# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 1818377'
_audit_update_record             
;
2018-01-21 deposited with the CCDC.
2018-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H28 N2 Ni O10'
_chemical_formula_weight         611.23

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

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

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

_cell_length_a                   9.596(7)
_cell_length_b                   10.606(8)
_cell_length_c                   13.967(10)
_cell_angle_alpha                76.205(9)
_cell_angle_beta                 84.844(9)
_cell_angle_gamma                84.742(9)
_cell_volume                     1371.3(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1903
_cell_measurement_theta_min      2.699
_cell_measurement_theta_max      27.693

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             636
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.769
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8535
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.982
_diffrn_reflns_theta_max         27.693
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             6095
_reflns_number_gt                3988
_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)+(0.1003P)²+0.7431P] 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         6095
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.1979
_refine_ls_wR_factor_gt          0.1756
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_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
C1 C 0.6230(4) 0.4952(4) 0.1946(3) 0.0276(9) Uani 1 1 d . . . . .
C2 C 0.5864(4) 0.3702(4) 0.1996(3) 0.0283(9) Uani 1 1 d . . . . .
H2 H 0.5519 0.3195 0.2594 0.034 Uiso 1 1 calc R U . . .
C3 C 0.6012(4) 0.3203(4) 0.1151(3) 0.0296(9) Uani 1 1 d . . . . .
C4 C 0.6565(5) 0.3939(4) 0.0274(3) 0.0330(10) Uani 1 1 d . . . . .
H4 H 0.6629 0.3621 -0.0295 0.040 Uiso 1 1 calc R U . . .
C5 C 0.7026(5) 0.5153(4) 0.0235(3) 0.0317(9) Uani 1 1 d . . . . .
C6 C 0.6831(5) 0.5675(4) 0.1064(3) 0.0331(10) Uani 1 1 d . . . . .
H6 H 0.7101 0.6505 0.1031 0.040 Uiso 1 1 calc R U . . .
C7 C 0.5949(4) 0.5539(4) 0.2821(3) 0.0286(9) Uani 1 1 d . . . . .
C8 C 0.5649(5) 0.1845(4) 0.1191(3) 0.0308(9) Uani 1 1 d . . . . .
C9 C 0.8311(5) 0.6907(4) -0.0683(3) 0.0385(11) Uani 1 1 d . . . . .
H9A H 0.9050 0.6727 -0.0228 0.046 Uiso 1 1 calc R U . . .
H9B H 0.7637 0.7562 -0.0500 0.046 Uiso 1 1 calc R U . . .
C10 C 0.8913(5) 0.7379(4) -0.1719(3) 0.0366(10) Uani 1 1 d . . . . .
C11 C 0.8040(5) 0.7701(4) -0.2489(3) 0.0337(10) Uani 1 1 d . . . . .
H11 H 0.7088 0.7575 -0.2360 0.040 Uiso 1 1 calc R U . . .
C12 C 0.8552(5) 0.8205(4) -0.3445(3) 0.0359(10) Uani 1 1 d . . . . .
C13 C 0.9975(5) 0.8368(5) -0.3644(4) 0.0498(13) Uani 1 1 d . . . . .
H13 H 1.0330 0.8713 -0.4286 0.060 Uiso 1 1 calc R U . . .
C14 C 1.0852(6) 0.8019(6) -0.2889(4) 0.0600(16) Uani 1 1 d . . . . .
H14 H 1.1808 0.8114 -0.3023 0.072 Uiso 1 1 calc R U . . .
C15 C 1.0329(5) 0.7525(5) -0.1930(4) 0.0512(13) Uani 1 1 d . . . . .
H15 H 1.0936 0.7291 -0.1423 0.061 Uiso 1 1 calc R U . . .
C16 C 0.7552(5) 0.8575(5) -0.4226(3) 0.0412(11) Uani 1 1 d . . . . .
C17 C 0.2955(5) -0.0561(5) 0.1832(3) 0.0416(11) Uani 1 1 d . . . . .
H17 H 0.3701 -0.0349 0.2131 0.050 Uiso 1 1 calc R U . . .
C18 C 0.1752(5) -0.0953(5) 0.2419(4) 0.0447(12) Uani 1 1 d . . . . .
H18 H 0.1719 -0.1012 0.3096 0.054 Uiso 1 1 calc R U . . .
C19 C 0.0618(5) -0.1253(5) 0.2014(4) 0.0419(11) Uani 1 1 d . . . . .
C20 C 0.0758(5) -0.1177(5) 0.1003(4) 0.0472(12) Uani 1 1 d . . . . .
H20 H 0.0026 -0.1386 0.0689 0.057 Uiso 1 1 calc R U . . .
C21 C 0.1983(5) -0.0793(5) 0.0470(4) 0.0442(12) Uani 1 1 d . . . . .
H21 H 0.2048 -0.0749 -0.0206 0.053 Uiso 1 1 calc R U . . .
C22 C -0.0706(5) -0.1685(5) 0.2622(4) 0.0525(14) Uani 1 1 d . . . . .
H22A H -0.1504 -0.1344 0.2235 0.063 Uiso 1 1 calc R U . . .
H22B H -0.0802 -0.1316 0.3199 0.063 Uiso 1 1 calc R U . . .
C23 C -0.0735(5) -0.3170(6) 0.2962(4) 0.0547(14) Uani 1 1 d . . . . .
H23A H -0.1582 -0.3380 0.3384 0.066 Uiso 1 1 calc R U . . .
H23B H -0.0764 -0.3532 0.2390 0.066 Uiso 1 1 calc R U . . .
C24 C 0.0513(5) -0.3783(5) 0.3514(4) 0.0413(11) Uani 1 1 d . . . . .
C25 C 0.1507(5) -0.4590(5) 0.3162(4) 0.0454(12) Uani 1 1 d . . . . .
H25 H 0.1373 -0.4843 0.2586 0.054 Uiso 1 1 calc R U . . .
C26 C 0.2698(5) -0.5035(5) 0.3641(4) 0.0421(11) Uani 1 1 d . . . . .
H26 H 0.3346 -0.5591 0.3378 0.050 Uiso 1 1 calc R U . . .
C27 C 0.1976(5) -0.3961(5) 0.4843(3) 0.0440(12) Uani 1 1 d . . . . .
H27 H 0.2116 -0.3744 0.5432 0.053 Uiso 1 1 calc R U . . .
C28 C 0.0757(5) -0.3500(5) 0.4399(4) 0.0472(12) Uani 1 1 d . . . . .
H28 H 0.0088 -0.2994 0.4694 0.057 Uiso 1 1 calc R U . . .
N1 N 0.3090(4) -0.0476(3) 0.0860(3) 0.0353(8) Uani 1 1 d . . . . .
N2 N 0.2981(4) -0.4713(3) 0.4469(3) 0.0347(8) Uani 1 1 d . . . . .
Ni1 Ni 0.5000 0.0000 0.0000 0.0283(2) Uani 1 2 d S . P . .
Ni2 Ni 0.5000 0.5000 0.5000 0.0295(2) Uani 1 2 d S . P . .
O1 O 0.5106(3) 0.1670(3) 0.0455(2) 0.0338(7) Uani 1 1 d . . . . .
O2 O 0.5960(4) 0.0971(3) 0.1925(2) 0.0530(10) Uani 1 1 d . . . . .
O3 O 0.5824(3) 0.4748(3) 0.3649(2) 0.0340(7) Uani 1 1 d . . . . .
O4 O 0.5840(4) 0.6751(3) 0.2692(2) 0.0395(8) Uani 1 1 d . . . . .
O5 O 0.7649(4) 0.5760(3) -0.0647(2) 0.0447(8) Uani 1 1 d . . . . .
O6 O 0.6353(4) 0.8283(4) -0.4108(3) 0.0576(10) Uani 1 1 d . . . . .
O7 O 0.8076(4) 0.9269(5) -0.5050(3) 0.0752(14) Uani 1 1 d . . . . .
H7 H 0.7505 0.9384 -0.5472 0.113 Uiso 1 1 calc R U . . .
O8 O 0.6173(3) -0.1083(3) 0.1154(2) 0.0354(7) Uani 1 1 d . . . . .
O9 O 0.5073(4) 0.7013(3) 0.4532(2) 0.0422(8) Uani 1 1 d . . . . .
O10 O 0.6071(5) 0.0144(5) 0.3836(4) 0.0833(13) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.386(5) . ?
C1 C6 1.393(6) . ?
C1 C7 1.492(5) . ?
C2 C3 1.395(6) . ?
C3 C4 1.377(6) . ?
C3 C8 1.500(5) . ?
C4 C5 1.387(6) . ?
C5 O5 1.360(5) . ?
C5 C6 1.389(6) . ?
C7 O4 1.251(5) . ?
C7 O3 1.259(5) . ?
C8 O2 1.245(5) . ?
C8 O1 1.253(5) . ?
C9 O5 1.411(5) . ?
C9 C10 1.494(6) . ?
C10 C15 1.379(7) . ?
C10 C11 1.382(6) . ?
C11 C12 1.379(6) . ?
C12 C13 1.387(7) . ?
C12 C16 1.476(7) . ?
C13 C14 1.369(7) . ?
C14 C15 1.384(7) . ?
C16 O6 1.206(6) . ?
C16 O7 1.296(6) . ?
C17 N1 1.334(6) . ?
C17 C18 1.390(6) . ?
C18 C19 1.366(7) . ?
C19 C20 1.390(7) . ?
C19 C22 1.507(7) . ?
C20 C21 1.375(7) . ?
C21 N1 1.340(6) . ?
C22 C23 1.536(7) . ?
C23 C24 1.495(7) . ?
C24 C25 1.361(7) . ?
C24 C28 1.383(7) . ?
C25 C26 1.365(7) . ?
C26 N2 1.338(6) . ?
C27 N2 1.343(6) . ?
C27 C28 1.369(7) . ?
N1 Ni1 2.131(4) . ?
N2 Ni2 2.107(4) 1_545 ?
Ni1 O1 2.032(3) . ?
Ni1 O1 2.032(3) 2_655 ?
Ni1 O8 2.096(3) . ?
Ni1 O8 2.096(3) 2_655 ?
Ni1 N1 2.131(4) 2_655 ?
Ni2 O3 2.048(3) . ?
Ni2 O3 2.048(3) 2_666 ?
Ni2 O9 2.084(3) . ?
Ni2 O9 2.084(3) 2_666 ?
Ni2 N2 2.107(4) 2_656 ?
Ni2 N2 2.107(4) 1_565 ?

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
C2 C1 C6 119.7(4) . . ?
C2 C1 C7 120.4(3) . . ?
C6 C1 C7 119.8(4) . . ?
C1 C2 C3 120.1(4) . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 C8 118.9(4) . . ?
C2 C3 C8 121.1(4) . . ?
C3 C4 C5 120.2(4) . . ?
O5 C5 C4 115.7(4) . . ?
O5 C5 C6 124.3(4) . . ?
C4 C5 C6 120.0(4) . . ?
C5 C6 C1 119.8(4) . . ?
O4 C7 O3 124.8(4) . . ?
O4 C7 C1 119.2(3) . . ?
O3 C7 C1 116.0(4) . . ?
O2 C8 O1 124.9(4) . . ?
O2 C8 C3 118.2(4) . . ?
O1 C8 C3 116.8(4) . . ?
O5 C9 C10 107.4(4) . . ?
C15 C10 C11 118.6(4) . . ?
C15 C10 C9 121.5(4) . . ?
C11 C10 C9 119.9(4) . . ?
C12 C11 C10 121.3(4) . . ?
C11 C12 C13 119.6(4) . . ?
C11 C12 C16 118.4(4) . . ?
C13 C12 C16 122.0(4) . . ?
C14 C13 C12 119.5(5) . . ?
C13 C14 C15 120.7(5) . . ?
C10 C15 C14 120.4(5) . . ?
O6 C16 O7 122.8(5) . . ?
O6 C16 C12 123.5(4) . . ?
O7 C16 C12 113.6(4) . . ?
N1 C17 C18 123.1(4) . . ?
C19 C18 C17 120.8(5) . . ?
C18 C19 C20 116.3(4) . . ?
C18 C19 C22 122.6(5) . . ?
C20 C19 C22 121.0(5) . . ?
C21 C20 C19 119.7(5) . . ?
N1 C21 C20 124.2(4) . . ?
C19 C22 C23 113.4(4) . . ?
C24 C23 C22 112.3(4) . . ?
C25 C24 C28 116.0(5) . . ?
C25 C24 C23 122.8(5) . . ?
C28 C24 C23 121.2(5) . . ?
C24 C25 C26 121.2(5) . . ?
N2 C26 C25 123.4(5) . . ?
N2 C27 C28 123.2(4) . . ?
C27 C28 C24 120.4(5) . . ?
C17 N1 C21 115.8(4) . . ?
C17 N1 Ni1 122.1(3) . . ?
C21 N1 Ni1 122.0(3) . . ?
C26 N2 C27 115.7(4) . . ?
C26 N2 Ni2 122.8(3) . 1_545 ?
C27 N2 Ni2 120.3(3) . 1_545 ?
O1 Ni1 O1 180.0 . 2_655 ?
O1 Ni1 O8 91.86(12) . . ?
O1 Ni1 O8 88.14(12) 2_655 . ?
O1 Ni1 O8 88.14(12) . 2_655 ?
O1 Ni1 O8 91.86(12) 2_655 2_655 ?
O8 Ni1 O8 180.0 . 2_655 ?
O1 Ni1 N1 93.75(13) . . ?
O1 Ni1 N1 86.25(13) 2_655 . ?
O8 Ni1 N1 90.93(14) . . ?
O8 Ni1 N1 89.07(14) 2_655 . ?
O1 Ni1 N1 86.25(13) . 2_655 ?
O1 Ni1 N1 93.75(13) 2_655 2_655 ?
O8 Ni1 N1 89.07(14) . 2_655 ?
O8 Ni1 N1 90.93(14) 2_655 2_655 ?
N1 Ni1 N1 180.00(18) . 2_655 ?
O3 Ni2 O3 180.00(16) . 2_666 ?
O3 Ni2 O9 91.41(12) . . ?
O3 Ni2 O9 88.59(12) 2_666 . ?
O3 Ni2 O9 88.59(12) . 2_666 ?
O3 Ni2 O9 91.41(12) 2_666 2_666 ?
O9 Ni2 O9 180.0 . 2_666 ?
O3 Ni2 N2 90.55(14) . 2_656 ?
O3 Ni2 N2 89.45(14) 2_666 2_656 ?
O9 Ni2 N2 94.02(13) . 2_656 ?
O9 Ni2 N2 85.98(13) 2_666 2_656 ?
O3 Ni2 N2 89.45(14) . 1_565 ?
O3 Ni2 N2 90.55(14) 2_666 1_565 ?
O9 Ni2 N2 85.98(13) . 1_565 ?
O9 Ni2 N2 94.02(13) 2_666 1_565 ?
N2 Ni2 N2 180.0 2_656 1_565 ?
C8 O1 Ni1 129.6(3) . . ?
C7 O3 Ni2 131.4(3) . . ?
C5 O5 C9 117.7(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
C6 C1 C2 C3 -4.2(6) . . . . ?
C7 C1 C2 C3 174.2(4) . . . . ?
C1 C2 C3 C4 2.1(6) . . . . ?
C1 C2 C3 C8 178.8(4) . . . . ?
C2 C3 C4 C5 2.5(7) . . . . ?
C8 C3 C4 C5 -174.2(4) . . . . ?
C3 C4 C5 O5 175.3(4) . . . . ?
C3 C4 C5 C6 -5.0(7) . . . . ?
O5 C5 C6 C1 -177.5(4) . . . . ?
C4 C5 C6 C1 2.9(7) . . . . ?
C2 C1 C6 C5 1.7(7) . . . . ?
C7 C1 C6 C5 -176.7(4) . . . . ?
C2 C1 C7 O4 -156.5(4) . . . . ?
C6 C1 C7 O4 21.8(6) . . . . ?
C2 C1 C7 O3 22.8(6) . . . . ?
C6 C1 C7 O3 -158.8(4) . . . . ?
C4 C3 C8 O2 137.6(5) . . . . ?
C2 C3 C8 O2 -39.2(6) . . . . ?
C4 C3 C8 O1 -39.4(6) . . . . ?
C2 C3 C8 O1 143.8(4) . . . . ?
O5 C9 C10 C15 -120.9(5) . . . . ?
O5 C9 C10 C11 60.3(6) . . . . ?
C15 C10 C11 C12 -2.4(7) . . . . ?
C9 C10 C11 C12 176.5(4) . . . . ?
C10 C11 C12 C13 1.4(7) . . . . ?
C10 C11 C12 C16 -177.7(4) . . . . ?
C11 C12 C13 C14 0.4(8) . . . . ?
C16 C12 C13 C14 179.4(5) . . . . ?
C12 C13 C14 C15 -1.1(9) . . . . ?
C11 C10 C15 C14 1.8(8) . . . . ?
C9 C10 C15 C14 -177.1(5) . . . . ?
C13 C14 C15 C10 0.0(10) . . . . ?
C11 C12 C16 O6 -11.7(7) . . . . ?
C13 C12 C16 O6 169.3(5) . . . . ?
C11 C12 C16 O7 167.0(5) . . . . ?
C13 C12 C16 O7 -12.0(7) . . . . ?
N1 C17 C18 C19 -1.2(8) . . . . ?
C17 C18 C19 C20 1.7(7) . . . . ?
C17 C18 C19 C22 179.8(5) . . . . ?
C18 C19 C20 C21 -1.2(7) . . . . ?
C22 C19 C20 C21 -179.4(5) . . . . ?
C19 C20 C21 N1 0.1(8) . . . . ?
C18 C19 C22 C23 -93.7(6) . . . . ?
C20 C19 C22 C23 84.3(6) . . . . ?
C19 C22 C23 C24 55.1(6) . . . . ?
C22 C23 C24 C25 -113.7(6) . . . . ?
C22 C23 C24 C28 62.9(6) . . . . ?
C28 C24 C25 C26 -2.9(7) . . . . ?
C23 C24 C25 C26 173.9(5) . . . . ?
C24 C25 C26 N2 -0.6(8) . . . . ?
N2 C27 C28 C24 -1.0(8) . . . . ?
C25 C24 C28 C27 3.6(7) . . . . ?
C23 C24 C28 C27 -173.2(5) . . . . ?
C18 C17 N1 C21 0.0(7) . . . . ?
C18 C17 N1 Ni1 -175.6(4) . . . . ?
C20 C21 N1 C17 0.5(7) . . . . ?
C20 C21 N1 Ni1 176.2(4) . . . . ?
C25 C26 N2 C27 3.3(7) . . . . ?
C25 C26 N2 Ni2 -164.1(4) . . . 1_545 ?
C28 C27 N2 C26 -2.5(7) . . . . ?
C28 C27 N2 Ni2 165.2(4) . . . 1_545 ?
O2 C8 O1 Ni1 -17.6(7) . . . . ?
C3 C8 O1 Ni1 159.2(3) . . . . ?
O4 C7 O3 Ni2 15.9(6) . . . . ?
C1 C7 O3 Ni2 -163.4(3) . . . . ?
C4 C5 O5 C9 -171.2(4) . . . . ?
C6 C5 O5 C9 9.1(7) . . . . ?
C10 C9 O5 C5 179.8(4) . . . . ?

_refine_diff_density_max         3.658
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.105


_exptl_crystal_recrystallization_method 'hydrothermal synthesis'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1818380'
_audit_update_record             
;
2018-01-21 deposited with the CCDC.
2018-07-30 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT601_a                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        232 Ang**3
RESPONSE:  It should be noted that the solvent molecules in the channels of compound.
;
# Added during the CSD deposition process: Sunday 21 January 2018 05:09 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H22 N2 Ni O10'
_chemical_formula_weight         605.18

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

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

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

_cell_length_a                   13.498(3)
_cell_length_b                   15.706(4)
_cell_length_c                   15.066(4)
_cell_angle_alpha                90
_cell_angle_beta                 110.796(3)
_cell_angle_gamma                90
_cell_volume                     2985.9(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3145
_cell_measurement_theta_min      2.173
_cell_measurement_theta_max      27.626

_exptl_crystal_description       ROD
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_F_000             1248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.706
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18466
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.942
_diffrn_reflns_theta_max         27.626
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6834
_reflns_number_gt                4638
_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 (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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6834
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0857
_refine_ls_wR_factor_ref         0.3175
_refine_ls_wR_factor_gt          0.2897
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.181
_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
C1 C 0.0369(4) 0.4201(3) 0.2833(3) 0.0308(10) Uani 1 1 d . . . . .
C2 C 0.0758(4) 0.4642(3) 0.3762(3) 0.0332(10) Uani 1 1 d . . . . .
C3 C 0.1235(4) 0.4185(3) 0.4588(3) 0.0352(11) Uani 1 1 d . . . . .
H3 H 0.1290 0.3596 0.4560 0.042 Uiso 1 1 calc R U . . .
C4 C 0.1630(4) 0.4594(3) 0.5455(4) 0.0372(11) Uani 1 1 d . . . . .
C5 C 0.1564(4) 0.5477(3) 0.5505(3) 0.0339(11) Uani 1 1 d . . . . .
H5 H 0.1848 0.5756 0.6084 0.041 Uiso 1 1 calc R U . . .
C6 C 0.1067(4) 0.5933(3) 0.4675(3) 0.0298(10) Uani 1 1 d . . . . .
C7 C 0.0666(4) 0.5528(3) 0.3807(3) 0.0312(10) Uani 1 1 d . . . . .
H7 H 0.0337 0.5841 0.3257 0.037 Uiso 1 1 calc R U . . .
C8 C 0.0995(4) 0.6883(3) 0.4707(3) 0.0297(10) Uani 1 1 d . . . . .
C9 C 0.2499(5) 0.4438(4) 0.7133(4) 0.0459(13) Uani 1 1 d . . . . .
H9A H 0.1932 0.4647 0.7328 0.055 Uiso 1 1 calc R U . . .
H9B H 0.2971 0.4908 0.7146 0.055 Uiso 1 1 calc R U . . .
C10 C 0.3097(5) 0.3730(4) 0.7780(4) 0.0466(13) Uani 1 1 d . . . . .
C11 C 0.4162(5) 0.3656(4) 0.8021(4) 0.0418(12) Uani 1 1 d . . . . .
H11 H 0.4527 0.4079 0.7831 0.050 Uiso 1 1 calc R U . . .
C12 C 0.4723(4) 0.2973(4) 0.8541(4) 0.0411(12) Uani 1 1 d . . . . .
C13 C 0.4192(5) 0.2347(4) 0.8832(4) 0.0532(16) Uani 1 1 d . . . . .
H13 H 0.4561 0.1891 0.9194 0.064 Uiso 1 1 calc R U . . .
C14 C 0.3080(6) 0.2403(5) 0.8573(5) 0.0624(18) Uani 1 1 d . . . . .
H14 H 0.2714 0.1976 0.8755 0.075 Uiso 1 1 calc R U . . .
C15 C 0.2542(5) 0.3082(5) 0.8059(5) 0.0555(16) Uani 1 1 d . . . . .
H15 H 0.1810 0.3117 0.7892 0.067 Uiso 1 1 calc R U . . .
C16 C 0.5879(4) 0.2927(3) 0.8754(4) 0.0410(12) Uani 1 1 d . . . . .
C17 C 0.1793(4) 0.2937(4) 0.1031(4) 0.0421(13) Uani 1 1 d . . . . .
H17 H 0.1478 0.2404 0.0974 0.050 Uiso 1 1 calc R U . . .
C18 C 0.2758(5) 0.3004(4) 0.0924(5) 0.0502(15) Uani 1 1 d . . . . .
H18 H 0.3071 0.2524 0.0775 0.060 Uiso 1 1 calc R U . . .
C19 C 0.3270(4) 0.3784(4) 0.1036(4) 0.0482(14) Uani 1 1 d . . . . .
C20 C 0.2778(5) 0.4457(4) 0.1256(5) 0.0492(14) Uani 1 1 d . . . . .
H20 H 0.3105 0.4988 0.1360 0.059 Uiso 1 1 calc R U . . .
C21 C 0.1779(4) 0.4360(4) 0.1329(4) 0.0452(13) Uani 1 1 d . . . . .
H21 H 0.1448 0.4837 0.1462 0.054 Uiso 1 1 calc R U . . .
C22 C 0.4325(5) 0.3888(5) 0.0910(5) 0.0584(17) Uani 1 1 d . . . . .
H22A H 0.4265 0.3678 0.0288 0.070 Uiso 1 1 calc R U . . .
H22B H 0.4499 0.4489 0.0936 0.070 Uiso 1 1 calc R U . . .
C23 C 0.5198(6) 0.3431(6) 0.1641(6) 0.076(3) Uani 1 1 d . . . . .
H23A H 0.4985 0.2842 0.1655 0.091 Uiso 1 1 calc R U . . .
H23B H 0.5289 0.3677 0.2256 0.091 Uiso 1 1 calc R U . . .
C24 C 0.6264(5) 0.3441(4) 0.1511(5) 0.0504(16) Uani 1 1 d . . . . .
C25 C 0.6534(5) 0.4040(5) 0.0966(4) 0.0541(16) Uani 1 1 d . . . . .
H25 H 0.6045 0.4452 0.0641 0.065 Uiso 1 1 calc R U . . .
C26 C 0.7525(4) 0.4029(4) 0.0902(4) 0.0412(12) Uani 1 1 d . . . . .
H26 H 0.7689 0.4440 0.0532 0.049 Uiso 1 1 calc R U . . .
C27 C 0.7999(4) 0.2882(4) 0.1869(4) 0.0479(14) Uani 1 1 d . . . . .
H27 H 0.8506 0.2480 0.2190 0.057 Uiso 1 1 calc R U . . .
C28 C 0.7024(5) 0.2841(4) 0.1968(5) 0.0557(16) Uani 1 1 d . . . . .
H28 H 0.6879 0.2418 0.2336 0.067 Uiso 1 1 calc R U . . .
N1 N 0.1284(3) 0.3615(3) 0.1217(3) 0.0313(9) Uani 1 1 d . . . . .
N2 N 0.8262(3) 0.3454(3) 0.1348(3) 0.0335(9) Uani 1 1 d . . . . .
Ni1 Ni -0.02219(4) 0.34885(4) 0.12813(4) 0.0277(3) Uani 1 1 d . . . . .
O1 O 0.0429(3) 0.3407(2) 0.2791(3) 0.0380(9) Uani 1 1 d . . . . .
O2 O -0.0026(3) 0.4635(2) 0.2077(2) 0.0375(8) Uani 1 1 d . . . . .
O3 O 0.0299(3) 0.7237(2) 0.4015(2) 0.0331(8) Uani 1 1 d . . . . .
O4 O 0.1631(3) 0.7268(2) 0.5417(3) 0.0427(9) Uani 1 1 d . . . . .
O5 O 0.2088(4) 0.4084(2) 0.6221(3) 0.0521(11) Uani 1 1 d . . . . .
O6 O 0.6327(3) 0.2210(3) 0.9172(4) 0.0610(12) Uani 1 1 d . . . . .
H6 H 0.6974 0.2259 0.9360 0.091 Uiso 1 1 calc R U . . .
O7 O 0.6374(4) 0.3484(3) 0.8548(4) 0.0572(12) Uani 1 1 d . . . . .
O8 O -0.0887(3) 0.3867(2) -0.0127(2) 0.0389(8) Uani 1 1 d . . . . .
O10 O 0.0352(6) 0.3770(6) 0.8765(5) 0.127(3) 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 O1 1.252(6) . ?
C1 O2 1.270(6) . ?
C1 C2 1.481(7) . ?
C2 C3 1.382(7) . ?
C2 C7 1.401(7) . ?
C3 C4 1.382(7) . ?
C3 H3 0.9300 . ?
C4 O5 1.361(6) . ?
C4 C5 1.392(7) . ?
C5 C6 1.389(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.380(7) . ?
C6 C8 1.497(7) . ?
C7 H7 0.9300 . ?
C8 O3 1.259(6) . ?
C8 O4 1.263(6) . ?
C9 O5 1.401(6) . ?
C9 C10 1.511(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.357(8) . ?
C10 C15 1.413(9) . ?
C11 C12 1.384(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.378(8) . ?
C12 C16 1.478(8) . ?
C13 C14 1.413(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.366(9) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O7 1.206(7) . ?
C16 O6 1.327(7) . ?
C17 N1 1.349(7) . ?
C17 C18 1.373(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.352(8) . ?
C19 C22 1.511(8) . ?
C20 C21 1.399(7) . ?
C20 H20 0.9300 . ?
C21 N1 1.329(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.481(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.520(8) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.381(8) . ?
C24 C28 1.382(9) . ?
C25 C26 1.375(8) . ?
C25 H25 0.9300 . ?
C26 N2 1.335(7) . ?
C26 H26 0.9300 . ?
C27 N2 1.322(7) . ?
C27 C28 1.378(8) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
N1 Ni1 2.078(4) . ?
N2 Ni1 2.085(4) 1_655 ?
Ni1 O3 2.010(3) 2_545 ?
Ni1 O8 2.075(4) . ?
Ni1 N2 2.085(4) 1_455 ?
Ni1 O2 2.127(4) . ?
Ni1 O1 2.132(4) . ?
O3 Ni1 2.010(3) 2 ?
O6 H6 0.8200 . ?

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 C1 O2 120.2(4) . . ?
O1 C1 C2 120.3(4) . . ?
O2 C1 C2 119.4(4) . . ?
C3 C2 C7 119.5(4) . . ?
C3 C2 C1 120.2(4) . . ?
C7 C2 C1 120.2(4) . . ?
C4 C3 C2 120.6(5) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
O5 C4 C3 115.7(4) . . ?
O5 C4 C5 124.0(5) . . ?
C3 C4 C5 120.2(5) . . ?
C6 C5 C4 119.0(4) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C7 C6 C5 121.1(4) . . ?
C7 C6 C8 118.8(4) . . ?
C5 C6 C8 120.1(4) . . ?
C6 C7 C2 119.5(4) . . ?
C6 C7 H7 120.3 . . ?
C2 C7 H7 120.3 . . ?
O3 C8 O4 124.9(4) . . ?
O3 C8 C6 116.8(4) . . ?
O4 C8 C6 118.2(4) . . ?
O5 C9 C10 106.0(4) . . ?
O5 C9 H9A 110.5 . . ?
C10 C9 H9A 110.5 . . ?
O5 C9 H9B 110.5 . . ?
C10 C9 H9B 110.5 . . ?
H9A C9 H9B 108.7 . . ?
C11 C10 C15 118.9(6) . . ?
C11 C10 C9 120.5(6) . . ?
C15 C10 C9 120.3(6) . . ?
C10 C11 C12 122.1(6) . . ?
C10 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C13 C12 C11 119.5(6) . . ?
C13 C12 C16 121.6(5) . . ?
C11 C12 C16 119.0(5) . . ?
C12 C13 C14 119.3(6) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 120.3(6) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C10 120.0(6) . . ?
C14 C15 H15 120.0 . . ?
C10 C15 H15 120.0 . . ?
O7 C16 O6 122.4(5) . . ?
O7 C16 C12 123.2(5) . . ?
O6 C16 C12 114.4(5) . . ?
N1 C17 C18 122.6(5) . . ?
N1 C17 H17 118.7 . . ?
C18 C17 H17 118.7 . . ?
C17 C18 C19 120.4(5) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C20 C19 C18 117.0(5) . . ?
C20 C19 C22 120.9(6) . . ?
C18 C19 C22 122.1(6) . . ?
C19 C20 C21 120.3(5) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
N1 C21 C20 122.8(5) . . ?
N1 C21 H21 118.6 . . ?
C20 C21 H21 118.6 . . ?
C23 C22 C19 113.0(6) . . ?
C23 C22 H22A 109.0 . . ?
C19 C22 H22A 109.0 . . ?
C23 C22 H22B 109.0 . . ?
C19 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C22 C23 C24 116.0(6) . . ?
C22 C23 H23A 108.3 . . ?
C24 C23 H23A 108.3 . . ?
C22 C23 H23B 108.3 . . ?
C24 C23 H23B 108.3 . . ?
H23A C23 H23B 107.4 . . ?
C25 C24 C28 117.1(5) . . ?
C25 C24 C23 123.0(6) . . ?
C28 C24 C23 119.8(5) . . ?
C26 C25 C24 120.1(6) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
N2 C26 C25 122.9(5) . . ?
N2 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
N2 C27 C28 124.3(5) . . ?
N2 C27 H27 117.8 . . ?
C28 C27 H27 117.8 . . ?
C27 C28 C24 118.9(5) . . ?
C27 C28 H28 120.6 . . ?
C24 C28 H28 120.6 . . ?
C21 N1 C17 116.8(4) . . ?
C21 N1 Ni1 122.3(4) . . ?
C17 N1 Ni1 120.8(3) . . ?
C27 N2 C26 116.7(5) . . ?
C27 N2 Ni1 121.4(4) . 1_655 ?
C26 N2 Ni1 121.8(4) . 1_655 ?
O3 Ni1 O8 94.82(15) 2_545 . ?
O3 Ni1 N1 93.32(15) 2_545 . ?
O8 Ni1 N1 90.00(15) . . ?
O3 Ni1 N2 90.60(15) 2_545 1_455 ?
O8 Ni1 N2 88.92(16) . 1_455 ?
N1 Ni1 N2 176.01(16) . 1_455 ?
O3 Ni1 O2 159.90(14) 2_545 . ?
O8 Ni1 O2 104.81(15) . . ?
N1 Ni1 O2 91.00(15) . . ?
N2 Ni1 O2 85.56(15) 1_455 . ?
O3 Ni1 O1 98.49(14) 2_545 . ?
O8 Ni1 O1 166.58(14) . . ?
N1 Ni1 O1 90.91(16) . . ?
N2 Ni1 O1 89.25(16) 1_455 . ?
O2 Ni1 O1 61.79(13) . . ?
C1 O1 Ni1 89.1(3) . . ?
C1 O2 Ni1 88.8(3) . . ?
C8 O3 Ni1 125.5(3) . 2 ?
C4 O5 C9 120.0(4) . . ?
C16 O6 H6 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 3.0(8) . . . . ?
O2 C1 C2 C3 -177.0(5) . . . . ?
O1 C1 C2 C7 -178.5(5) . . . . ?
O2 C1 C2 C7 1.5(7) . . . . ?
C7 C2 C3 C4 -0.7(8) . . . . ?
C1 C2 C3 C4 177.9(5) . . . . ?
C2 C3 C4 O5 -179.7(5) . . . . ?
C2 C3 C4 C5 -0.8(8) . . . . ?
O5 C4 C5 C6 -179.2(5) . . . . ?
C3 C4 C5 C6 1.9(8) . . . . ?
C4 C5 C6 C7 -1.6(7) . . . . ?
C4 C5 C6 C8 -179.3(5) . . . . ?
C5 C6 C7 C2 0.2(7) . . . . ?
C8 C6 C7 C2 177.9(4) . . . . ?
C3 C2 C7 C6 0.9(7) . . . . ?
C1 C2 C7 C6 -177.6(4) . . . . ?
C7 C6 C8 O3 21.9(6) . . . . ?
C5 C6 C8 O3 -160.4(4) . . . . ?
C7 C6 C8 O4 -157.9(5) . . . . ?
C5 C6 C8 O4 19.8(6) . . . . ?
O5 C9 C10 C11 97.1(6) . . . . ?
O5 C9 C10 C15 -76.0(7) . . . . ?
C15 C10 C11 C12 -0.8(9) . . . . ?
C9 C10 C11 C12 -174.0(5) . . . . ?
C10 C11 C12 C13 -0.4(9) . . . . ?
C10 C11 C12 C16 178.4(5) . . . . ?
C11 C12 C13 C14 1.6(9) . . . . ?
C16 C12 C13 C14 -177.2(6) . . . . ?
C12 C13 C14 C15 -1.5(11) . . . . ?
C13 C14 C15 C10 0.2(11) . . . . ?
C11 C10 C15 C14 0.9(10) . . . . ?
C9 C10 C15 C14 174.1(6) . . . . ?
C13 C12 C16 O7 -176.4(6) . . . . ?
C11 C12 C16 O7 4.8(9) . . . . ?
C13 C12 C16 O6 5.2(8) . . . . ?
C11 C12 C16 O6 -173.6(5) . . . . ?
N1 C17 C18 C19 2.2(10) . . . . ?
C17 C18 C19 C20 0.3(10) . . . . ?
C17 C18 C19 C22 -179.2(6) . . . . ?
C18 C19 C20 C21 -2.3(9) . . . . ?
C22 C19 C20 C21 177.2(6) . . . . ?
C19 C20 C21 N1 2.0(10) . . . . ?
C20 C19 C22 C23 114.4(8) . . . . ?
C18 C19 C22 C23 -66.2(9) . . . . ?
C19 C22 C23 C24 174.8(6) . . . . ?
C22 C23 C24 C25 20.8(12) . . . . ?
C22 C23 C24 C28 -160.7(8) . . . . ?
C28 C24 C25 C26 -0.6(10) . . . . ?
C23 C24 C25 C26 178.0(7) . . . . ?
C24 C25 C26 N2 0.2(10) . . . . ?
N2 C27 C28 C24 -1.1(11) . . . . ?
C25 C24 C28 C27 1.0(10) . . . . ?
C23 C24 C28 C27 -177.6(7) . . . . ?
C20 C21 N1 C17 0.4(9) . . . . ?
C20 C21 N1 Ni1 -177.8(4) . . . . ?
C18 C17 N1 C21 -2.5(9) . . . . ?
C18 C17 N1 Ni1 175.8(5) . . . . ?
C28 C27 N2 C26 0.7(9) . . . . ?
C28 C27 N2 Ni1 177.8(5) . . . 1_655 ?
C25 C26 N2 C27 -0.2(9) . . . . ?
C25 C26 N2 Ni1 -177.3(5) . . . 1_655 ?
O2 C1 O1 Ni1 2.2(5) . . . . ?
C2 C1 O1 Ni1 -177.8(4) . . . . ?
O1 C1 O2 Ni1 -2.2(5) . . . . ?
C2 C1 O2 Ni1 177.8(4) . . . . ?
O4 C8 O3 Ni1 14.0(7) . . . 2 ?
C6 C8 O3 Ni1 -165.8(3) . . . 2 ?
C3 C4 O5 C9 -179.1(5) . . . . ?
C5 C4 O5 C9 2.0(9) . . . . ?
C10 C9 O5 C4 -170.9(5) . . . . ?

_refine_diff_density_max         2.970
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.186


_exptl_crystal_recrystallization_method 'hydrothermal synthesis'
####################################################################### 
# 
# 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_22
_database_code_depnum_ccdc_archive 'CCDC 1818379'
_audit_update_record             
;
2018-01-21 deposited with the CCDC.
2018-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H27 N3 Ni1.50 O11'
_chemical_formula_weight         741.65

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

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

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

_cell_length_a                   10.173(6)
_cell_length_b                   13.321(7)
_cell_length_c                   13.327(7)
_cell_angle_alpha                72.941(5)
_cell_angle_beta                 83.845(6)
_cell_angle_gamma                81.978(6)
_cell_volume                     1705.5(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2621
_cell_measurement_theta_min      2.441
_cell_measurement_theta_max      27.589

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_F_000             764
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.901
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10532
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.923
_diffrn_reflns_theta_max         27.589
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             7519
_reflns_number_gt                5410
_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 (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)+(0.0703P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7519
_refine_ls_number_parameters     448
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1432
_refine_ls_wR_factor_gt          0.1261
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
C1 C -0.0221(4) 0.3621(3) 0.4688(3) 0.0426(9) Uani 1 1 d . . . . .
H1 H -0.0454 0.4243 0.4169 0.051 Uiso 1 1 calc R U . . .
C2 C 0.0558(4) 0.1862(3) 0.5154(3) 0.0427(9) Uani 1 1 d . . . . .
H2 H 0.0867 0.1245 0.4970 0.051 Uiso 1 1 calc R U . . .
C3 C 0.0411(4) 0.1828(4) 0.6219(3) 0.0521(11) Uani 1 1 d . . . . .
H3 H 0.0626 0.1195 0.6729 0.063 Uiso 1 1 calc R U . . .
C4 C -0.0046(4) 0.2720(4) 0.6514(3) 0.0503(11) Uani 1 1 d . . . . .
C5 C -0.0393(4) 0.3632(4) 0.5723(3) 0.0514(11) Uani 1 1 d . . . . .
H5 H -0.0742 0.4250 0.5892 0.062 Uiso 1 1 calc R U . . .
C6 C -0.0125(5) 0.2709(5) 0.7653(3) 0.0729(15) Uani 1 1 d . . . . .
H6A H -0.0915 0.3157 0.7800 0.087 Uiso 1 1 calc R U . . .
H6B H -0.0208 0.1995 0.8095 0.087 Uiso 1 1 calc R U . . .
C7 C -0.0038(4) 0.3642(3) 1.0516(3) 0.0385(8) Uani 1 1 d . . . . .
H7 H -0.0685 0.4093 1.0767 0.046 Uiso 1 1 calc R U . . .
C8 C 0.0051(4) 0.3718(3) 0.9462(3) 0.0461(10) Uani 1 1 d . . . . .
H8 H -0.0521 0.4215 0.9017 0.055 Uiso 1 1 calc R U . . .
C9 C 0.0990(4) 0.3057(3) 0.9062(3) 0.0415(9) Uani 1 1 d . . . . .
C10 C 0.1823(4) 0.2344(3) 0.9763(3) 0.0420(9) Uani 1 1 d . . . . .
H10 H 0.2471 0.1884 0.9527 0.050 Uiso 1 1 calc R U . . .
C11 C 0.1691(3) 0.2314(3) 1.0817(3) 0.0365(8) Uani 1 1 d . . . . .
H11 H 0.2270 0.1836 1.1272 0.044 Uiso 1 1 calc R U . . .
C12 C 0.1061(4) 0.3082(4) 0.7923(3) 0.0563(11) Uani 1 1 d . . . . .
H12A H 0.1138 0.3800 0.7488 0.068 Uiso 1 1 calc R U . . .
H12B H 0.1852 0.2640 0.7767 0.068 Uiso 1 1 calc R U . . .
C13 C 0.2663(3) 0.3630(2) 0.2565(2) 0.0261(7) Uani 1 1 d . . . . .
C14 C 0.3976(3) 0.4049(2) 0.2323(2) 0.0271(7) Uani 1 1 d . . . . .
C15 C 0.4062(3) 0.5107(3) 0.1763(3) 0.0324(7) Uani 1 1 d . . . . .
H15 H 0.3296 0.5557 0.1548 0.039 Uiso 1 1 calc R U . . .
C16 C 0.7633(3) 0.3067(2) 0.2740(2) 0.0251(7) Uani 1 1 d . . . . .
C17 C 0.6368(3) 0.3778(2) 0.2424(2) 0.0255(7) Uani 1 1 d . . . . .
C18 C 0.5138(3) 0.3385(2) 0.2635(2) 0.0267(7) Uani 1 1 d . . . . .
H18 H 0.5090 0.2674 0.2985 0.032 Uiso 1 1 calc R U . . .
C19 C 0.6442(3) 0.4825(2) 0.1870(3) 0.0301(7) Uani 1 1 d . . . . .
H19 H 0.7262 0.5089 0.1726 0.036 Uiso 1 1 calc R U . . .
C20 C 0.5303(3) 0.5483(2) 0.1529(3) 0.0323(7) Uani 1 1 d . . . . .
C22 C 0.4760(4) 0.6969(3) 0.0055(3) 0.0429(9) Uani 1 1 d . . . . .
H22A H 0.4377 0.6419 -0.0119 0.051 Uiso 1 1 calc R U . . .
H22B H 0.5371 0.7275 -0.0531 0.051 Uiso 1 1 calc R U . . .
C23 C 0.3664(3) 0.7813(3) 0.0193(3) 0.0330(8) Uani 1 1 d . . . . .
C24 C 0.3614(3) 0.8292(3) 0.0988(3) 0.0346(8) Uani 1 1 d . . . . .
H24 H 0.4258 0.8083 0.1476 0.042 Uiso 1 1 calc R U . . .
C25 C 0.2596(4) 0.9088(3) 0.1054(3) 0.0369(8) Uani 1 1 d . . . . .
C26 C 0.1670(4) 0.9408(3) 0.0307(3) 0.0457(10) Uani 1 1 d . . . . .
H26 H 0.0995 0.9946 0.0349 0.055 Uiso 1 1 calc R U . . .
C27 C 0.1722(4) 0.8948(3) -0.0500(3) 0.0553(11) Uani 1 1 d . . . . .
H27 H 0.1097 0.9174 -0.1004 0.066 Uiso 1 1 calc R U . . .
C28 C 0.2725(4) 0.8143(3) -0.0544(3) 0.0465(10) Uani 1 1 d . . . . .
H28 H 0.2767 0.7818 -0.1078 0.056 Uiso 1 1 calc R U . . .
C29 C 0.2452(4) 0.9602(3) 0.1945(3) 0.0427(9) Uani 1 1 d . . . . .
C58 C 0.6163(4) 0.1863(3) 0.5295(3) 0.0374(8) Uani 1 1 d . . . . .
H58 H 0.6969 0.1442 0.5268 0.045 Uiso 1 1 calc R U . . .
C59 C 0.6177(4) 0.2849(3) 0.5426(3) 0.0464(10) Uani 1 1 d . . . . .
H59 H 0.6980 0.3078 0.5487 0.056 Uiso 1 1 calc R U . . .
C60 C 0.5012(4) 0.3490(3) 0.5465(3) 0.0437(10) Uani 1 1 d . . . . .
C61 C 0.3844(4) 0.3101(3) 0.5386(3) 0.0464(10) Uani 1 1 d . . . . .
H61 H 0.3027 0.3505 0.5420 0.056 Uiso 1 1 calc R U . . .
C62 C 0.3911(4) 0.2110(3) 0.5256(3) 0.0389(8) Uani 1 1 d . . . . .
H62 H 0.3120 0.1861 0.5200 0.047 Uiso 1 1 calc R U . . .
C63 C 0.4997(5) 0.4603(3) 0.5541(3) 0.0592(12) Uani 1 1 d . . . . .
H63A H 0.5771 0.4643 0.5888 0.071 Uiso 1 1 calc R U . . .
H63B H 0.4209 0.4776 0.5963 0.071 Uiso 1 1 calc R U . . .
N1 N 0.0268(3) 0.2755(2) 0.4393(2) 0.0307(6) Uani 1 1 d . . . . .
N2 N 0.0765(3) 0.2946(2) 1.1208(2) 0.0296(6) Uani 1 1 d . . . . .
N5 N 0.5047(3) 0.14832(19) 0.5206(2) 0.0295(6) Uani 1 1 d . . . . .
Ni1 Ni 0.05457(4) 0.28338(3) 0.28109(3) 0.02339(12) Uani 1 1 d . . . . .
Ni2 Ni 0.5000 0.0000 0.5000 0.02640(15) Uani 1 2 d S . P . .
O1 O 0.2624(2) 0.26393(16) 0.28602(17) 0.0300(5) Uani 1 1 d . . . . .
O2 O 0.1596(2) 0.42492(17) 0.24552(18) 0.0318(5) Uani 1 1 d . . . . .
O3 O 0.8654(2) 0.35302(17) 0.26566(17) 0.0290(5) Uani 1 1 d . . . . .
O4 O 0.7608(2) 0.20881(18) 0.3035(2) 0.0382(6) Uani 1 1 d . . . . .
O5 O 0.0182(2) 0.12815(17) 0.32192(17) 0.0309(5) Uani 1 1 d . . . . .
O6 O 0.1316(3) 0.9973(2) 0.2170(2) 0.0618(8) Uani 1 1 d . . . . .
O7 O 0.3484(3) 0.9636(2) 0.2364(2) 0.0655(9) Uani 1 1 d . . . . .
O8 O 0.5483(2) 0.65084(18) 0.0969(2) 0.0469(7) Uani 1 1 d . . . . .
O17 O 0.6536(2) 0.02321(18) 0.37911(19) 0.0417(6) Uani 1 1 d . . . . .
O18 O 0.6415(3) -0.05945(18) 0.61270(19) 0.0423(6) Uani 1 1 d . . . . .
O21 O 0.3844(4) 0.0550(3) 0.7865(3) 0.0770(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.340(4) . ?
C1 C5 1.377(5) . ?
C1 H1 0.9300 . ?
C2 N1 1.338(4) . ?
C2 C3 1.399(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.364(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(6) . ?
C4 C6 1.508(5) . ?
C5 H5 0.9300 . ?
C6 C12 1.482(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N2 1.352(4) . ?
C7 C8 1.372(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.379(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.385(5) . ?
C9 C12 1.504(5) . ?
C10 C11 1.385(5) . ?
C10 H10 0.9300 . ?
C11 N2 1.341(4) . ?
C11 H11 0.9300 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 O2 1.262(3) . ?
C13 O1 1.266(4) . ?
C13 C14 1.487(4) . ?
C13 Ni1 2.480(3) . ?
C14 C18 1.396(4) . ?
C14 C15 1.398(4) . ?
C15 C20 1.394(5) . ?
C15 H15 0.9300 . ?
C16 O4 1.249(4) . ?
C16 O3 1.259(4) . ?
C16 C17 1.508(4) . ?
C17 C19 1.382(4) . ?
C17 C18 1.393(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.383(4) . ?
C19 H19 0.9300 . ?
C20 O8 1.378(4) . ?
C22 O8 1.425(4) . ?
C22 C23 1.505(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C28 1.379(5) . ?
C23 C24 1.381(5) . ?
C24 C25 1.391(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.378(5) . ?
C25 C29 1.520(5) . ?
C26 C27 1.379(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.384(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 O6 1.234(5) . ?
C29 O7 1.253(5) . ?
C58 N5 1.336(4) . ?
C58 C59 1.376(5) . ?
C58 H58 0.9300 . ?
C59 C60 1.367(5) . ?
C59 H59 0.9300 . ?
C60 C61 1.386(6) . ?
C60 C63 1.513(5) . ?
C61 C62 1.372(5) . ?
C61 H61 0.9300 . ?
C62 N5 1.336(4) . ?
C62 H62 0.9300 . ?
C63 C63 1.518(8) 2_666 ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
N1 Ni1 2.070(3) . ?
N2 Ni1 2.086(3) 1_556 ?
N5 Ni2 2.081(3) . ?
Ni1 O3 2.021(2) 1_455 ?
Ni1 O5 2.054(2) . ?
Ni1 N2 2.086(3) 1_554 ?
Ni1 O1 2.099(2) . ?
Ni1 O2 2.202(2) . ?
Ni2 N5 2.081(3) 2_656 ?
Ni2 O18 2.098(2) 2_656 ?
Ni2 O18 2.098(2) . ?
Ni2 O17 2.106(2) 2_656 ?
Ni2 O17 2.106(2) . ?
O3 Ni1 2.021(2) 1_655 ?

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 C5 123.0(4) . . ?
N1 C1 H1 118.5 . . ?
C5 C1 H1 118.5 . . ?
N1 C2 C3 122.0(4) . . ?
N1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 117.3(4) . . ?
C3 C4 C6 120.8(4) . . ?
C5 C4 C6 121.9(4) . . ?
C1 C5 C4 119.8(4) . . ?
C1 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C12 C6 C4 112.3(3) . . ?
C12 C6 H6A 109.2 . . ?
C4 C6 H6A 109.2 . . ?
C12 C6 H6B 109.2 . . ?
C4 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 C8 123.4(3) . . ?
N2 C7 H7 118.3 . . ?
C8 C7 H7 118.3 . . ?
C7 C8 C9 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 C10 117.2(3) . . ?
C8 C9 C12 121.1(4) . . ?
C10 C9 C12 121.7(4) . . ?
C9 C10 C11 120.0(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
N2 C11 C10 122.8(3) . . ?
N2 C11 H11 118.6 . . ?
C10 C11 H11 118.6 . . ?
C6 C12 C9 112.2(3) . . ?
C6 C12 H12A 109.2 . . ?
C9 C12 H12A 109.2 . . ?
C6 C12 H12B 109.2 . . ?
C9 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
O2 C13 O1 120.1(3) . . ?
O2 C13 C14 120.7(3) . . ?
O1 C13 C14 119.2(3) . . ?
O2 C13 Ni1 62.46(17) . . ?
O1 C13 Ni1 57.79(16) . . ?
C14 C13 Ni1 173.6(2) . . ?
C18 C14 C15 119.4(3) . . ?
C18 C14 C13 120.3(3) . . ?
C15 C14 C13 120.3(3) . . ?
C20 C15 C14 119.5(3) . . ?
C20 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
O4 C16 O3 125.3(3) . . ?
O4 C16 C17 119.2(3) . . ?
O3 C16 C17 115.5(3) . . ?
C19 C17 C18 119.7(3) . . ?
C19 C17 C16 119.2(3) . . ?
C18 C17 C16 121.1(3) . . ?
C17 C18 C14 120.5(3) . . ?
C17 C18 H18 119.8 . . ?
C14 C18 H18 119.8 . . ?
C17 C19 C20 120.3(3) . . ?
C17 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
O8 C20 C19 116.0(3) . . ?
O8 C20 C15 123.4(3) . . ?
C19 C20 C15 120.6(3) . . ?
O8 C22 C23 113.0(3) . . ?
O8 C22 H22A 109.0 . . ?
C23 C22 H22A 109.0 . . ?
O8 C22 H22B 109.0 . . ?
C23 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C28 C23 C24 119.9(3) . . ?
C28 C23 C22 117.5(3) . . ?
C24 C23 C22 122.5(3) . . ?
C23 C24 C25 119.7(3) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 119.4(3) . . ?
C26 C25 C29 118.7(3) . . ?
C24 C25 C29 121.9(3) . . ?
C25 C26 C27 121.4(3) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 H26 119.3 . . ?
C26 C27 C28 118.5(4) . . ?
C26 C27 H27 120.8 . . ?
C28 C27 H27 120.8 . . ?
C23 C28 C27 121.1(4) . . ?
C23 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
O6 C29 O7 126.0(4) . . ?
O6 C29 C25 116.1(4) . . ?
O7 C29 C25 117.9(3) . . ?
N5 C58 C59 123.1(3) . . ?
N5 C58 H58 118.5 . . ?
C59 C58 H58 118.5 . . ?
C60 C59 C58 120.0(4) . . ?
C60 C59 H59 120.0 . . ?
C58 C59 H59 120.0 . . ?
C59 C60 C61 117.6(3) . . ?
C59 C60 C63 121.4(4) . . ?
C61 C60 C63 121.0(4) . . ?
C62 C61 C60 119.1(4) . . ?
C62 C61 H61 120.5 . . ?
C60 C61 H61 120.5 . . ?
N5 C62 C61 123.7(4) . . ?
N5 C62 H62 118.1 . . ?
C61 C62 H62 118.1 . . ?
C60 C63 C63 111.2(4) . 2_666 ?
C60 C63 H63A 109.4 . . ?
C63 C63 H63A 109.4 2_666 . ?
C60 C63 H63B 109.4 . . ?
C63 C63 H63B 109.4 2_666 . ?
H63A C63 H63B 108.0 . . ?
C2 N1 C1 117.4(3) . . ?
C2 N1 Ni1 122.6(2) . . ?
C1 N1 Ni1 120.0(2) . . ?
C11 N2 C7 116.6(3) . . ?
C11 N2 Ni1 121.6(2) . 1_556 ?
C7 N2 Ni1 121.7(2) . 1_556 ?
C58 N5 C62 116.6(3) . . ?
C58 N5 Ni2 123.8(2) . . ?
C62 N5 Ni2 119.6(2) . . ?
O3 Ni1 O5 98.89(9) 1_455 . ?
O3 Ni1 N1 87.86(10) 1_455 . ?
O5 Ni1 N1 87.85(10) . . ?
O3 Ni1 N2 90.23(10) 1_455 1_554 ?
O5 Ni1 N2 92.79(10) . 1_554 ?
N1 Ni1 N2 178.06(10) . 1_554 ?
O3 Ni1 O1 160.82(9) 1_455 . ?
O5 Ni1 O1 100.25(9) . . ?
N1 Ni1 O1 91.84(10) . . ?
N2 Ni1 O1 89.86(10) 1_554 . ?
O3 Ni1 O2 99.66(9) 1_455 . ?
O5 Ni1 O2 161.42(8) . . ?
N1 Ni1 O2 91.92(10) . . ?
N2 Ni1 O2 88.06(10) 1_554 . ?
O1 Ni1 O2 61.18(8) . . ?
O3 Ni1 C13 130.19(10) 1_455 . ?
O5 Ni1 C13 130.92(9) . . ?
N1 Ni1 C13 93.58(10) . . ?
N2 Ni1 C13 87.39(10) 1_554 . ?
O1 Ni1 C13 30.69(9) . . ?
O2 Ni1 C13 30.55(8) . . ?
N5 Ni2 N5 180.0 . 2_656 ?
N5 Ni2 O18 92.18(10) . 2_656 ?
N5 Ni2 O18 87.82(10) 2_656 2_656 ?
N5 Ni2 O18 87.82(10) . . ?
N5 Ni2 O18 92.18(10) 2_656 . ?
O18 Ni2 O18 180.0 2_656 . ?
N5 Ni2 O17 87.45(10) . 2_656 ?
N5 Ni2 O17 92.55(10) 2_656 2_656 ?
O18 Ni2 O17 90.16(11) 2_656 2_656 ?
O18 Ni2 O17 89.84(11) . 2_656 ?
N5 Ni2 O17 92.55(10) . . ?
N5 Ni2 O17 87.45(10) 2_656 . ?
O18 Ni2 O17 89.84(11) 2_656 . ?
O18 Ni2 O17 90.16(11) . . ?
O17 Ni2 O17 180.0 2_656 . ?
C13 O1 Ni1 91.53(17) . . ?
C13 O2 Ni1 86.99(19) . . ?
C16 O3 Ni1 126.2(2) . 1_655 ?
C20 O8 C22 117.3(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
N1 C2 C3 C4 0.3(6) . . . . ?
C2 C3 C4 C5 2.1(6) . . . . ?
C2 C3 C4 C6 -176.0(4) . . . . ?
N1 C1 C5 C4 0.4(6) . . . . ?
C3 C4 C5 C1 -2.5(6) . . . . ?
C6 C4 C5 C1 175.6(4) . . . . ?
C3 C4 C6 C12 95.8(5) . . . . ?
C5 C4 C6 C12 -82.3(6) . . . . ?
N2 C7 C8 C9 0.5(6) . . . . ?
C7 C8 C9 C10 -0.8(6) . . . . ?
C7 C8 C9 C12 176.6(4) . . . . ?
C8 C9 C10 C11 0.1(6) . . . . ?
C12 C9 C10 C11 -177.3(4) . . . . ?
C9 C10 C11 N2 1.0(6) . . . . ?
C4 C6 C12 C9 -179.2(4) . . . . ?
C8 C9 C12 C6 -66.8(6) . . . . ?
C10 C9 C12 C6 110.5(5) . . . . ?
O2 C13 C14 C18 167.6(3) . . . . ?
O1 C13 C14 C18 -14.2(5) . . . . ?
O2 C13 C14 C15 -13.7(5) . . . . ?
O1 C13 C14 C15 164.6(3) . . . . ?
C18 C14 C15 C20 -0.3(5) . . . . ?
C13 C14 C15 C20 -179.1(3) . . . . ?
O4 C16 C17 C19 -164.9(3) . . . . ?
O3 C16 C17 C19 13.6(4) . . . . ?
O4 C16 C17 C18 11.9(5) . . . . ?
O3 C16 C17 C18 -169.6(3) . . . . ?
C19 C17 C18 C14 -2.3(5) . . . . ?
C16 C17 C18 C14 -179.0(3) . . . . ?
C15 C14 C18 C17 2.3(5) . . . . ?
C13 C14 C18 C17 -179.0(3) . . . . ?
C18 C17 C19 C20 0.3(5) . . . . ?
C16 C17 C19 C20 177.1(3) . . . . ?
C17 C19 C20 O8 -179.0(3) . . . . ?
C17 C19 C20 C15 1.7(5) . . . . ?
C14 C15 C20 O8 179.1(3) . . . . ?
C14 C15 C20 C19 -1.7(5) . . . . ?
O8 C22 C23 C28 -166.0(3) . . . . ?
O8 C22 C23 C24 17.4(5) . . . . ?
C28 C23 C24 C25 1.6(5) . . . . ?
C22 C23 C24 C25 178.1(3) . . . . ?
C23 C24 C25 C26 -1.8(5) . . . . ?
C23 C24 C25 C29 176.7(3) . . . . ?
C24 C25 C26 C27 0.7(6) . . . . ?
C29 C25 C26 C27 -177.9(4) . . . . ?
C25 C26 C27 C28 0.6(7) . . . . ?
C24 C23 C28 C27 -0.3(6) . . . . ?
C22 C23 C28 C27 -177.0(4) . . . . ?
C26 C27 C28 C23 -0.8(7) . . . . ?
C26 C25 C29 O6 25.2(5) . . . . ?
C24 C25 C29 O6 -153.3(4) . . . . ?
C26 C25 C29 O7 -153.0(4) . . . . ?
C24 C25 C29 O7 28.5(5) . . . . ?
N5 C58 C59 C60 -0.3(6) . . . . ?
C58 C59 C60 C61 1.0(6) . . . . ?
C58 C59 C60 C63 -176.2(3) . . . . ?
C59 C60 C61 C62 -1.1(6) . . . . ?
C63 C60 C61 C62 176.2(3) . . . . ?
C60 C61 C62 N5 0.4(6) . . . . ?
C59 C60 C63 C63 93.3(6) . . . 2_666 ?
C61 C60 C63 C63 -83.8(6) . . . 2_666 ?
C3 C2 N1 C1 -2.4(5) . . . . ?
C3 C2 N1 Ni1 177.6(3) . . . . ?
C5 C1 N1 C2 2.0(5) . . . . ?
C5 C1 N1 Ni1 -178.0(3) . . . . ?
C10 C11 N2 C7 -1.2(5) . . . . ?
C10 C11 N2 Ni1 177.4(3) . . . 1_556 ?
C8 C7 N2 C11 0.5(5) . . . . ?
C8 C7 N2 Ni1 -178.1(3) . . . 1_556 ?
C59 C58 N5 C62 -0.4(5) . . . . ?
C59 C58 N5 Ni2 179.6(3) . . . . ?
C61 C62 N5 C58 0.3(5) . . . . ?
C61 C62 N5 Ni2 -179.7(3) . . . . ?
O2 C13 O1 Ni1 4.9(3) . . . . ?
C14 C13 O1 Ni1 -173.4(3) . . . . ?
O1 C13 O2 Ni1 -4.6(3) . . . . ?
C14 C13 O2 Ni1 173.6(3) . . . . ?
O4 C16 O3 Ni1 7.5(5) . . . 1_655 ?
C17 C16 O3 Ni1 -170.86(18) . . . 1_655 ?
C19 C20 O8 C22 137.0(3) . . . . ?
C15 C20 O8 C22 -43.7(5) . . . . ?
C23 C22 O8 C20 109.2(4) . . . . ?

_refine_diff_density_max         0.620
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.086


_exptl_crystal_recrystallization_method 'hydrothermal synthesis'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1818378'
_audit_update_record             
;
2018-01-21 deposited with the CCDC.
2018-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H28 N2 Ni2 O11'
_chemical_formula_weight         685.94

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           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

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

_cell_length_a                   15.224(6)
_cell_length_b                   11.113(4)
_cell_length_c                   19.333(7)
_cell_angle_alpha                90
_cell_angle_beta                 108.501(5)
_cell_angle_gamma                90
_cell_volume                     3102(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2565
_cell_measurement_theta_min      2.313
_cell_measurement_theta_max      27.665

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    1.274
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18062
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.054
_diffrn_reflns_theta_max         27.665
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7066
_reflns_number_gt                3919
_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)+(0.1213P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7066
_refine_ls_number_parameters     389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0660
_refine_ls_wR_factor_ref         0.2230
_refine_ls_wR_factor_gt          0.1896
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
C1 C 0.5546(3) 0.6940(4) 0.2899(3) 0.0250(11) Uani 1 1 d . . . . .
C2 C 0.4795(4) 0.6959(4) 0.3174(3) 0.0285(11) Uani 1 1 d . . . . .
H2 H 0.4542 0.6242 0.3271 0.034 Uiso 1 1 calc R U . . .
C3 C 0.4435(4) 0.8045(4) 0.3299(3) 0.0283(11) Uani 1 1 d . . . . .
C4 C 0.4803(3) 0.9115(5) 0.3150(3) 0.0287(11) Uani 1 1 d . . . . .
H4 H 0.4554 0.9844 0.3233 0.034 Uiso 1 1 calc R U . . .
C5 C 0.5541(3) 0.9106(4) 0.2877(3) 0.0244(11) Uani 1 1 d . . . . .
C6 C 0.5916(3) 0.8020(4) 0.2749(3) 0.0242(10) Uani 1 1 d . . . . .
H6 H 0.6410 0.8013 0.2563 0.029 Uiso 1 1 calc R U . . .
C7 C 0.5967(4) 0.5759(4) 0.2793(3) 0.0292(12) Uani 1 1 d . . . . .
C8 C 0.5893(4) 1.0312(4) 0.2728(3) 0.0280(12) Uani 1 1 d . . . . .
C9 C 0.3303(5) 0.9044(6) 0.3689(4) 0.061(2) Uani 1 1 d . . . . .
H9A H 0.3013 0.9438 0.3225 0.073 Uiso 1 1 calc R U . . .
H9B H 0.3781 0.9574 0.3985 0.073 Uiso 1 1 calc R U . . .
C10 C 0.2583(5) 0.8834(6) 0.4068(4) 0.0534(18) Uani 1 1 d . . . . .
C11 C 0.1663(5) 0.9048(9) 0.3716(4) 0.077(3) Uani 1 1 d . . . . .
H11 H 0.1464 0.9269 0.3227 0.092 Uiso 1 1 calc R U . . .
C12 C 0.1035(5) 0.8935(9) 0.4091(4) 0.075(3) Uani 1 1 d . . . . .
H12 H 0.0411 0.9095 0.3857 0.091 Uiso 1 1 calc R U . . .
C13 C 0.1324(4) 0.8590(7) 0.4802(3) 0.0527(17) Uani 1 1 d . . . . .
H13 H 0.0897 0.8540 0.5055 0.063 Uiso 1 1 calc R U . . .
C14 C 0.2244(4) 0.8311(5) 0.5157(3) 0.0350(13) Uani 1 1 d . . . . .
C15 C 0.2868(4) 0.8436(6) 0.4782(3) 0.0447(15) Uani 1 1 d . . . . .
H15 H 0.3489 0.8250 0.5011 0.054 Uiso 1 1 calc R U . . .
C16 C 0.2588(4) 0.7956(5) 0.5949(3) 0.0341(13) Uani 1 1 d . . . . .
C17 C 0.3968(4) 0.4096(6) 0.1772(4) 0.0535(17) Uani 1 1 d . . . . .
H17 H 0.4021 0.4690 0.2122 0.064 Uiso 1 1 calc R U . . .
C18 C 0.3258(5) 0.4185(7) 0.1115(4) 0.062(2) Uani 1 1 d . . . . .
H18 H 0.2846 0.4827 0.1038 0.074 Uiso 1 1 calc R U . . .
C19 C 0.3156(4) 0.3340(7) 0.0577(4) 0.0514(18) Uani 1 1 d . . . . .
C20 C 0.3821(5) 0.2412(7) 0.0731(4) 0.0569(18) Uani 1 1 d . . . . .
H20 H 0.3798 0.1821 0.0385 0.068 Uiso 1 1 calc R U . . .
C21 C 0.4501(4) 0.2388(6) 0.1393(4) 0.0491(16) Uani 1 1 d . . . . .
H21 H 0.4936 0.1772 0.1478 0.059 Uiso 1 1 calc R U . . .
C22 C 0.2349(5) 0.3309(7) -0.0124(4) 0.063(2) Uani 1 1 d . . . . .
H22A H 0.2041 0.4085 -0.0199 0.076 Uiso 1 1 calc R U . . .
H22B H 0.2579 0.3164 -0.0530 0.076 Uiso 1 1 calc R U . . .
C23 C 0.1665(5) 0.2349(8) -0.0108(4) 0.063(2) Uani 1 1 d . . . . .
H23A H 0.1210 0.2279 -0.0588 0.075 Uiso 1 1 calc R U . . .
H23B H 0.1985 0.1584 0.0009 0.075 Uiso 1 1 calc R U . . .
C24 C 0.1181(4) 0.2607(6) 0.0437(3) 0.0434(15) Uani 1 1 d . . . . .
C25 C 0.1484(4) 0.2137(6) 0.1140(4) 0.0457(16) Uani 1 1 d . . . . .
H25 H 0.2019 0.1672 0.1291 0.055 Uiso 1 1 calc R U . . .
C26 C 0.0984(4) 0.2363(6) 0.1613(4) 0.0431(15) Uani 1 1 d . . . . .
H26 H 0.1201 0.2035 0.2079 0.052 Uiso 1 1 calc R U . . .
C27 C -0.0059(5) 0.3492(6) 0.0785(4) 0.0496(16) Uani 1 1 d . . . . .
H27 H -0.0583 0.3978 0.0659 0.060 Uiso 1 1 calc R U . . .
C28 C 0.0394(4) 0.3297(6) 0.0274(4) 0.0521(18) Uani 1 1 d . . . . .
H28 H 0.0160 0.3641 -0.0187 0.062 Uiso 1 1 calc R U . . .
N1 N 0.4583(3) 0.3185(4) 0.1925(3) 0.0381(12) Uani 1 1 d . . . . .
N2 N 0.0229(3) 0.3009(4) 0.1446(3) 0.0323(10) Uani 1 1 d . . . . .
Ni1 Ni 0.56799(5) 0.30345(6) 0.29095(4) 0.0268(2) Uani 1 1 d . . . . .
Ni2 Ni 0.7500 0.44713(8) 0.2500 0.0290(3) Uani 1 2 d S T P . .
Ni3 Ni 0.7500 1.16797(8) 0.2500 0.0231(2) Uani 1 2 d S T P . .
O1 O 0.5732(3) 0.4860(3) 0.3094(2) 0.0384(10) Uani 1 1 d . . . . .
O2 O 0.6518(3) 0.5765(3) 0.2430(2) 0.0434(10) Uani 1 1 d . . . . .
O3 O 0.6551(2) 1.0300(3) 0.2438(2) 0.0320(9) Uani 1 1 d . . . . .
O4 O 0.5524(3) 1.1184(3) 0.2872(2) 0.0401(10) Uani 1 1 d . . . . .
O5 O 0.3702(3) 0.7973(4) 0.3572(2) 0.0468(11) Uani 1 1 d . . . . .
O6 O 0.3250(3) 0.7206(4) 0.6128(2) 0.0397(10) Uani 1 1 d . . . . .
O7 O 0.2190(3) 0.8404(3) 0.63673(19) 0.0336(9) Uani 1 1 d . . . . .
O8 O 0.7117(3) 0.4580(4) 0.1357(2) 0.0476(11) Uani 1 1 d . . . . .
O9 O 0.6581(2) 1.3069(3) 0.23534(19) 0.0251(7) Uani 1 1 d . . . . .
O10 O 0.5910(5) 0.6693(6) 0.0984(4) 0.105(2) Uani 1 1 d . . . . .
O11 O 0.6540(5) 0.9081(6) 0.1114(3) 0.118(3) 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 C6 1.395(6) . ?
C1 C2 1.405(7) . ?
C1 C7 1.503(7) . ?
C2 C3 1.379(7) . ?
C3 O5 1.379(6) . ?
C3 C4 1.383(7) . ?
C4 C5 1.385(6) . ?
C5 C6 1.390(6) . ?
C5 C8 1.505(6) . ?
C7 O2 1.253(6) . ?
C7 O1 1.264(6) . ?
C8 O4 1.196(6) . ?
C8 O3 1.294(6) . ?
C9 O5 1.388(7) . ?
C9 C10 1.517(8) . ?
C10 C11 1.370(9) . ?
C10 C15 1.381(8) . ?
C11 C12 1.377(9) . ?
C12 C13 1.360(9) . ?
C13 C14 1.384(8) . ?
C14 C15 1.374(8) . ?
C14 C16 1.505(8) . ?
C16 O7 1.258(6) . ?
C16 O6 1.269(6) . ?
C17 N1 1.347(7) . ?
C17 C18 1.385(9) . ?
C18 C19 1.374(10) . ?
C19 C20 1.410(9) . ?
C19 C22 1.513(9) . ?
C20 C21 1.367(9) . ?
C21 N1 1.333(7) . ?
C22 C23 1.498(10) . ?
C23 C24 1.492(8) . ?
C24 C28 1.372(9) . ?
C24 C25 1.391(9) . ?
C25 C26 1.386(8) . ?
C26 N2 1.306(7) . ?
C27 N2 1.325(8) . ?
C27 C28 1.391(9) . ?
N1 Ni1 2.103(5) . ?
N2 Ni1 2.136(4) 2 ?
Ni1 O9 1.994(3) 1_545 ?
Ni1 O1 2.057(4) . ?
Ni1 O6 2.065(4) 3_666 ?
Ni1 O4 2.069(4) 1_545 ?
Ni1 N2 2.136(4) 2 ?
Ni2 O2 2.048(4) 2_655 ?
Ni2 O2 2.048(4) . ?
Ni2 O9 2.052(3) 1_545 ?
Ni2 O9 2.052(3) 2_645 ?
Ni2 O8 2.103(4) . ?
Ni2 O8 2.103(4) 2_655 ?
Ni3 O9 2.042(3) . ?
Ni3 O9 2.042(3) 2_655 ?
Ni3 O3 2.084(3) . ?
Ni3 O3 2.084(3) 2_655 ?
Ni3 O7 2.091(4) 4_675 ?
Ni3 O7 2.091(4) 3_676 ?
O4 Ni1 2.069(4) 1_565 ?
O6 Ni1 2.065(4) 3_666 ?
O7 Ni3 2.091(4) 3_676 ?
O9 Ni1 1.994(3) 1_565 ?
O9 Ni2 2.052(3) 1_565 ?

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
C6 C1 C2 119.8(4) . . ?
C6 C1 C7 120.3(4) . . ?
C2 C1 C7 119.9(4) . . ?
C3 C2 C1 119.7(5) . . ?
C2 C3 O5 115.5(4) . . ?
C2 C3 C4 120.4(5) . . ?
O5 C3 C4 124.1(4) . . ?
C3 C4 C5 120.3(5) . . ?
C4 C5 C6 120.2(5) . . ?
C4 C5 C8 116.6(5) . . ?
C6 C5 C8 123.2(4) . . ?
C5 C6 C1 119.6(4) . . ?
O2 C7 O1 126.8(5) . . ?
O2 C7 C1 117.6(4) . . ?
O1 C7 C1 115.6(4) . . ?
O4 C8 O3 126.5(5) . . ?
O4 C8 C5 117.1(5) . . ?
O3 C8 C5 116.4(4) . . ?
O5 C9 C10 111.6(5) . . ?
C11 C10 C15 120.0(6) . . ?
C11 C10 C9 120.9(6) . . ?
C15 C10 C9 119.1(6) . . ?
C10 C11 C12 119.6(6) . . ?
C13 C12 C11 120.1(6) . . ?
C12 C13 C14 121.1(6) . . ?
C15 C14 C13 118.5(5) . . ?
C15 C14 C16 119.2(5) . . ?
C13 C14 C16 122.2(5) . . ?
C14 C15 C10 120.6(6) . . ?
O7 C16 O6 126.0(5) . . ?
O7 C16 C14 117.9(5) . . ?
O6 C16 C14 116.1(5) . . ?
N1 C17 C18 122.7(7) . . ?
C19 C18 C17 120.9(7) . . ?
C18 C19 C20 116.0(6) . . ?
C18 C19 C22 124.0(7) . . ?
C20 C19 C22 119.8(7) . . ?
C21 C20 C19 119.4(7) . . ?
N1 C21 C20 124.6(6) . . ?
C23 C22 C19 111.7(6) . . ?
C24 C23 C22 112.3(6) . . ?
C28 C24 C25 115.4(6) . . ?
C28 C24 C23 122.4(6) . . ?
C25 C24 C23 122.2(6) . . ?
C26 C25 C24 119.7(6) . . ?
N2 C26 C25 124.2(6) . . ?
N2 C27 C28 122.4(6) . . ?
C24 C28 C27 121.1(6) . . ?
C21 N1 C17 116.2(6) . . ?
C21 N1 Ni1 119.9(4) . . ?
C17 N1 Ni1 123.8(4) . . ?
C26 N2 C27 117.1(5) . . ?
C26 N2 Ni1 123.1(4) . 2 ?
C27 N2 Ni1 118.7(4) . 2 ?
O9 Ni1 O1 94.53(14) 1_545 . ?
O9 Ni1 O6 90.43(15) 1_545 3_666 ?
O1 Ni1 O6 89.74(16) . 3_666 ?
O9 Ni1 O4 95.23(13) 1_545 1_545 ?
O1 Ni1 O4 169.81(15) . 1_545 ?
O6 Ni1 O4 87.23(16) 3_666 1_545 ?
O9 Ni1 N1 89.74(17) 1_545 . ?
O1 Ni1 N1 93.11(17) . . ?
O6 Ni1 N1 177.11(17) 3_666 . ?
O4 Ni1 N1 89.89(17) 1_545 . ?
O9 Ni1 N2 177.15(17) 1_545 2 ?
O1 Ni1 N2 84.75(15) . 2 ?
O6 Ni1 N2 86.81(17) 3_666 2 ?
O4 Ni1 N2 85.37(15) 1_545 2 ?
N1 Ni1 N2 93.05(19) . 2 ?
O2 Ni2 O2 90.8(2) 2_655 . ?
O2 Ni2 O9 173.46(14) 2_655 1_545 ?
O2 Ni2 O9 94.15(15) . 1_545 ?
O2 Ni2 O9 94.15(15) 2_655 2_645 ?
O2 Ni2 O9 173.46(14) . 2_645 ?
O9 Ni2 O9 81.23(19) 1_545 2_645 ?
O2 Ni2 O8 88.99(17) 2_655 . ?
O2 Ni2 O8 86.39(16) . . ?
O9 Ni2 O8 87.08(15) 1_545 . ?
O9 Ni2 O8 97.94(15) 2_645 . ?
O2 Ni2 O8 86.39(16) 2_655 2_655 ?
O2 Ni2 O8 88.99(17) . 2_655 ?
O9 Ni2 O8 97.94(15) 1_545 2_655 ?
O9 Ni2 O8 87.08(15) 2_645 2_655 ?
O8 Ni2 O8 173.4(2) . 2_655 ?
O9 Ni3 O9 81.72(18) . 2_655 ?
O9 Ni3 O3 96.71(14) . . ?
O9 Ni3 O3 175.06(13) 2_655 . ?
O9 Ni3 O3 175.05(13) . 2_655 ?
O9 Ni3 O3 96.71(14) 2_655 2_655 ?
O3 Ni3 O3 85.2(2) . 2_655 ?
O9 Ni3 O7 88.35(14) . 4_675 ?
O9 Ni3 O7 95.52(14) 2_655 4_675 ?
O3 Ni3 O7 89.10(14) . 4_675 ?
O3 Ni3 O7 87.13(14) 2_655 4_675 ?
O9 Ni3 O7 95.53(14) . 3_676 ?
O9 Ni3 O7 88.35(14) 2_655 3_676 ?
O3 Ni3 O7 87.13(14) . 3_676 ?
O3 Ni3 O7 89.10(14) 2_655 3_676 ?
O7 Ni3 O7 174.9(2) 4_675 3_676 ?
C7 O1 Ni1 134.5(4) . . ?
C7 O2 Ni2 124.3(3) . . ?
C8 O3 Ni3 125.8(3) . . ?
C8 O4 Ni1 139.1(4) . 1_565 ?
C3 O5 C9 117.5(4) . . ?
C16 O6 Ni1 131.5(4) . 3_666 ?
C16 O7 Ni3 131.4(4) . 3_676 ?
Ni1 O9 Ni3 117.94(16) 1_565 . ?
Ni1 O9 Ni2 119.72(16) 1_565 1_565 ?
Ni3 O9 Ni2 98.53(15) . 1_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.6(8) . . . . ?
C7 C1 C2 C3 177.4(5) . . . . ?
C1 C2 C3 O5 -179.7(5) . . . . ?
C1 C2 C3 C4 0.5(8) . . . . ?
C2 C3 C4 C5 -0.3(8) . . . . ?
O5 C3 C4 C5 179.9(5) . . . . ?
C3 C4 C5 C6 0.2(8) . . . . ?
C3 C4 C5 C8 179.7(5) . . . . ?
C4 C5 C6 C1 -0.3(8) . . . . ?
C8 C5 C6 C1 -179.8(4) . . . . ?
C2 C1 C6 C5 0.5(8) . . . . ?
C7 C1 C6 C5 -177.5(5) . . . . ?
C6 C1 C7 O2 -14.5(8) . . . . ?
C2 C1 C7 O2 167.5(5) . . . . ?
C6 C1 C7 O1 164.5(5) . . . . ?
C2 C1 C7 O1 -13.5(7) . . . . ?
C4 C5 C8 O4 1.6(7) . . . . ?
C6 C5 C8 O4 -178.9(5) . . . . ?
C4 C5 C8 O3 -176.5(5) . . . . ?
C6 C5 C8 O3 3.0(7) . . . . ?
O5 C9 C10 C11 -112.9(8) . . . . ?
O5 C9 C10 C15 67.9(9) . . . . ?
C15 C10 C11 C12 4.0(13) . . . . ?
C9 C10 C11 C12 -175.3(8) . . . . ?
C10 C11 C12 C13 -1.3(14) . . . . ?
C11 C12 C13 C14 -2.0(13) . . . . ?
C12 C13 C14 C15 2.5(11) . . . . ?
C12 C13 C14 C16 178.5(7) . . . . ?
C13 C14 C15 C10 0.2(10) . . . . ?
C16 C14 C15 C10 -175.9(6) . . . . ?
C11 C10 C15 C14 -3.4(11) . . . . ?
C9 C10 C15 C14 175.8(6) . . . . ?
C15 C14 C16 O7 144.4(6) . . . . ?
C13 C14 C16 O7 -31.6(9) . . . . ?
C15 C14 C16 O6 -36.8(8) . . . . ?
C13 C14 C16 O6 147.3(6) . . . . ?
N1 C17 C18 C19 -0.8(11) . . . . ?
C17 C18 C19 C20 -1.3(10) . . . . ?
C17 C18 C19 C22 173.9(6) . . . . ?
C18 C19 C20 C21 1.3(10) . . . . ?
C22 C19 C20 C21 -174.1(6) . . . . ?
C19 C20 C21 N1 0.9(11) . . . . ?
C18 C19 C22 C23 -103.3(8) . . . . ?
C20 C19 C22 C23 71.8(8) . . . . ?
C19 C22 C23 C24 67.1(8) . . . . ?
C22 C23 C24 C28 86.7(8) . . . . ?
C22 C23 C24 C25 -95.0(8) . . . . ?
C28 C24 C25 C26 1.2(9) . . . . ?
C23 C24 C25 C26 -177.2(6) . . . . ?
C24 C25 C26 N2 -0.3(10) . . . . ?
C25 C24 C28 C27 -0.4(10) . . . . ?
C23 C24 C28 C27 178.0(7) . . . . ?
N2 C27 C28 C24 -1.3(11) . . . . ?
C20 C21 N1 C17 -3.0(10) . . . . ?
C20 C21 N1 Ni1 -179.2(5) . . . . ?
C18 C17 N1 C21 2.9(9) . . . . ?
C18 C17 N1 Ni1 179.0(5) . . . . ?
C25 C26 N2 C27 -1.4(9) . . . . ?
C25 C26 N2 Ni1 166.4(5) . . . 2 ?
C28 C27 N2 C26 2.2(9) . . . . ?
C28 C27 N2 Ni1 -166.1(5) . . . 2 ?
O2 C7 O1 Ni1 -25.2(9) . . . . ?
C1 C7 O1 Ni1 156.0(4) . . . . ?
O1 C7 O2 Ni2 -21.2(8) . . . . ?
C1 C7 O2 Ni2 157.7(4) . . . . ?
O4 C8 O3 Ni3 25.5(8) . . . . ?
C5 C8 O3 Ni3 -156.6(3) . . . . ?
O3 C8 O4 Ni1 -9.0(10) . . . 1_565 ?
C5 C8 O4 Ni1 173.1(4) . . . 1_565 ?
C2 C3 O5 C9 -178.5(5) . . . . ?
C4 C3 O5 C9 1.3(9) . . . . ?
C10 C9 O5 C3 -173.5(6) . . . . ?
O7 C16 O6 Ni1 -31.7(8) . . . 3_666 ?
C14 C16 O6 Ni1 149.5(4) . . . 3_666 ?
O6 C16 O7 Ni3 8.3(9) . . . 3_676 ?
C14 C16 O7 Ni3 -173.0(4) . . . 3_676 ?

_refine_diff_density_max         1.749
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.130


_exptl_crystal_recrystallization_method 'hydrothermal synthesis'
_exptl_crystal_preparation       'Magnetic properties'
