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

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

data_czl-hzb-ps474
_database_code_depnum_ccdc_archive 'CCDC 1580697'
_audit_update_record             
;
2017-10-17 deposited with the CCDC.
2018-01-11 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         'C28 H62 Dy2 N8 Ni4 O22, H2 O'
_chemical_formula_sum            'C28 H64 Dy2 N8 Ni4 O23'
_chemical_formula_weight         1440.71

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'
Dy Dy -0.1892 4.4098 '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                   20.6575(10)
_cell_length_b                   12.7612(6)
_cell_length_c                   17.9948(9)
_cell_angle_alpha                90
_cell_angle_beta                 102.786(5)
_cell_angle_gamma                90
_cell_volume                     4626.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5351
_cell_measurement_theta_min      3.7400
_cell_measurement_theta_max      28.8410

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_F_000             2864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    4.872
_shelx_estimated_absorpt_T_min   0.280
_shelx_estimated_absorpt_T_max   0.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_reflns_number            8872
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.397
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_full        25.019
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             4029
_reflns_number_gt                3678
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0198P)²+20.6705P] 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         4029
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0590
_refine_ls_wR_factor_gt          0.0565
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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
Dy1 Dy 0.20761(2) 0.03984(2) 0.05658(2) 0.02221(7) Uani 1 1 d . . . . .
Ni1 Ni 0.35932(3) 0.07530(4) 0.10683(3) 0.02310(13) Uani 1 1 d . . . . .
Ni2 Ni 0.23850(2) 0.30145(4) 0.07162(3) 0.01935(12) Uani 1 1 d . . . . .
O1 O 0.18467(15) 0.0079(3) 0.18276(17) 0.0364(8) Uani 1 1 d . . . . .
O2 O 0.11178(15) 0.0978(3) 0.10018(17) 0.0364(8) Uani 1 1 d . . . . .
C1 C 0.1313(2) 0.0573(4) 0.1660(2) 0.0301(10) Uani 1 1 d . . . . .
C2 C 0.0895(3) 0.0724(5) 0.2237(3) 0.0485(14) Uani 1 1 d . . . . .
H2A H 0.0725 0.1426 0.2202 0.073 Uiso 1 1 calc R U . . .
H2B H 0.1162 0.0606 0.2739 0.073 Uiso 1 1 calc R U . . .
H2C H 0.0533 0.0235 0.2138 0.073 Uiso 1 1 calc R U . . .
O3 O 0.14464(17) -0.1201(3) 0.0345(2) 0.0479(9) Uani 1 1 d . . . . .
O4 O 0.14248(19) -0.0202(3) -0.06392(18) 0.0479(9) Uani 1 1 d . . . . .
C3 C 0.1202(2) -0.0969(4) -0.0332(3) 0.0354(11) Uani 1 1 d . . . . .
C4 C 0.0631(3) -0.1582(4) -0.0786(3) 0.0517(14) Uani 1 1 d . . . . .
H4A H 0.0601 -0.2244 -0.0543 0.078 Uiso 1 1 calc R U . . .
H4B H 0.0699 -0.1697 -0.1290 0.078 Uiso 1 1 calc R U . . .
H4C H 0.0227 -0.1197 -0.0815 0.078 Uiso 1 1 calc R U . . .
O5 O 0.29507(14) -0.0650(2) 0.11581(16) 0.0297(7) Uani 1 1 d . . . . .
O6 O 0.3562(2) -0.1571(3) 0.2103(2) 0.0558(11) Uani 1 1 d . . . . .
C5 C 0.3105(2) -0.1510(4) 0.1533(2) 0.0317(10) Uani 1 1 d . . . . .
C6 C 0.2710(3) -0.2462(4) 0.1222(3) 0.0403(12) Uani 1 1 d . . . . .
H6A H 0.2867 -0.3056 0.1539 0.060 Uiso 1 1 calc R U . . .
H6B H 0.2761 -0.2595 0.0713 0.060 Uiso 1 1 calc R U . . .
H6C H 0.2250 -0.2344 0.1215 0.060 Uiso 1 1 calc R U . . .
O7 O 0.41317(14) 0.2035(2) 0.09026(17) 0.0319(7) Uani 1 1 d . . . . .
O8 O 0.5147(2) 0.1436(4) 0.1303(3) 0.0952(18) Uani 1 1 d . . . . .
C7 C 0.4749(2) 0.2162(4) 0.1114(3) 0.0394(12) Uani 1 1 d . . . . .
C8 C 0.4999(3) 0.3264(5) 0.1100(4) 0.0687(19) Uani 1 1 d . . . . .
H8A H 0.4915 0.3642 0.1530 0.103 Uiso 1 1 calc R U . . .
H8B H 0.4774 0.3602 0.0638 0.103 Uiso 1 1 calc R U . . .
H8C H 0.5467 0.3252 0.1122 0.103 Uiso 1 1 calc R U . . .
O9 O 0.19155(13) 0.1944(2) -0.00682(14) 0.0200(6) Uani 1 1 d . . . . .
H9 H 0.1514 0.2050 -0.0283 0.030 Uiso 1 1 d R U . . .
N1 N 0.39124(18) 0.0707(3) 0.22335(19) 0.0318(9) Uani 1 1 d . . . . .
H1A H 0.4034 0.0059 0.2386 0.038 Uiso 1 1 calc R U . . .
H1B H 0.4259 0.1131 0.2383 0.038 Uiso 1 1 calc R U . . .
C9 C 0.3355(2) 0.1052(4) 0.2563(2) 0.0295(10) Uani 1 1 d . . . . .
H9A H 0.3523 0.1295 0.3081 0.035 Uiso 1 1 calc R U . . .
H9B H 0.3059 0.0467 0.2579 0.035 Uiso 1 1 calc R U . . .
O10 O 0.28053(13) 0.1641(2) 0.13013(13) 0.0200(6) Uani 1 1 d . . . . .
C10 C 0.2977(2) 0.1935(3) 0.2084(2) 0.0242(9) Uani 1 1 d . . . . .
H10 H 0.2566 0.2061 0.2257 0.029 Uiso 1 1 calc R U . . .
C11 C 0.3371(2) 0.2950(4) 0.2166(2) 0.0303(10) Uani 1 1 d . . . . .
H11A H 0.3444 0.3196 0.2689 0.036 Uiso 1 1 calc R U . . .
H11B H 0.3801 0.2825 0.2049 0.036 Uiso 1 1 calc R U . . .
N2 N 0.30096(18) 0.3762(3) 0.16463(19) 0.0291(8) Uani 1 1 d . . . . .
H2D H 0.3297 0.4173 0.1483 0.035 Uiso 1 1 calc R U . . .
H2E H 0.2770 0.4158 0.1891 0.035 Uiso 1 1 calc R U . . .
N3 N 0.15483(17) 0.3218(3) 0.11861(19) 0.0270(8) Uani 1 1 d . . . . .
H3A H 0.1298 0.2643 0.1115 0.032 Uiso 1 1 calc R U . . .
H3B H 0.1675 0.3336 0.1685 0.032 Uiso 1 1 calc R U . . .
C12 C 0.1165(2) 0.4122(4) 0.0806(2) 0.0303(10) Uani 1 1 d . . . . .
H12A H 0.0957 0.4482 0.1167 0.036 Uiso 1 1 calc R U . . .
H12B H 0.0816 0.3873 0.0390 0.036 Uiso 1 1 calc R U . . .
C13 C 0.1607(2) 0.4883(4) 0.0499(2) 0.0269(10) Uani 1 1 d . . . . .
H13 H 0.1917 0.5201 0.0931 0.032 Uiso 1 1 calc R U . . .
O11 O 0.19828(13) 0.4328(2) 0.00449(14) 0.0228(6) Uani 1 1 d . . . . .
C14 C 0.1191(2) 0.5754(4) 0.0043(2) 0.0350(11) Uani 1 1 d . . . . .
H14A H 0.0890 0.6042 0.0333 0.042 Uiso 1 1 calc R U . . .
H14B H 0.1480 0.6312 -0.0056 0.042 Uiso 1 1 calc R U . . .
N4 N 0.08092(18) 0.5324(3) -0.0688(2) 0.0326(9) Uani 1 1 d . . . . .
H4D H 0.0696 0.5836 -0.1028 0.039 Uiso 1 1 calc R U . . .
H4E H 0.0440 0.5016 -0.0619 0.039 Uiso 1 1 calc R U . . .
O12 O 0.5000 0.8623(11) 0.2500 0.281(10) Uani 1 2 d S T P . .
H12 H 0.5379 0.8350 0.2687 0.422 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O9 2.266(3) . ?
Dy1 O5 2.311(3) . ?
Dy1 O10 2.378(3) . ?
Dy1 O2 2.402(3) . ?
Dy1 O3 2.406(3) . ?
Dy1 O4 2.410(3) . ?
Dy1 O1 2.454(3) . ?
Dy1 O11 2.461(3) 7 ?
Dy1 C3 2.761(5) . ?
Dy1 C1 2.789(4) . ?
Dy1 Ni1 3.0968(6) . ?
Dy1 Ni2 3.3985(6) . ?
Ni1 O7 2.037(3) . ?
Ni1 N1 2.055(3) . ?
Ni1 N4 2.063(4) 7 ?
Ni1 O11 2.094(3) 7 ?
Ni1 O10 2.100(3) . ?
Ni1 O5 2.256(3) . ?
Ni2 O9 2.048(3) . ?
Ni2 O9 2.048(3) 7 ?
Ni2 N3 2.102(3) . ?
Ni2 N2 2.102(3) . ?
Ni2 O11 2.125(3) . ?
Ni2 O10 2.128(3) . ?
Ni2 Dy1 3.4352(5) 7 ?
O1 C1 1.247(5) . ?
O2 C1 1.273(5) . ?
C1 C2 1.503(6) . ?
O3 C3 1.247(6) . ?
O4 C3 1.261(6) . ?
C3 C4 1.497(6) . ?
O5 C5 1.291(5) . ?
O6 C5 1.232(5) . ?
C5 C6 1.501(7) . ?
O7 C7 1.257(5) . ?
O8 C7 1.236(7) . ?
C7 C8 1.500(8) . ?
O9 Ni2 2.048(2) 7 ?
N1 C9 1.474(5) . ?
C9 C10 1.525(6) . ?
O10 C10 1.424(4) . ?
C10 C11 1.519(6) . ?
C11 N2 1.482(5) . ?
N3 C12 1.478(5) . ?
C12 C13 1.518(6) . ?
C13 O11 1.432(5) . ?
C13 C14 1.528(6) . ?
O11 Ni1 2.094(3) 7 ?
O11 Dy1 2.461(3) 7 ?
C14 N4 1.480(6) . ?
N4 Ni1 2.063(4) 7 ?

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
O9 Dy1 O5 138.49(10) . . ?
O9 Dy1 O10 72.77(9) . . ?
O5 Dy1 O10 78.18(10) . . ?
O9 Dy1 O2 81.78(10) . . ?
O5 Dy1 O2 130.13(10) . . ?
O10 Dy1 O2 94.54(10) . . ?
O9 Dy1 O3 129.94(10) . . ?
O5 Dy1 O3 85.62(11) . . ?
O10 Dy1 O3 155.59(10) . . ?
O2 Dy1 O3 81.99(13) . . ?
O9 Dy1 O4 80.40(11) . . ?
O5 Dy1 O4 117.06(12) . . ?
O10 Dy1 O4 150.64(10) . . ?
O2 Dy1 O4 93.18(12) . . ?
O3 Dy1 O4 53.71(11) . . ?
O9 Dy1 O1 125.02(10) . . ?
O5 Dy1 O1 76.60(10) . . ?
O10 Dy1 O1 79.87(10) . . ?
O2 Dy1 O1 53.64(10) . . ?
O3 Dy1 O1 78.67(12) . . ?
O4 Dy1 O1 126.59(11) . . ?
O9 Dy1 O11 72.17(9) . 7 ?
O5 Dy1 O11 70.95(9) . 7 ?
O10 Dy1 O11 71.83(9) . 7 ?
O2 Dy1 O11 153.13(10) . 7 ?
O3 Dy1 O11 119.89(12) . 7 ?
O4 Dy1 O11 88.98(11) . 7 ?
O1 Dy1 O11 140.37(9) . 7 ?
O9 Dy1 C3 104.58(12) . . ?
O5 Dy1 C3 104.32(13) . . ?
O10 Dy1 C3 177.31(12) . . ?
O2 Dy1 C3 84.59(12) . . ?
O3 Dy1 C3 26.81(12) . . ?
O4 Dy1 C3 27.16(13) . . ?
O1 Dy1 C3 101.58(13) . . ?
O11 Dy1 C3 107.92(12) 7 . ?
O9 Dy1 C1 104.08(11) . . ?
O5 Dy1 C1 103.11(12) . . ?
O10 Dy1 C1 86.63(11) . . ?
O2 Dy1 C1 27.09(12) . . ?
O3 Dy1 C1 79.34(13) . . ?
O4 Dy1 C1 111.74(13) . . ?
O1 Dy1 C1 26.55(12) . . ?
O11 Dy1 C1 158.35(11) 7 . ?
C3 Dy1 C1 93.70(14) . . ?
O9 Dy1 Ni1 92.62(7) . . ?
O5 Dy1 Ni1 46.57(8) . . ?
O10 Dy1 Ni1 42.65(6) . . ?
O2 Dy1 Ni1 135.53(8) . . ?
O3 Dy1 Ni1 130.35(9) . . ?
O4 Dy1 Ni1 129.54(9) . . ?
O1 Dy1 Ni1 98.29(7) . . ?
O11 Dy1 Ni1 42.37(6) 7 . ?
C3 Dy1 Ni1 138.76(10) . . ?
C1 Dy1 Ni1 118.39(9) . . ?
O9 Dy1 Ni2 35.81(7) . . ?
O5 Dy1 Ni2 114.73(8) . . ?
O10 Dy1 Ni2 38.35(6) . . ?
O2 Dy1 Ni2 79.94(8) . . ?
O3 Dy1 Ni2 158.72(9) . . ?
O4 Dy1 Ni2 116.20(9) . . ?
O1 Dy1 Ni2 99.26(8) . . ?
O11 Dy1 Ni2 75.13(7) 7 . ?
C3 Dy1 Ni2 138.97(10) . . ?
C1 Dy1 Ni2 89.47(9) . . ?
Ni1 Dy1 Ni2 70.918(14) . . ?
O7 Ni1 N1 96.31(14) . . ?
O7 Ni1 N4 95.76(14) . 7 ?
N1 Ni1 N4 103.85(14) . 7 ?
O7 Ni1 O11 96.48(11) . 7 ?
N1 Ni1 O11 163.92(13) . 7 ?
N4 Ni1 O11 84.51(12) 7 7 ?
O7 Ni1 O10 93.91(11) . . ?
N1 Ni1 O10 84.23(12) . . ?
N4 Ni1 O10 166.61(13) 7 . ?
O11 Ni1 O10 85.21(10) 7 . ?
O7 Ni1 O5 175.53(11) . . ?
N1 Ni1 O5 88.02(13) . . ?
N4 Ni1 O5 84.24(13) 7 . ?
O11 Ni1 O5 79.07(11) 7 . ?
O10 Ni1 O5 85.41(11) . . ?
O7 Ni1 Dy1 128.66(8) . . ?
N1 Ni1 Dy1 111.67(11) . . ?
N4 Ni1 Dy1 116.54(11) 7 . ?
O11 Ni1 Dy1 52.36(7) 7 . ?
O10 Ni1 Dy1 50.08(7) . . ?
O5 Ni1 Dy1 48.05(7) . . ?
O9 Ni2 O9 84.90(11) . 7 ?
O9 Ni2 N3 93.07(12) . . ?
O9 Ni2 N3 166.49(12) 7 . ?
O9 Ni2 N2 164.80(13) . . ?
O9 Ni2 N2 93.18(12) 7 . ?
N3 Ni2 N2 92.18(14) . . ?
O9 Ni2 O11 93.93(11) . . ?
O9 Ni2 O11 83.82(10) 7 . ?
N3 Ni2 O11 83.00(12) . . ?
N2 Ni2 O11 100.86(13) . . ?
O9 Ni2 O10 82.57(10) . . ?
O9 Ni2 O10 92.35(10) 7 . ?
N3 Ni2 O10 100.64(12) . . ?
N2 Ni2 O10 82.44(12) . . ?
O11 Ni2 O10 175.05(10) . . ?
O9 Ni2 Dy1 40.34(7) . . ?
O9 Ni2 Dy1 97.11(8) 7 . ?
N3 Ni2 Dy1 89.82(10) . . ?
N2 Ni2 Dy1 125.49(10) . . ?
O11 Ni2 Dy1 133.38(8) . . ?
O10 Ni2 Dy1 43.89(7) . . ?
O9 Ni2 Dy1 96.02(7) . 7 ?
O9 Ni2 Dy1 39.48(8) 7 7 ?
N3 Ni2 Dy1 127.94(10) . 7 ?
N2 Ni2 Dy1 91.95(10) . 7 ?
O11 Ni2 Dy1 45.35(7) . 7 ?
O10 Ni2 Dy1 131.33(7) . 7 ?
Dy1 Ni2 Dy1 127.497(15) . 7 ?
C1 O1 Dy1 91.9(2) . . ?
C1 O2 Dy1 93.7(3) . . ?
O1 C1 O2 120.8(4) . . ?
O1 C1 C2 120.6(4) . . ?
O2 C1 C2 118.6(4) . . ?
O1 C1 Dy1 61.6(2) . . ?
O2 C1 Dy1 59.2(2) . . ?
C2 C1 Dy1 177.1(4) . . ?
C3 O3 Dy1 92.7(3) . . ?
C3 O4 Dy1 92.1(3) . . ?
O3 C3 O4 120.3(4) . . ?
O3 C3 C4 120.6(5) . . ?
O4 C3 C4 119.1(4) . . ?
O3 C3 Dy1 60.5(2) . . ?
O4 C3 Dy1 60.7(2) . . ?
C4 C3 Dy1 169.5(4) . . ?
C5 O5 Ni1 129.1(3) . . ?
C5 O5 Dy1 144.2(3) . . ?
Ni1 O5 Dy1 85.39(10) . . ?
O6 C5 O5 122.9(4) . . ?
O6 C5 C6 120.8(4) . . ?
O5 C5 C6 116.2(4) . . ?
C7 O7 Ni1 127.5(3) . . ?
O8 C7 O7 123.7(5) . . ?
O8 C7 C8 119.7(5) . . ?
O7 C7 C8 116.5(5) . . ?
Ni2 O9 Ni2 95.11(11) . 7 ?
Ni2 O9 Dy1 103.86(11) . . ?
Ni2 O9 Dy1 105.43(11) 7 . ?
C9 N1 Ni1 107.4(2) . . ?
N1 C9 C10 109.9(3) . . ?
C10 O10 Ni1 107.8(2) . . ?
C10 O10 Ni2 104.9(2) . . ?
Ni1 O10 Ni2 126.51(12) . . ?
C10 O10 Dy1 135.6(2) . . ?
Ni1 O10 Dy1 87.27(9) . . ?
Ni2 O10 Dy1 97.76(10) . . ?
O10 C10 C11 109.4(3) . . ?
O10 C10 C9 110.4(3) . . ?
C11 C10 C9 112.2(3) . . ?
N2 C11 C10 110.5(3) . . ?
C11 N2 Ni2 108.7(3) . . ?
C12 N3 Ni2 108.3(2) . . ?
N3 C12 C13 111.3(3) . . ?
O11 C13 C12 109.7(4) . . ?
O11 C13 C14 111.4(3) . . ?
C12 C13 C14 110.5(4) . . ?
C13 O11 Ni1 107.7(2) . 7 ?
C13 O11 Ni2 105.0(2) . . ?
Ni1 O11 Ni2 124.93(14) 7 . ?
C13 O11 Dy1 140.0(3) . 7 ?
Ni1 O11 Dy1 85.27(9) 7 7 ?
Ni2 O11 Dy1 96.74(10) . 7 ?
N4 C14 C13 109.5(4) . . ?
C14 N4 Ni1 107.5(3) . 7 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C1 O2 0.8(5) . . . . ?
Dy1 O1 C1 C2 -177.8(4) . . . . ?
Dy1 O2 C1 O1 -0.8(5) . . . . ?
Dy1 O2 C1 C2 177.8(4) . . . . ?
Dy1 O3 C3 O4 10.9(5) . . . . ?
Dy1 O3 C3 C4 -167.9(4) . . . . ?
Dy1 O4 C3 O3 -10.9(5) . . . . ?
Dy1 O4 C3 C4 167.9(4) . . . . ?
Ni1 O5 C5 O6 25.6(6) . . . . ?
Dy1 O5 C5 O6 -136.4(5) . . . . ?
Ni1 O5 C5 C6 -152.4(3) . . . . ?
Dy1 O5 C5 C6 45.6(7) . . . . ?
Ni1 O7 C7 O8 17.6(8) . . . . ?
Ni1 O7 C7 C8 -164.8(4) . . . . ?
Ni1 N1 C9 C10 -37.8(4) . . . . ?
Ni1 O10 C10 C11 87.2(3) . . . . ?
Ni2 O10 C10 C11 -49.8(3) . . . . ?
Dy1 O10 C10 C11 -168.0(3) . . . . ?
Ni1 O10 C10 C9 -36.8(4) . . . . ?
Ni2 O10 C10 C9 -173.8(3) . . . . ?
Dy1 O10 C10 C9 68.1(4) . . . . ?
N1 C9 C10 O10 51.4(5) . . . . ?
N1 C9 C10 C11 -70.9(4) . . . . ?
O10 C10 C11 N2 52.6(4) . . . . ?
C9 C10 C11 N2 175.5(3) . . . . ?
C10 C11 N2 Ni2 -26.0(4) . . . . ?
Ni2 N3 C12 C13 -25.8(4) . . . . ?
N3 C12 C13 O11 51.4(4) . . . . ?
N3 C12 C13 C14 174.6(3) . . . . ?
C12 C13 O11 Ni1 87.0(3) . . . 7 ?
C14 C13 O11 Ni1 -35.6(4) . . . 7 ?
C12 C13 O11 Ni2 -48.0(3) . . . . ?
C14 C13 O11 Ni2 -170.7(3) . . . . ?
C12 C13 O11 Dy1 -168.6(3) . . . 7 ?
C14 C13 O11 Dy1 68.7(5) . . . 7 ?
O11 C13 C14 N4 50.4(5) . . . . ?
C12 C13 C14 N4 -71.8(4) . . . . ?
C13 C14 N4 Ni1 -37.6(4) . . . 7 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C6 H6C O3 0.96 2.49 3.173(6) 128.4 .
O9 H9 O7 0.84 1.93 2.682(4) 147.6 7
N1 H1A O6 0.89 2.31 2.993(6) 133.9 .
N1 H1A O12 0.89 2.68 3.446(12) 144.4 1_545
N1 H1B O8 0.89 2.44 3.051(6) 126.0 2_655
C9 H9B O1 0.97 2.62 3.344(5) 132.0 .
C11 H11B O7 0.97 2.52 3.254(5) 132.1 .
N2 H2D O4 0.89 2.18 2.994(5) 152.1 7
N2 H2E O1 0.89 2.55 3.177(4) 127.8 4
N3 H3A O2 0.89 2.16 2.991(5) 155.2 .
N3 H3B O6 0.89 2.34 3.149(5) 150.8 4
C12 H12B O7 0.97 2.62 3.343(5) 131.3 7
C14 H14A O8 0.97 2.62 3.567(7) 166.9 3_455
N4 H4E O8 0.89 2.40 3.034(6) 128.4 7
O12 H12 O6 0.85 2.14 2.909(4) 149.5 2_665

_refine_diff_density_max         0.953
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.108

####################################################################### 
# 
# 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_AAAA
_database_code_depnum_ccdc_archive 'CCDC 1580698'
_audit_update_record             
;
2017-10-17 deposited with the CCDC.
2018-01-11 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         'C28 H62 N8 Ni4 O22 Y2, H2 O'
_chemical_formula_sum            'C28 H64 N8 Ni4 O23 Y2'
_chemical_formula_weight         1293.53

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'
Y Y -2.7962 3.5667 '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                   20.6575(10)
_cell_length_b                   12.7612(6)
_cell_length_c                   17.9948(9)
_cell_angle_alpha                90
_cell_angle_beta                 102.786(5)
_cell_angle_gamma                90
_cell_volume                     4626.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6254
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      26.10

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_F_000             2648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    4.163
_shelx_estimated_absorpt_T_min   0.368
_shelx_estimated_absorpt_T_max   0.505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.298
_exptl_absorpt_correction_T_max  0.453
_exptl_absorpt_process_details   'SADABS (Bruker, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18512
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.889
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_full        25.019
_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             4084
_reflns_number_gt                3456
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0270P)²+6.3121P] 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         4084
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0616
_refine_ls_wR_factor_gt          0.0572
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Y1 Y 0.20840(2) 0.04081(2) 0.05721(2) 0.02330(9) Uani 1 1 d . . . . .
Ni1 Ni 0.35982(2) 0.07602(3) 0.10722(2) 0.02433(10) Uani 1 1 d . . . . .
Ni2 Ni 0.23858(2) 0.30151(3) 0.07156(2) 0.02074(10) Uani 1 1 d . . . . .
O1 O 0.18553(11) 0.00903(18) 0.18300(12) 0.0377(5) Uani 1 1 d . . . . .
O2 O 0.11260(11) 0.09811(18) 0.09972(12) 0.0380(5) Uani 1 1 d . . . . .
C1 C 0.13182(16) 0.0583(2) 0.16538(18) 0.0326(7) Uani 1 1 d . . . . .
C2 C 0.09011(18) 0.0728(3) 0.2229(2) 0.0500(10) Uani 1 1 d . . . . .
H2A H 0.0754 0.1442 0.2219 0.075 Uiso 1 1 calc R U . . .
H2B H 0.1159 0.0563 0.2727 0.075 Uiso 1 1 calc R U . . .
H2C H 0.0523 0.0271 0.2109 0.075 Uiso 1 1 calc R U . . .
O3 O 0.14528(12) -0.11764(19) 0.03602(14) 0.0509(7) Uani 1 1 d . . . . .
O4 O 0.14466(13) -0.02023(19) -0.06275(13) 0.0497(7) Uani 1 1 d . . . . .
C3 C 0.12143(16) -0.0955(3) -0.03220(19) 0.0357(8) Uani 1 1 d . . . . .
C4 C 0.06418(19) -0.1574(3) -0.0770(2) 0.0553(10) Uani 1 1 d . . . . .
H4A H 0.0595 -0.2213 -0.0504 0.083 Uiso 1 1 calc R U . . .
H4B H 0.0722 -0.1737 -0.1262 0.083 Uiso 1 1 calc R U . . .
H4C H 0.0242 -0.1170 -0.0829 0.083 Uiso 1 1 calc R U . . .
O5 O 0.29537(10) -0.06385(15) 0.11606(11) 0.0297(5) Uani 1 1 d . . . . .
O6 O 0.35665(14) -0.1562(2) 0.21033(14) 0.0580(7) Uani 1 1 d . . . . .
C5 C 0.31099(16) -0.1494(2) 0.15338(17) 0.0318(7) Uani 1 1 d . . . . .
C6 C 0.27148(18) -0.2443(3) 0.12261(19) 0.0435(9) Uani 1 1 d . . . . .
H6A H 0.2864 -0.3032 0.1550 0.065 Uiso 1 1 calc R U . . .
H6B H 0.2773 -0.2587 0.0722 0.065 Uiso 1 1 calc R U . . .
H6C H 0.2254 -0.2317 0.1209 0.065 Uiso 1 1 calc R U . . .
O7 O 0.41331(10) 0.20390(16) 0.09042(12) 0.0334(5) Uani 1 1 d . . . . .
O8 O 0.51497(14) 0.1461(3) 0.1292(2) 0.1018(13) Uani 1 1 d . . . . .
C7 C 0.47481(16) 0.2183(3) 0.11109(19) 0.0427(9) Uani 1 1 d . . . . .
C8 C 0.4994(2) 0.3288(3) 0.1092(3) 0.0747(14) Uani 1 1 d . . . . .
H8A H 0.4938 0.3655 0.1539 0.112 Uiso 1 1 calc R U . . .
H8B H 0.4746 0.3637 0.0646 0.112 Uiso 1 1 calc R U . . .
H8C H 0.5456 0.3280 0.1078 0.112 Uiso 1 1 calc R U . . .
O9 O 0.19190(9) 0.19371(14) -0.00639(10) 0.0210(4) Uani 1 1 d . . . . .
H9 H 0.1518 0.2043 -0.0279 0.032 Uiso 1 1 d R U . . .
N1 N 0.39194(12) 0.0714(2) 0.22375(14) 0.0320(6) Uani 1 1 d . . . . .
H1A H 0.4041 0.0066 0.2390 0.038 Uiso 1 1 calc R U . . .
H1B H 0.4267 0.1137 0.2386 0.038 Uiso 1 1 calc R U . . .
C9 C 0.33608(15) 0.1061(2) 0.25697(16) 0.0305(7) Uani 1 1 d . . . . .
H9A H 0.3530 0.1309 0.3086 0.037 Uiso 1 1 calc R U . . .
H9B H 0.3066 0.0474 0.2590 0.037 Uiso 1 1 calc R U . . .
O10 O 0.28057(9) 0.16386(14) 0.13055(10) 0.0212(4) Uani 1 1 d . . . . .
C10 C 0.29786(14) 0.1934(2) 0.20884(15) 0.0251(6) Uani 1 1 d . . . . .
H10 H 0.2568 0.2057 0.2262 0.030 Uiso 1 1 calc R U . . .
C11 C 0.33695(15) 0.2950(2) 0.21696(16) 0.0302(7) Uani 1 1 d . . . . .
H11A H 0.3440 0.3198 0.2691 0.036 Uiso 1 1 calc R U . . .
H11B H 0.3800 0.2826 0.2055 0.036 Uiso 1 1 calc R U . . .
N2 N 0.30107(12) 0.37585(19) 0.16483(13) 0.0296(6) Uani 1 1 d . . . . .
H2D H 0.3299 0.4168 0.1486 0.036 Uiso 1 1 calc R U . . .
H2E H 0.2771 0.4156 0.1892 0.036 Uiso 1 1 calc R U . . .
N3 N 0.15475(12) 0.3221(2) 0.11828(14) 0.0306(6) Uani 1 1 d . . . . .
H3A H 0.1297 0.2647 0.1110 0.037 Uiso 1 1 calc R U . . .
H3B H 0.1673 0.3336 0.1682 0.037 Uiso 1 1 calc R U . . .
C12 C 0.11680(15) 0.4121(2) 0.08078(17) 0.0310(7) Uani 1 1 d . . . . .
H12A H 0.0964 0.4482 0.1171 0.037 Uiso 1 1 calc R U . . .
H12B H 0.0816 0.3872 0.0395 0.037 Uiso 1 1 calc R U . . .
C13 C 0.16074(15) 0.4884(2) 0.04923(16) 0.0278(7) Uani 1 1 d . . . . .
H13 H 0.1918 0.5208 0.0922 0.033 Uiso 1 1 calc R U . . .
O11 O 0.19827(9) 0.43235(14) 0.00428(10) 0.0229(4) Uani 1 1 d . . . . .
C14 C 0.11910(16) 0.5745(3) 0.00376(18) 0.0357(7) Uani 1 1 d . . . . .
H14A H 0.0891 0.6035 0.0330 0.043 Uiso 1 1 calc R U . . .
H14B H 0.1478 0.6304 -0.0065 0.043 Uiso 1 1 calc R U . . .
N4 N 0.08038(13) 0.5313(2) -0.06921(15) 0.0356(6) Uani 1 1 d . . . . .
H4D H 0.0689 0.5823 -0.1033 0.043 Uiso 1 1 calc R U . . .
H4E H 0.0436 0.5003 -0.0620 0.043 Uiso 1 1 calc R U . . .
O12 O 0.5000 0.8628(6) 0.2500 0.228(5) Uani 1 2 d S T P . .
H12 H 0.5379 0.8354 0.2687 0.343 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 O9 2.2495(18) . ?
Y1 O5 2.3003(19) . ?
Y1 O10 2.3579(18) . ?
Y1 O2 2.389(2) . ?
Y1 O3 2.390(2) . ?
Y1 O4 2.396(2) . ?
Y1 O1 2.446(2) . ?
Y1 O11 2.4502(18) 7 ?
Y1 C3 2.750(3) . ?
Y1 C1 2.776(3) . ?
Y1 Ni1 3.0904(5) . ?
Y1 Ni2 3.3841(5) . ?
Ni1 O7 2.031(2) . ?
Ni1 N1 2.055(2) . ?
Ni1 N4 2.060(3) 7 ?
Ni1 O11 2.1004(18) 7 ?
Ni1 O10 2.1018(18) . ?
Ni1 O5 2.253(2) . ?
Ni2 O9 2.0460(18) 7 ?
Ni2 O9 2.0473(18) . ?
Ni2 N3 2.102(2) . ?
Ni2 N2 2.103(2) . ?
Ni2 O11 2.1216(18) . ?
Ni2 O10 2.1347(18) . ?
Ni2 Y1 3.4265(4) 7 ?
O1 C1 1.253(4) . ?
O2 C1 1.267(4) . ?
C1 C2 1.497(4) . ?
O3 C3 1.250(4) . ?
O4 C3 1.254(4) . ?
C3 C4 1.500(5) . ?
O5 C5 1.285(3) . ?
O6 C5 1.233(4) . ?
C5 C6 1.496(5) . ?
O7 C7 1.256(4) . ?
O8 C7 1.235(5) . ?
C7 C8 1.502(5) . ?
O9 Ni2 2.0461(18) 7 ?
N1 C9 1.480(4) . ?
C9 C10 1.521(4) . ?
O10 C10 1.425(3) . ?
C10 C11 1.517(4) . ?
C11 N2 1.478(4) . ?
N3 C12 1.468(4) . ?
C12 C13 1.525(4) . ?
C13 O11 1.430(3) . ?
C13 C14 1.518(4) . ?
O11 Ni1 2.1004(18) 7 ?
O11 Y1 2.4501(18) 7 ?
C14 N4 1.484(4) . ?
N4 Ni1 2.060(3) 7 ?

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
O9 Y1 O5 138.84(7) . . ?
O9 Y1 O10 73.32(6) . . ?
O5 Y1 O10 78.25(7) . . ?
O9 Y1 O2 81.63(7) . . ?
O5 Y1 O2 130.41(7) . . ?
O10 Y1 O2 94.75(7) . . ?
O9 Y1 O3 129.54(7) . . ?
O5 Y1 O3 85.71(8) . . ?
O10 Y1 O3 155.18(7) . . ?
O2 Y1 O3 81.29(9) . . ?
O9 Y1 O4 80.36(7) . . ?
O5 Y1 O4 116.33(8) . . ?
O10 Y1 O4 150.93(7) . . ?
O2 Y1 O4 93.38(9) . . ?
O3 Y1 O4 53.83(8) . . ?
O9 Y1 O1 125.17(7) . . ?
O5 Y1 O1 76.63(7) . . ?
O10 Y1 O1 79.63(7) . . ?
O2 Y1 O1 53.92(7) . . ?
O3 Y1 O1 78.30(8) . . ?
O4 Y1 O1 126.84(8) . . ?
O9 Y1 O11 72.23(6) . 7 ?
O5 Y1 O11 71.13(7) . 7 ?
O10 Y1 O11 72.33(6) . 7 ?
O2 Y1 O11 153.17(7) . 7 ?
O3 Y1 O11 120.15(8) . 7 ?
O4 Y1 O11 88.23(7) . 7 ?
O1 Y1 O11 140.66(7) . 7 ?
O9 Y1 C3 104.20(8) . . ?
O5 Y1 C3 104.15(8) . . ?
O10 Y1 C3 177.47(8) . . ?
O2 Y1 C3 84.31(9) . . ?
O3 Y1 C3 26.99(9) . . ?
O4 Y1 C3 27.11(9) . . ?
O1 Y1 C3 101.62(9) . . ?
O11 Y1 C3 107.56(8) 7 . ?
O9 Y1 C1 103.98(8) . . ?
O5 Y1 C1 103.41(8) . . ?
O10 Y1 C1 86.67(8) . . ?
O2 Y1 C1 27.09(8) . . ?
O3 Y1 C1 78.71(9) . . ?
O4 Y1 C1 111.90(9) . . ?
O1 Y1 C1 26.83(8) . . ?
O11 Y1 C1 158.92(8) 7 . ?
C3 Y1 C1 93.50(10) . . ?
O9 Y1 Ni1 92.96(5) . . ?
O5 Y1 Ni1 46.63(5) . . ?
O10 Y1 Ni1 42.80(4) . . ?
O2 Y1 Ni1 135.98(6) . . ?
O3 Y1 Ni1 130.59(6) . . ?
O4 Y1 Ni1 128.95(6) . . ?
O1 Y1 Ni1 98.33(5) . . ?
O11 Y1 Ni1 42.63(4) 7 . ?
C3 Y1 Ni1 138.62(7) . . ?
C1 Y1 Ni1 118.77(7) . . ?
O9 Y1 Ni2 35.98(5) . . ?
O5 Y1 Ni2 115.07(5) . . ?
O10 Y1 Ni2 38.70(4) . . ?
O2 Y1 Ni2 80.00(6) . . ?
O3 Y1 Ni2 158.21(6) . . ?
O4 Y1 Ni2 116.33(6) . . ?
O1 Y1 Ni2 99.35(6) . . ?
O11 Y1 Ni2 75.34(4) 7 . ?
C3 Y1 Ni2 138.77(7) . . ?
C1 Y1 Ni2 89.52(6) . . ?
Ni1 Y1 Ni2 71.174(11) . . ?
O7 Ni1 N1 96.40(10) . . ?
O7 Ni1 N4 95.66(10) . 7 ?
N1 Ni1 N4 103.76(10) . 7 ?
O7 Ni1 O11 96.51(8) . 7 ?
N1 Ni1 O11 163.80(9) . 7 ?
N4 Ni1 O11 84.64(9) 7 7 ?
O7 Ni1 O10 94.29(8) . . ?
N1 Ni1 O10 84.34(9) . . ?
N4 Ni1 O10 166.36(9) 7 . ?
O11 Ni1 O10 84.97(7) 7 . ?
O7 Ni1 O5 175.27(8) . . ?
N1 Ni1 O5 88.15(9) . . ?
N4 Ni1 O5 84.49(9) 7 . ?
O11 Ni1 O5 78.79(7) 7 . ?
O10 Ni1 O5 84.83(7) . . ?
O7 Ni1 Y1 128.50(6) . . ?
N1 Ni1 Y1 111.74(7) . . ?
N4 Ni1 Y1 116.70(8) 7 . ?
O11 Ni1 Y1 52.19(5) 7 . ?
O10 Ni1 Y1 49.66(5) . . ?
O5 Ni1 Y1 47.90(5) . . ?
O9 Ni2 O9 84.91(7) 7 . ?
O9 Ni2 N3 165.99(8) 7 . ?
O9 Ni2 N3 93.05(9) . . ?
O9 Ni2 N2 93.40(9) 7 . ?
O9 Ni2 N2 164.28(8) . . ?
N3 Ni2 N2 92.23(10) . . ?
O9 Ni2 O11 83.46(7) 7 . ?
O9 Ni2 O11 94.13(7) . . ?
N3 Ni2 O11 82.87(8) . . ?
N2 Ni2 O11 101.21(8) . . ?
O9 Ni2 O10 92.87(7) 7 . ?
O9 Ni2 O10 82.28(7) . . ?
N3 Ni2 O10 100.60(8) . . ?
N2 Ni2 O10 82.20(8) . . ?
O11 Ni2 O10 175.10(7) . . ?
O9 Ni2 Y1 97.26(5) 7 . ?
O9 Ni2 Y1 40.20(5) . . ?
N3 Ni2 Y1 89.95(7) . . ?
N2 Ni2 Y1 125.06(7) . . ?
O11 Ni2 Y1 133.45(5) . . ?
O10 Ni2 Y1 43.68(5) . . ?
O9 Ni2 Y1 39.20(5) 7 7 ?
O9 Ni2 Y1 95.96(5) . 7 ?
N3 Ni2 Y1 127.73(7) . 7 ?
N2 Ni2 Y1 92.48(7) . 7 ?
O11 Ni2 Y1 45.23(5) . 7 ?
O10 Ni2 Y1 131.61(5) . 7 ?
Y1 Ni2 Y1 127.357(11) . 7 ?
C1 O1 Y1 91.39(18) . . ?
C1 O2 Y1 93.73(18) . . ?
O1 C1 O2 121.0(3) . . ?
O1 C1 C2 120.0(3) . . ?
O2 C1 C2 119.0(3) . . ?
O1 C1 Y1 61.78(15) . . ?
O2 C1 Y1 59.18(15) . . ?
C2 C1 Y1 177.4(2) . . ?
C3 O3 Y1 92.77(19) . . ?
C3 O4 Y1 92.38(19) . . ?
O3 C3 O4 119.8(3) . . ?
O3 C3 C4 120.1(3) . . ?
O4 C3 C4 120.1(3) . . ?
O3 C3 Y1 60.24(16) . . ?
O4 C3 Y1 60.52(16) . . ?
C4 C3 Y1 169.3(3) . . ?
C5 O5 Ni1 128.76(19) . . ?
C5 O5 Y1 144.5(2) . . ?
Ni1 O5 Y1 85.47(7) . . ?
O6 C5 O5 123.4(3) . . ?
O6 C5 C6 120.4(3) . . ?
O5 C5 C6 116.2(3) . . ?
C7 O7 Ni1 128.4(2) . . ?
O8 C7 O7 123.0(4) . . ?
O8 C7 C8 119.7(3) . . ?
O7 C7 C8 117.1(3) . . ?
Ni2 O9 Ni2 95.09(7) 7 . ?
Ni2 O9 Y1 105.72(8) 7 . ?
Ni2 O9 Y1 103.82(7) . . ?
C9 N1 Ni1 107.39(17) . . ?
N1 C9 C10 110.0(2) . . ?
C10 O10 Ni1 107.62(15) . . ?
C10 O10 Ni2 105.01(15) . . ?
Ni1 O10 Ni2 126.03(8) . . ?
C10 O10 Y1 135.94(16) . . ?
Ni1 O10 Y1 87.53(6) . . ?
Ni2 O10 Y1 97.62(7) . . ?
O10 C10 C11 109.5(2) . . ?
O10 C10 C9 110.7(2) . . ?
C11 C10 C9 111.9(2) . . ?
N2 C11 C10 110.7(2) . . ?
C11 N2 Ni2 108.95(17) . . ?
C12 N3 Ni2 108.50(17) . . ?
N3 C12 C13 111.7(2) . . ?
O11 C13 C14 111.8(2) . . ?
O11 C13 C12 109.4(2) . . ?
C14 C13 C12 110.5(2) . . ?
C13 O11 Ni1 107.41(16) . 7 ?
C13 O11 Ni2 105.34(15) . . ?
Ni1 O11 Ni2 125.04(9) 7 . ?
C13 O11 Y1 139.88(17) . 7 ?
Ni1 O11 Y1 85.19(6) 7 7 ?
Ni2 O11 Y1 96.83(7) . 7 ?
N4 C14 C13 109.8(2) . . ?
C14 N4 Ni1 107.19(18) . 7 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O1 C1 O2 0.7(3) . . . . ?
Y1 O1 C1 C2 -177.9(3) . . . . ?
Y1 O2 C1 O1 -0.7(3) . . . . ?
Y1 O2 C1 C2 177.9(3) . . . . ?
Y1 O3 C3 O4 11.0(3) . . . . ?
Y1 O3 C3 C4 -167.7(3) . . . . ?
Y1 O4 C3 O3 -11.0(3) . . . . ?
Y1 O4 C3 C4 167.7(3) . . . . ?
Ni1 O5 C5 O6 25.7(4) . . . . ?
Y1 O5 C5 O6 -136.3(3) . . . . ?
Ni1 O5 C5 C6 -152.6(2) . . . . ?
Y1 O5 C5 C6 45.4(5) . . . . ?
Ni1 O7 C7 O8 18.6(5) . . . . ?
Ni1 O7 C7 C8 -164.8(3) . . . . ?
Ni1 N1 C9 C10 -37.3(3) . . . . ?
Ni1 O10 C10 C11 87.0(2) . . . . ?
Ni2 O10 C10 C11 -49.4(2) . . . . ?
Y1 O10 C10 C11 -167.75(17) . . . . ?
Ni1 O10 C10 C9 -36.9(2) . . . . ?
Ni2 O10 C10 C9 -173.26(19) . . . . ?
Y1 O10 C10 C9 68.4(3) . . . . ?
N1 C9 C10 O10 51.1(3) . . . . ?
N1 C9 C10 C11 -71.3(3) . . . . ?
O10 C10 C11 N2 52.2(3) . . . . ?
C9 C10 C11 N2 175.3(2) . . . . ?
C10 C11 N2 Ni2 -25.8(3) . . . . ?
Ni2 N3 C12 C13 -25.2(3) . . . . ?
N3 C12 C13 O11 50.6(3) . . . . ?
N3 C12 C13 C14 174.1(2) . . . . ?
C14 C13 O11 Ni1 -35.1(3) . . . 7 ?
C12 C13 O11 Ni1 87.6(2) . . . 7 ?
C14 C13 O11 Ni2 -170.4(2) . . . . ?
C12 C13 O11 Ni2 -47.6(2) . . . . ?
C14 C13 O11 Y1 68.5(3) . . . 7 ?
C12 C13 O11 Y1 -168.77(18) . . . 7 ?
O11 C13 C14 N4 50.3(3) . . . . ?
C12 C13 C14 N4 -71.8(3) . . . . ?
C13 C14 N4 Ni1 -37.6(3) . . . 7 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9 O7 0.84 1.94 2.695(3) 147.7 7
N1 H1A O6 0.89 2.31 2.991(4) 133.7 .
N1 H1B O8 0.89 2.45 3.059(4) 125.7 2_655
N2 H2D O4 0.89 2.18 2.990(3) 150.7 7
N2 H2E O1 0.89 2.55 3.182(3) 128.3 4
N3 H3A O2 0.89 2.16 2.985(3) 154.5 .
N3 H3B O6 0.89 2.35 3.157(4) 150.9 4
N4 H4E O8 0.89 2.40 3.037(4) 128.6 7
O12 H12 O6 0.85 2.13 2.898(3) 149.4 2_665

_refine_diff_density_max         0.784
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.073

