.24

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   7.361(2)
_cell_length_b                   15.645(3)
_cell_length_c                   26.957(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3104.4(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3365
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      20.12

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_F_000             1472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.708
_shelx_estimated_absorpt_T_min   0.826
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26930
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.505
_diffrn_reflns_theta_max         27.677
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7089
_reflns_number_gt                4415
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_max     0.963
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0240P)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_abs_structure_details 
;
 Flack x determined using 1398 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7089
_refine_ls_number_parameters     343
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1157
_refine_ls_wR_factor_gt          0.1093
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.189
_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 0.48950(9) 0.65587(5) 0.68717(2) 0.03925(19) Uani 1 1 d . . . . .
O1 O 0.3887(5) 0.6430(3) 0.61404(13) 0.0548(11) Uani 1 1 d . . . . .
O2 O 0.6014(5) 0.5562(3) 0.64209(13) 0.0547(11) Uani 1 1 d . . . . .
O3 O 0.6210(4) 0.6357(2) 0.75192(12) 0.0413(9) Uani 1 1 d . . . . .
O4 O 0.8563(6) 0.7228(3) 0.75000(14) 0.0644(13) Uani 1 1 d . . . . .
O5 O 0.0869(8) 0.5571(6) 0.4582(2) 0.152(3) Uani 1 1 d . U . . .
O6 O 0.2806(8) 0.5468(5) 0.39648(19) 0.121(2) Uani 1 1 d . U . . .
O7 O 1.3251(8) 0.6813(6) 0.8722(3) 0.167(3) Uani 1 1 d . U . . .
O8 O 1.2657(8) 0.6431(5) 0.9438(2) 0.130(2) Uani 1 1 d . U . . .
O9 O 0.7004(5) 0.7380(3) 0.66324(14) 0.0623(12) Uani 1 1 d . . . . .
H9A H 0.7912 0.7412 0.6887 0.075 Uiso 1 1 d R U . . .
H9B H 0.6521 0.7941 0.6571 0.075 Uiso 1 1 d R U . . .
N1 N 0.3440(6) 0.7609(3) 0.70996(17) 0.0442(12) Uani 1 1 d . . . . .
N2 N 0.2907(6) 0.5716(3) 0.71141(16) 0.0438(12) Uani 1 1 d . . . . .
N3 N 0.2413(9) 0.5401(5) 0.4404(2) 0.103(2) Uani 1 1 d . U . . .
N4 N 1.2155(9) 0.6560(6) 0.9034(3) 0.113(2) Uani 1 1 d . U . . .
C1 C 0.3420(8) 0.7896(4) 0.7564(2) 0.0540(17) Uani 1 1 d . . . . .
H1 H 0.4207 0.7646 0.7792 0.065 Uiso 1 1 calc R U . . .
C2 C 0.2326(8) 0.7998(4) 0.6777(2) 0.0523(16) Uani 1 1 d . . . . .
H2 H 0.2370 0.7832 0.6446 0.063 Uiso 1 1 calc R U . . .
C3 C 0.2316(7) 0.8533(4) 0.7723(2) 0.0577(17) Uani 1 1 d . . . . .
H3 H 0.2389 0.8722 0.8050 0.069 Uiso 1 1 calc R U . . .
C4 C 0.1136(8) 0.8620(4) 0.6909(2) 0.0534(16) Uani 1 1 d . . . . .
H4 H 0.0364 0.8857 0.6673 0.064 Uiso 1 1 calc R U . . .
C5 C 0.1072(7) 0.8906(4) 0.7399(2) 0.0469(15) Uani 1 1 d . . . . .
C6 C 0.0278(7) 0.4554(4) 0.74336(18) 0.0406(13) Uani 1 1 d . . . . .
C7 C 0.2005(8) 0.4520(4) 0.7620(2) 0.0565(17) Uani 1 1 d . . . . .
H7 H 0.2323 0.4111 0.7854 0.068 Uiso 1 1 calc R U . . .
C8 C -0.0161(8) 0.5153(3) 0.7084(2) 0.0487(14) Uani 1 1 d . . . . .
H8 H -0.1321 0.5178 0.6948 0.058 Uiso 1 1 calc R U . . .
C9 C 0.3287(8) 0.5115(4) 0.7450(2) 0.0488(16) Uani 1 1 d . . . . .
H9 H 0.4459 0.5090 0.7578 0.059 Uiso 1 1 calc R U . . .
C10 C 0.1195(7) 0.5726(4) 0.6939(2) 0.0468(14) Uani 1 1 d . . . . .
H10 H 0.0895 0.6142 0.6706 0.056 Uiso 1 1 calc R U . . .
C11 C 0.4968(9) 0.5817(4) 0.60780(19) 0.0541(15) Uani 1 1 d . . . . .
C12 C 0.5066(10) 0.5392(4) 0.55684(18) 0.0578(15) Uani 1 1 d . . . . .
C13 C 0.6412(8) 0.4828(4) 0.54632(19) 0.0520(16) Uani 1 1 d . . . . .
H13 H 0.7249 0.4674 0.5706 0.062 Uiso 1 1 calc R U . . .
C14 C 0.6531(9) 0.4480(4) 0.4989(2) 0.0609(18) Uani 1 1 d . . . . .
H14 H 0.7495 0.4118 0.4914 0.073 Uiso 1 1 calc R U . . .
C15 C 0.5259(9) 0.4658(4) 0.46254(19) 0.0558(16) Uani 1 1 d . . . . .
C16 C 0.3839(8) 0.5180(4) 0.4765(2) 0.0601(18) Uani 1 1 d . . . . .
C17 C 0.3731(9) 0.5545(5) 0.5229(2) 0.069(2) Uani 1 1 d . . . . .
H17 H 0.2753 0.5894 0.5310 0.083 Uiso 1 1 calc R U . . .
C18 C 0.7644(7) 0.6678(3) 0.76936(18) 0.0358(12) Uani 1 1 d . . . . .
C19 C 0.8233(7) 0.6312(3) 0.81801(18) 0.0388(13) Uani 1 1 d . . . . .
C20 C 0.9878(8) 0.6548(4) 0.83744(18) 0.0570(15) Uani 1 1 d . . . . .
H20 H 1.0633 0.6917 0.8199 0.068 Uiso 1 1 calc R U . . .
C21 C 1.0421(8) 0.6233(4) 0.8838(2) 0.0602(18) Uani 1 1 d . . . . .
C22 C 0.9361(8) 0.5682(4) 0.9109(2) 0.0531(17) Uani 1 1 d . . . . .
C23 C 0.7715(8) 0.5433(4) 0.8912(2) 0.0539(16) Uani 1 1 d . . . . .
H23 H 0.6982 0.5047 0.9082 0.065 Uiso 1 1 calc R U . . .
C24 C 0.7145(8) 0.5771(4) 0.8445(2) 0.0512(16) Uani 1 1 d . . . . .
H24 H 0.6013 0.5620 0.8319 0.061 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
Ni1 O3 2.021(3) . ?
Ni1 N1 2.055(5) . ?
Ni1 N2 2.075(5) . ?
Ni1 O1 2.116(3) . ?
Ni1 O9 2.116(4) . ?
Ni1 O2 2.142(4) . ?
O1 C11 1.257(7) . ?
O2 C11 1.268(6) . ?
O3 C18 1.260(6) . ?
O4 C18 1.213(6) . ?
O5 N3 1.263(8) . ?
O6 N3 1.223(7) . ?
O7 N4 1.231(7) . ?
O8 N4 1.166(6) . ?
O9 H9A 0.9600 . ?
O9 H9B 0.9600 . ?
N1 C1 1.330(7) . ?
N1 C2 1.341(6) . ?
N2 C9 1.335(7) . ?
N2 C10 1.346(6) . ?
N3 C16 1.473(8) . ?
N4 C21 1.474(8) . ?
C1 C3 1.356(8) . ?
C1 H1 0.9300 . ?
C2 C4 1.357(7) . ?
C2 H2 0.9300 . ?
C3 C5 1.393(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.490(7) 4_556 ?
C6 C7 1.368(8) . ?
C6 C8 1.368(7) . ?
C6 C5 1.490(7) 4_546 ?
C7 C9 1.402(8) . ?
C7 H7 0.9300 . ?
C8 C10 1.398(8) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.528(7) . ?
C12 C13 1.357(8) . ?
C12 C17 1.364(8) . ?
C13 C14 1.393(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.383(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.379(8) . ?
C15 C22 1.517(7) 2_664 ?
C16 C17 1.376(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.495(7) . ?
C19 C24 1.367(7) . ?
C19 C20 1.370(7) . ?
C20 C21 1.401(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.372(8) . ?
C22 C23 1.379(8) . ?
C22 C15 1.518(7) 2_665 ?
C23 C24 1.429(7) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ni1 N1 96.68(17) . . ?
O3 Ni1 N2 88.09(16) . . ?
N1 Ni1 N2 92.64(18) . . ?
O3 Ni1 O1 163.32(16) . . ?
N1 Ni1 O1 99.89(17) . . ?
N2 Ni1 O1 89.18(17) . . ?
O3 Ni1 O9 90.38(14) . . ?
N1 Ni1 O9 89.31(18) . . ?
N2 Ni1 O9 177.64(18) . . ?
O1 Ni1 O9 91.78(15) . . ?
O3 Ni1 O2 101.08(15) . . ?
N1 Ni1 O2 162.20(16) . . ?
N2 Ni1 O2 89.26(17) . . ?
O1 Ni1 O2 62.42(15) . . ?
O9 Ni1 O2 89.28(16) . . ?
C11 O1 Ni1 88.6(3) . . ?
C11 O2 Ni1 87.1(3) . . ?
C18 O3 Ni1 131.4(3) . . ?
Ni1 O9 H9A 108.9 . . ?
Ni1 O9 H9B 109.6 . . ?
H9A O9 H9B 109.5 . . ?
C1 N1 C2 116.7(5) . . ?
C1 N1 Ni1 123.9(4) . . ?
C2 N1 Ni1 119.2(4) . . ?
C9 N2 C10 116.3(5) . . ?
C9 N2 Ni1 120.9(4) . . ?
C10 N2 Ni1 122.8(4) . . ?
O6 N3 O5 124.3(7) . . ?
O6 N3 C16 119.5(6) . . ?
O5 N3 C16 116.0(6) . . ?
O8 N4 O7 119.0(7) . . ?
O8 N4 C21 123.4(7) . . ?
O7 N4 C21 115.7(6) . . ?
N1 C1 C3 123.6(6) . . ?
N1 C1 H1 118.2 . . ?
C3 C1 H1 118.2 . . ?
N1 C2 C4 123.4(5) . . ?
N1 C2 H2 118.3 . . ?
C4 C2 H2 118.3 . . ?
C1 C3 C5 120.2(6) . . ?
C1 C3 H3 119.9 . . ?
C5 C3 H3 119.9 . . ?
C2 C4 C5 120.0(5) . . ?
C2 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C5 C4 115.9(6) . . ?
C3 C5 C6 122.3(5) . 4_556 ?
C4 C5 C6 121.8(5) . 4_556 ?
C7 C6 C8 119.9(6) . . ?
C7 C6 C5 118.9(5) . 4_546 ?
C8 C6 C5 121.1(5) . 4_546 ?
C6 C7 C9 118.7(6) . . ?
C6 C7 H7 120.6 . . ?
C9 C7 H7 120.6 . . ?
C6 C8 C10 117.6(5) . . ?
C6 C8 H8 121.2 . . ?
C10 C8 H8 121.2 . . ?
N2 C9 C7 123.2(5) . . ?
N2 C9 H9 118.4 . . ?
C7 C9 H9 118.4 . . ?
N2 C10 C8 124.3(5) . . ?
N2 C10 H10 117.9 . . ?
C8 C10 H10 117.9 . . ?
O1 C11 O2 121.8(5) . . ?
O1 C11 C12 118.9(5) . . ?
O2 C11 C12 119.3(5) . . ?
C13 C12 C17 120.0(5) . . ?
C13 C12 C11 120.4(6) . . ?
C17 C12 C11 119.5(6) . . ?
C12 C13 C14 119.4(5) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C15 C14 C13 122.0(6) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C16 C15 C14 116.0(5) . . ?
C16 C15 C22 126.7(5) . 2_664 ?
C14 C15 C22 117.1(5) . 2_664 ?
C17 C16 C15 122.5(6) . . ?
C17 C16 N3 117.5(6) . . ?
C15 C16 N3 119.9(5) . . ?
C12 C17 C16 119.7(6) . . ?
C12 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
O4 C18 O3 126.1(5) . . ?
O4 C18 C19 119.2(5) . . ?
O3 C18 C19 114.7(5) . . ?
C24 C19 C20 119.0(5) . . ?
C24 C19 C18 121.7(5) . . ?
C20 C19 C18 119.2(5) . . ?
C19 C20 C21 119.8(6) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 122.2(5) . . ?
C22 C21 N4 121.2(5) . . ?
C20 C21 N4 116.5(6) . . ?
C21 C22 C23 118.2(5) . . ?
C21 C22 C15 127.2(5) . 2_665 ?
C23 C22 C15 114.5(6) . 2_665 ?
C22 C23 C24 119.4(6) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C19 C24 C23 121.2(5) . . ?
C19 C24 H24 119.4 . . ?
C23 C24 H24 119.4 . . ?

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
C2 N1 C1 C3 1.8(9) . . . . ?
Ni1 N1 C1 C3 -172.9(5) . . . . ?
C1 N1 C2 C4 -4.0(9) . . . . ?
Ni1 N1 C2 C4 171.0(4) . . . . ?
N1 C1 C3 C5 2.2(10) . . . . ?
N1 C2 C4 C5 2.2(9) . . . . ?
C1 C3 C5 C4 -3.9(9) . . . . ?
C1 C3 C5 C6 174.6(6) . . . 4_556 ?
C2 C4 C5 C3 1.8(8) . . . . ?
C2 C4 C5 C6 -176.7(5) . . . 4_556 ?
C8 C6 C7 C9 0.8(9) . . . . ?
C5 C6 C7 C9 178.1(5) 4_546 . . . ?
C7 C6 C8 C10 -1.4(8) . . . . ?
C5 C6 C8 C10 -178.6(5) 4_546 . . . ?
C10 N2 C9 C7 -0.2(9) . . . . ?
Ni1 N2 C9 C7 -178.8(5) . . . . ?
C6 C7 C9 N2 0.0(10) . . . . ?
C9 N2 C10 C8 -0.5(8) . . . . ?
Ni1 N2 C10 C8 178.1(4) . . . . ?
C6 C8 C10 N2 1.3(8) . . . . ?
Ni1 O1 C11 O2 1.1(6) . . . . ?
Ni1 O1 C11 C12 -176.7(6) . . . . ?
Ni1 O2 C11 O1 -1.0(6) . . . . ?
Ni1 O2 C11 C12 176.7(6) . . . . ?
O1 C11 C12 C13 169.1(6) . . . . ?
O2 C11 C12 C13 -8.7(10) . . . . ?
O1 C11 C12 C17 -14.6(10) . . . . ?
O2 C11 C12 C17 167.5(6) . . . . ?
C17 C12 C13 C14 7.0(10) . . . . ?
C11 C12 C13 C14 -176.7(6) . . . . ?
C12 C13 C14 C15 -3.5(10) . . . . ?
C13 C14 C15 C16 -1.7(10) . . . . ?
C13 C14 C15 C22 173.8(6) . . . 2_664 ?
C14 C15 C16 C17 3.5(11) . . . . ?
C22 C15 C16 C17 -171.5(7) 2_664 . . . ?
C14 C15 C16 N3 -179.7(6) . . . . ?
C22 C15 C16 N3 5.3(11) 2_664 . . . ?
O6 N3 C16 C17 144.6(8) . . . . ?
O5 N3 C16 C17 -30.3(11) . . . . ?
O6 N3 C16 C15 -32.3(12) . . . . ?
O5 N3 C16 C15 152.7(8) . . . . ?
C13 C12 C17 C16 -5.4(11) . . . . ?
C11 C12 C17 C16 178.4(7) . . . . ?
C15 C16 C17 C12 0.0(11) . . . . ?
N3 C16 C17 C12 -176.9(7) . . . . ?
Ni1 O3 C18 O4 2.4(8) . . . . ?
Ni1 O3 C18 C19 -176.4(3) . . . . ?
O4 C18 C19 C24 171.7(5) . . . . ?
O3 C18 C19 C24 -9.5(8) . . . . ?
O4 C18 C19 C20 -6.0(8) . . . . ?
O3 C18 C19 C20 172.9(5) . . . . ?
C24 C19 C20 C21 0.1(9) . . . . ?
C18 C19 C20 C21 177.9(5) . . . . ?
C19 C20 C21 C22 0.5(10) . . . . ?
C19 C20 C21 N4 -176.3(6) . . . . ?
O8 N4 C21 C22 -6.4(14) . . . . ?
O7 N4 C21 C22 157.7(9) . . . . ?
O8 N4 C21 C20 170.5(9) . . . . ?
O7 N4 C21 C20 -25.4(12) . . . . ?
C20 C21 C22 C23 0.4(11) . . . . ?
N4 C21 C22 C23 177.1(7) . . . . ?
C20 C21 C22 C15 -175.9(6) . . . 2_665 ?
N4 C21 C22 C15 0.8(11) . . . 2_665 ?
C21 C22 C23 C24 -1.8(10) . . . . ?
C15 C22 C23 C24 174.9(5) 2_665 . . . ?
C20 C19 C24 C23 -1.7(9) . . . . ?
C18 C19 C24 C23 -179.3(5) . . . . ?
C22 C23 C24 C19 2.5(9) . . . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.254 0.204 0.000 473.5 155.3
2 -0.313 0.084 0.500 473.5 154.5
_platon_squeeze_details          
;
;


_refine_diff_density_max         0.388
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.085

