# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2145462'
loop_
_audit_author_name
_audit_author_address
'Jayasree K'
;Indian Institute of Technology, Madras
India
;
_audit_update_record             
;
2022-01-30 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H76 N4 Ni4 O16, C4 H8 O, C H4 O '

_chemical_formula_sum            'C73 H88 N4 Ni4 O18'
_chemical_formula_weight         1544.31

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

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

_cell_length_a                   11.8537(3)
_cell_length_b                   27.7370(6)
_cell_length_c                   22.5414(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7411.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)

_cell_measurement_reflns_used    9152
_cell_measurement_theta_min      2.93
_cell_measurement_theta_max      24.38
_exptl_crystal_description       BLOCK
_exptl_crystal_colour            black


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_F_000             3240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.071
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.814

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5582
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'


_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker D8 VENTURE diffractometer with PHOTON II detector'
_diffrn_measurement_method       'ω and φ scan'


_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            123783
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.293
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7286
_reflns_number_gt                6215
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'

_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'


_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)+(0.0555P)²+6.2428P] 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_abs_structure_details 
;
 Flack x determined using 2545 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7286
_refine_ls_number_parameters     483
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1086
_refine_ls_wR_factor_gt          0.0974
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.52852(5) 0.30268(2) 0.67898(3) 0.03150(16) Uani 1 1 d . . . . .
Ni2 Ni 0.36419(7) 0.22790(2) 0.73698(3) 0.03961(19) Uani 1 1 d . . . . .
C1 C 0.3278(5) 0.3409(2) 0.7204(2) 0.0424(13) Uani 1 1 d . . . . .
C2 C 0.2134(6) 0.3445(3) 0.7336(3) 0.0626(18) Uani 1 1 d . . . . .
H2 H 0.173759 0.317514 0.749115 0.075 Uiso 1 1 calc R U . . .
C3 C 0.1575(7) 0.3880(4) 0.7238(3) 0.088(3) Uani 1 1 d . . . . .
H3 H 0.079297 0.389867 0.732759 0.106 Uiso 1 1 calc DR U . . .
C4 C 0.2096(9) 0.4276(4) 0.7022(4) 0.090(3) Uani 1 1 d . . . . .
C5 C 0.3216(7) 0.4239(3) 0.6863(3) 0.070(2) Uani 1 1 d . . . . .
H5 H 0.359042 0.450889 0.669475 0.084 Uiso 1 1 calc R U . . .
C6 C 0.3807(6) 0.3808(2) 0.6946(2) 0.0469(14) Uani 1 1 d . . . . .
C7 C 0.5611(6) 0.4053(2) 0.6561(3) 0.0511(16) Uani 1 1 d . . . . .
H7 H 0.532779 0.437363 0.654733 0.061 Uiso 1 1 calc R U . . .
C8 C 0.6736(6) 0.3982(2) 0.6355(3) 0.0544(17) Uani 1 1 d . . . . .
C9 C 0.7350(9) 0.4407(3) 0.6200(4) 0.087(3) Uani 1 1 d . . . . .
H9 H 0.698658 0.471173 0.621742 0.105 Uiso 1 1 calc R U . . .
C10 C 0.8443(11) 0.4381(4) 0.6031(4) 0.106(4) Uani 1 1 d . . . . .
H10 H 0.883519 0.466577 0.591947 0.127 Uiso 1 1 calc R U . . .
C11 C 0.8993(8) 0.3940(4) 0.6019(4) 0.089(3) Uani 1 1 d . . . . .
H11 H 0.976727 0.392473 0.591070 0.106 Uiso 1 1 calc R U . . .
C12 C 0.8426(6) 0.3527(3) 0.6162(3) 0.0621(19) Uani 1 1 d . . . . .
C13 C 0.7261(5) 0.3526(2) 0.6316(2) 0.0468(14) Uani 1 1 d . . . . .
C14 C 1.0073(7) 0.3027(5) 0.6022(5) 0.108(3) Uani 1 1 d . . . . .
H14A H 1.018505 0.312141 0.560692 0.162 Uiso 1 1 calc R U . . .
H14B H 1.031579 0.269198 0.607606 0.162 Uiso 1 1 calc R U . . .
H14C H 1.051821 0.323786 0.627983 0.162 Uiso 1 1 calc R U . . .
C15 C 0.1467(13) 0.4752(4) 0.6955(6) 0.150(6) Uani 1 1 d . . . . .
H15A H 0.191658 0.497347 0.671264 0.226 Uiso 1 1 calc R U . . .
H15B H 0.134100 0.489398 0.734735 0.226 Uiso 1 1 calc R U . . .
H15C H 0.073917 0.469396 0.676144 0.226 Uiso 1 1 calc R U . . .
C16 C 0.2325(7) 0.1806(3) 0.5742(3) 0.066(2) Uani 1 1 d . . . . .
C17 C 0.2184(8) 0.1382(4) 0.5419(3) 0.095(3) Uani 1 1 d . . . . .
H17 H 0.194813 0.139838 0.501648 0.114 Uiso 1 1 calc R U . . .
C18 C 0.2387(11) 0.0933(4) 0.5679(4) 0.113(4) Uani 1 1 d . . . . .
H18 H 0.228691 0.064620 0.545445 0.136 Uiso 1 1 calc R U . . .
C19 C 0.2726(10) 0.0907(3) 0.6250(4) 0.104(4) Uani 1 1 d . . . . .
H19 H 0.286105 0.059981 0.642268 0.124 Uiso 1 1 calc R U . . .
C20 C 0.2885(8) 0.1331(3) 0.6603(3) 0.077(3) Uani 1 1 d . . . . .
C21 C 0.2682(6) 0.1789(3) 0.6349(3) 0.0608(19) Uani 1 1 d . . . . .
C22 C 0.3301(9) 0.1251(3) 0.7190(3) 0.081(3) Uani 1 1 d . . . . .
H22 H 0.335903 0.092546 0.731905 0.097 Uiso 1 1 calc R U . . .
C23 C 0.3963(7) 0.1498(2) 0.8150(3) 0.0600(18) Uani 1 1 d . . . . .
C24 C 0.3799(10) 0.1067(2) 0.8473(3) 0.086(3) Uani 1 1 d . . . . .
H24 H 0.343483 0.080033 0.828993 0.103 Uiso 1 1 calc R U . . .
C25 C 0.4163(9) 0.1029(3) 0.9052(3) 0.083(3) Uani 1 1 d . . . . .
C26 C 0.4625(8) 0.1428(2) 0.9322(3) 0.071(2) Uani 1 1 d . . . . .
H26 H 0.483942 0.140798 0.972728 0.086 Uiso 1 1 calc R U . . .
C27 C 0.4786(7) 0.1856(2) 0.9021(3) 0.0538(16) Uani 1 1 d . . . . .
H27 H 0.510467 0.212566 0.922053 0.065 Uiso 1 1 calc R U . . .
C28 C 0.4485(6) 0.18946(19) 0.8430(2) 0.0458(14) Uani 1 1 d . . . . .
C29 C 0.4048(15) 0.0558(3) 0.9405(4) 0.141(6) Uani 1 1 d . . . . .
H29A H 0.331280 0.041059 0.932154 0.212 Uiso 1 1 calc R U . . .
H29B H 0.410751 0.062667 0.983016 0.212 Uiso 1 1 calc R U . . .
H29C H 0.464964 0.033470 0.928823 0.212 Uiso 1 1 calc R U . . .
C30 C 0.1944(8) 0.2305(4) 0.4907(3) 0.089(3) Uani 1 1 d . . . . .
H30A H 0.256196 0.216999 0.466996 0.134 Uiso 1 1 calc R U . . .
H30B H 0.184751 0.264633 0.480896 0.134 Uiso 1 1 calc R U . . .
H30C H 0.124536 0.213000 0.481916 0.134 Uiso 1 1 calc R U . . .
C31 C 0.1258(7) 0.2148(4) 0.8011(4) 0.094(3) Uani 1 1 d . . . . .
H31A H 0.115716 0.192482 0.767279 0.113 Uiso 1 1 calc R U . . .
H31B H 0.064442 0.239033 0.799489 0.113 Uiso 1 1 calc R U . . .
C32 C 0.1170(12) 0.1863(5) 0.8597(6) 0.152(6) Uani 1 1 d . . . . .
H32A H 0.043198 0.170470 0.861849 0.229 Uiso 1 1 calc R U . . .
H32B H 0.176703 0.161909 0.861070 0.229 Uiso 1 1 calc R U . . .
H32C H 0.125455 0.208436 0.893262 0.229 Uiso 1 1 calc R U . . .
C33 C 0.3981(6) 0.3177(3) 0.5529(3) 0.0601(18) Uani 1 1 d . . . . .
H33A H 0.398676 0.294620 0.519401 0.072 Uiso 1 1 calc R U . . .
H33B H 0.461186 0.340606 0.546845 0.072 Uiso 1 1 calc R U . . .
C34 C 0.2905(8) 0.3448(4) 0.5521(4) 0.088(3) Uani 1 1 d . . . . .
H34A H 0.282742 0.361651 0.514104 0.132 Uiso 1 1 calc R U . . .
H34B H 0.227454 0.322263 0.557070 0.132 Uiso 1 1 calc R U . . .
H34C H 0.289993 0.368271 0.584527 0.132 Uiso 1 1 calc R U . . .
N1 N 0.4943(4) 0.37268(15) 0.6763(2) 0.0410(11) Uani 1 1 d . . . . .
N2 N 0.3605(6) 0.15802(17) 0.7560(2) 0.0582(15) Uani 1 1 d . . . . .
O1 O 0.8899(4) 0.3069(2) 0.6171(2) 0.0740(15) Uani 1 1 d . . . . .
O2 O 0.6761(3) 0.31109(14) 0.64046(15) 0.0412(9) Uani 1 1 d . . . . .
O3 O 0.4158(3) 0.29218(15) 0.60658(16) 0.0454(10) Uani 1 1 d . . . . .
H3A H 0.364896 0.271366 0.610771 0.068 Uiso 1 1 calc R U . . .
O4 O 0.3895(3) 0.30106(13) 0.73291(14) 0.0328(7) Uani 1 1 d . . . . .
O5 O 0.4698(3) 0.22917(12) 0.80934(14) 0.0368(8) Uani 1 1 d . . . . .
O6 O 0.2297(4) 0.23819(18) 0.79576(18) 0.0580(12) Uani 1 1 d . . . . .
H6A H 0.236983 0.258224 0.823437 0.087 Uiso 1 1 calc R U . . .
O7 O 0.2832(4) 0.22069(16) 0.66153(17) 0.0509(11) Uani 1 1 d . . . . .
O8 O 0.2205(4) 0.2257(2) 0.55236(19) 0.0692(14) Uani 1 1 d . . . . .
C36 C 0.390(5) 0.541(2) 0.724(3) 0.36(3) Uani 0.5 1 d D U P A -1
H36A H 0.325229 0.562422 0.732265 0.437 Uiso 0.5 1 calc R U P A -1
H36B H 0.362018 0.511875 0.702889 0.437 Uiso 0.5 1 calc R U P A -1
C37 C 0.481(7) 0.567(3) 0.687(3) 0.37(3) Uani 0.5 1 d D U P A -1
H37A H 0.446012 0.590459 0.658872 0.447 Uiso 0.5 1 calc R U P A -1
H37B H 0.527674 0.544081 0.664242 0.447 Uiso 0.5 1 calc R U P A -1
C39 C 0.532(6) 0.564(3) 0.792(3) 0.36(3) Uani 0.5 1 d D U P A -1
H39A H 0.603641 0.548192 0.803715 0.435 Uiso 0.5 1 calc R U P A -1
H39B H 0.506347 0.584843 0.824333 0.435 Uiso 0.5 1 calc R U P A -1
C38 C 0.551(5) 0.5935(18) 0.736(4) 0.33(3) Uani 0.5 1 d D U P A -1
H38A H 0.631658 0.594368 0.725137 0.401 Uiso 0.5 1 calc R U P A -1
H38B H 0.523516 0.626919 0.741458 0.401 Uiso 0.5 1 calc R U P A -1
O10 O 0.447(5) 0.5275(16) 0.779(3) 0.36(2) Uani 0.5 1 d D U P A -1
C35 C 0.450(3) 0.4736(11) 0.5200(12) 0.169(11) Uani 0.5 1 d D U P . .
H35A H 0.485709 0.444302 0.535463 0.253 Uiso 0.5 1 calc R U P B .
H35B H 0.496787 0.487137 0.488258 0.253 Uiso 0.5 1 calc R U P . .
H35C H 0.375220 0.465683 0.504280 0.253 Uiso 0.5 1 calc R U P . .
O9 O 0.439(3) 0.5092(11) 0.5682(12) 0.232(12) Uani 0.5 1 d D U P B -1
H9A H 0.502739 0.519391 0.577889 0.348 Uiso 0.5 1 calc R U P B -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 1.967(4) . ?
Ni1 N1 1.985(4) . ?
Ni1 O4 2.048(3) . ?
Ni1 O5 2.056(3) 3_656 ?
Ni1 O3 2.130(4) . ?
Ni1 O4 2.211(3) 3_656 ?
Ni2 O7 1.963(4) . ?
Ni2 N2 1.986(5) . ?
Ni2 O4 2.053(4) . ?
Ni2 O5 2.056(4) . ?
Ni2 O6 2.092(4) . ?
Ni2 O5 2.228(4) 3_656 ?
C1 O4 1.355(6) . ?
C1 C2 1.392(9) . ?
C1 C6 1.399(9) . ?
C2 C3 1.394(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.350(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(13) . ?
C4 C15 1.524(11) . ?
C5 C6 1.398(8) . ?
C5 H5 0.9500 . ?
C6 N1 1.426(8) . ?
C7 N1 1.287(7) . ?
C7 C8 1.426(10) . ?
C7 H7 0.9500 . ?
C8 C13 1.410(9) . ?
C8 C9 1.429(9) . ?
C9 C10 1.353(15) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.366(11) . ?
C11 H11 0.9500 . ?
C12 O1 1.389(10) . ?
C12 C13 1.424(9) . ?
C13 O2 1.311(7) . ?
C14 O1 1.436(9) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 O8 1.353(10) . ?
C16 C17 1.393(11) . ?
C16 C21 1.432(9) . ?
C17 C18 1.398(15) . ?
C17 H17 0.9500 . ?
C18 C19 1.351(13) . ?
C18 H18 0.9500 . ?
C19 C20 1.431(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.414(12) . ?
C20 C22 1.431(11) . ?
C21 O7 1.318(8) . ?
C22 N2 1.289(8) . ?
C22 H22 0.9500 . ?
C23 C28 1.411(9) . ?
C23 N2 1.414(9) . ?
C23 C24 1.414(9) . ?
C24 C25 1.378(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.376(11) . ?
C25 C29 1.537(10) . ?
C26 C27 1.382(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.384(8) . ?
C27 H27 0.9500 . ?
C28 O5 1.361(6) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 O8 1.430(8) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 O6 1.397(9) . ?
C31 C32 1.542(14) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 O3 1.419(7) . ?
C33 C34 1.479(11) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O3 H3A 0.8400 . ?
O6 H6A 0.8400 . ?
C36 O10 1.46(3) . ?
C36 C37 1.55(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.56(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C39 O10 1.45(2) . ?
C39 C38 1.52(2) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C35 O9 1.47(2) . ?
C35 C35 1.72(6) 4_566 ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
O9 H9A 0.8400 . ?

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
O2 Ni1 N1 93.00(18) . . ?
O2 Ni1 O4 168.56(14) . . ?
N1 Ni1 O4 82.84(17) . . ?
O2 Ni1 O5 99.52(16) . 3_656 ?
N1 Ni1 O5 167.49(17) . 3_656 ?
O4 Ni1 O5 84.84(14) . 3_656 ?
O2 Ni1 O3 103.67(15) . . ?
N1 Ni1 O3 88.98(18) . . ?
O4 Ni1 O3 86.96(14) . . ?
O5 Ni1 O3 88.20(15) 3_656 . ?
O2 Ni1 O4 90.47(14) . 3_656 ?
N1 Ni1 O4 97.88(17) . 3_656 ?
O4 Ni1 O4 79.62(14) . 3_656 ?
O5 Ni1 O4 81.98(13) 3_656 3_656 ?
O3 Ni1 O4 163.99(14) . 3_656 ?
O7 Ni2 N2 94.4(2) . . ?
O7 Ni2 O4 97.67(16) . . ?
N2 Ni2 O4 167.8(2) . . ?
O7 Ni2 O5 170.58(17) . . ?
N2 Ni2 O5 81.9(2) . . ?
O4 Ni2 O5 85.96(13) . . ?
O7 Ni2 O6 100.96(18) . . ?
N2 Ni2 O6 88.8(2) . . ?
O4 Ni2 O6 90.29(17) . . ?
O5 Ni2 O6 87.67(16) . . ?
O7 Ni2 O5 91.56(15) . 3_656 ?
N2 Ni2 O5 97.8(2) . 3_656 ?
O4 Ni2 O5 80.46(13) . 3_656 ?
O5 Ni2 O5 80.43(13) . 3_656 ?
O6 Ni2 O5 165.36(15) . 3_656 ?
O4 C1 C2 122.7(6) . . ?
O4 C1 C6 119.3(5) . . ?
C2 C1 C6 118.0(6) . . ?
C1 C2 C3 119.4(7) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 122.9(7) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 118.3(7) . . ?
C3 C4 C15 121.1(10) . . ?
C5 C4 C15 120.6(11) . . ?
C4 C5 C6 120.7(8) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 120.5(7) . . ?
C5 C6 N1 124.7(6) . . ?
C1 C6 N1 114.8(5) . . ?
N1 C7 C8 126.4(6) . . ?
N1 C7 H7 116.8 . . ?
C8 C7 H7 116.8 . . ?
C13 C8 C7 123.9(5) . . ?
C13 C8 C9 119.9(7) . . ?
C7 C8 C9 116.1(7) . . ?
C10 C9 C8 120.9(9) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 120.2(8) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C12 C11 C10 120.2(8) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 O1 124.8(7) . . ?
C11 C12 C13 122.5(8) . . ?
O1 C12 C13 112.7(6) . . ?
O2 C13 C8 125.3(6) . . ?
O2 C13 C12 118.5(6) . . ?
C8 C13 C12 116.2(6) . . ?
O1 C14 H14A 109.5 . . ?
O1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 C15 H15A 109.5 . . ?
C4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O8 C16 C17 125.3(7) . . ?
O8 C16 C21 114.1(6) . . ?
C17 C16 C21 120.5(9) . . ?
C16 C17 C18 120.8(8) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C19 C18 C17 119.9(8) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 121.6(9) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C21 C20 C22 125.0(6) . . ?
C21 C20 C19 119.4(7) . . ?
C22 C20 C19 115.6(8) . . ?
O7 C21 C20 125.7(6) . . ?
O7 C21 C16 116.5(7) . . ?
C20 C21 C16 117.8(6) . . ?
N2 C22 C20 125.8(7) . . ?
N2 C22 H22 117.1 . . ?
C20 C22 H22 117.1 . . ?
C28 C23 N2 115.2(5) . . ?
C28 C23 C24 119.3(6) . . ?
N2 C23 C24 125.4(6) . . ?
C25 C24 C23 120.6(7) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C24 118.9(6) . . ?
C26 C25 C29 119.4(8) . . ?
C24 C25 C29 121.8(8) . . ?
C25 C26 C27 121.9(7) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 H26 119.0 . . ?
C26 C27 C28 120.2(6) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
O5 C28 C27 123.4(5) . . ?
O5 C28 C23 117.6(5) . . ?
C27 C28 C23 118.9(5) . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O8 C30 H30A 109.5 . . ?
O8 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O8 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O6 C31 C32 111.8(8) . . ?
O6 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
O6 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O3 C33 C34 113.0(6) . . ?
O3 C33 H33A 109.0 . . ?
C34 C33 H33A 109.0 . . ?
O3 C33 H33B 109.0 . . ?
C34 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C7 N1 C6 125.0(5) . . ?
C7 N1 Ni1 125.0(4) . . ?
C6 N1 Ni1 109.7(4) . . ?
C22 N2 C23 125.3(6) . . ?
C22 N2 Ni2 124.0(5) . . ?
C23 N2 Ni2 110.7(4) . . ?
C12 O1 C14 117.6(7) . . ?
C13 O2 Ni1 125.0(4) . . ?
C33 O3 Ni1 132.7(4) . . ?
C33 O3 H3A 109.5 . . ?
Ni1 O3 H3A 117.3 . . ?
C1 O4 Ni1 107.0(3) . . ?
C1 O4 Ni2 137.4(3) . . ?
Ni1 O4 Ni2 99.56(15) . . ?
C1 O4 Ni1 114.1(3) . 3_656 ?
Ni1 O4 Ni1 100.33(14) . 3_656 ?
Ni2 O4 Ni1 92.54(13) . 3_656 ?
C28 O5 Ni1 137.2(3) . 3_656 ?
C28 O5 Ni2 108.4(4) . . ?
Ni1 O5 Ni2 97.15(14) 3_656 . ?
C28 O5 Ni2 114.4(3) . 3_656 ?
Ni1 O5 Ni2 93.84(14) 3_656 3_656 ?
Ni2 O5 Ni2 99.54(13) . 3_656 ?
C31 O6 Ni2 131.6(5) . . ?
C31 O6 H6A 109.5 . . ?
Ni2 O6 H6A 118.8 . . ?
C21 O7 Ni2 123.4(5) . . ?
C16 O8 C30 117.5(6) . . ?
O10 C36 C37 105(2) . . ?
O10 C36 H36A 110.8 . . ?
C37 C36 H36A 110.8 . . ?
O10 C36 H36B 110.8 . . ?
C37 C36 H36B 110.8 . . ?
H36A C36 H36B 108.9 . . ?
C36 C37 C38 102(2) . . ?
C36 C37 H37A 111.4 . . ?
C38 C37 H37A 111.4 . . ?
C36 C37 H37B 111.4 . . ?
C38 C37 H37B 111.4 . . ?
H37A C37 H37B 109.2 . . ?
O10 C39 C38 108.1(15) . . ?
O10 C39 H39A 110.1 . . ?
C38 C39 H39A 110.1 . . ?
O10 C39 H39B 110.1 . . ?
C38 C39 H39B 110.1 . . ?
H39A C39 H39B 108.4 . . ?
C39 C38 C37 104.8(16) . . ?
C39 C38 H38A 110.8 . . ?
C37 C38 H38A 110.8 . . ?
C39 C38 H38B 110.8 . . ?
C37 C38 H38B 110.8 . . ?
H38A C38 H38B 108.9 . . ?
C39 O10 C36 108.5(19) . . ?
O9 C35 C35 79(2) . 4_566 ?
O9 C35 H35A 109.5 . . ?
C35 C35 H35A 153.2 4_566 . ?
O9 C35 H35B 109.5 . . ?
C35 C35 H35B 44.8 4_566 . ?
H35A C35 H35B 109.5 . . ?
O9 C35 H35C 109.5 . . ?
C35 C35 H35C 90.1 4_566 . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C35 O9 H9A 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
O4 C1 C2 C3 174.8(6) . . . . ?
C6 C1 C2 C3 -3.5(9) . . . . ?
C1 C2 C3 C4 -0.5(12) . . . . ?
C2 C3 C4 C5 3.5(14) . . . . ?
C2 C3 C4 C15 -176.6(9) . . . . ?
C3 C4 C5 C6 -2.6(12) . . . . ?
C15 C4 C5 C6 177.5(9) . . . . ?
C4 C5 C6 C1 -1.3(10) . . . . ?
C4 C5 C6 N1 176.1(7) . . . . ?
O4 C1 C6 C5 -174.0(5) . . . . ?
C2 C1 C6 C5 4.3(9) . . . . ?
O4 C1 C6 N1 8.3(7) . . . . ?
C2 C1 C6 N1 -173.3(5) . . . . ?
N1 C7 C8 C13 3.4(10) . . . . ?
N1 C7 C8 C9 -174.5(7) . . . . ?
C13 C8 C9 C10 -1.6(12) . . . . ?
C7 C8 C9 C10 176.4(8) . . . . ?
C8 C9 C10 C11 -1.7(15) . . . . ?
C9 C10 C11 C12 1.9(15) . . . . ?
C10 C11 C12 O1 -179.1(8) . . . . ?
C10 C11 C12 C13 1.2(13) . . . . ?
C7 C8 C13 O2 7.2(10) . . . . ?
C9 C8 C13 O2 -174.9(6) . . . . ?
C7 C8 C13 C12 -173.4(6) . . . . ?
C9 C8 C13 C12 4.5(9) . . . . ?
C11 C12 C13 O2 175.1(6) . . . . ?
O1 C12 C13 O2 -4.6(8) . . . . ?
C11 C12 C13 C8 -4.4(9) . . . . ?
O1 C12 C13 C8 176.0(5) . . . . ?
O8 C16 C17 C18 176.5(9) . . . . ?
C21 C16 C17 C18 0.1(14) . . . . ?
C16 C17 C18 C19 -0.1(17) . . . . ?
C17 C18 C19 C20 0.0(19) . . . . ?
C18 C19 C20 C21 0.1(16) . . . . ?
C18 C19 C20 C22 -176.9(11) . . . . ?
C22 C20 C21 O7 -0.9(14) . . . . ?
C19 C20 C21 O7 -177.5(8) . . . . ?
C22 C20 C21 C16 176.5(8) . . . . ?
C19 C20 C21 C16 -0.1(12) . . . . ?
O8 C16 C21 O7 0.9(10) . . . . ?
C17 C16 C21 O7 177.7(7) . . . . ?
O8 C16 C21 C20 -176.8(7) . . . . ?
C17 C16 C21 C20 0.0(11) . . . . ?
C21 C20 C22 N2 -3.8(16) . . . . ?
C19 C20 C22 N2 173.0(9) . . . . ?
C28 C23 C24 C25 -1.2(14) . . . . ?
N2 C23 C24 C25 -178.7(9) . . . . ?
C23 C24 C25 C26 4.0(15) . . . . ?
C23 C24 C25 C29 -177.0(10) . . . . ?
C24 C25 C26 C27 -3.3(15) . . . . ?
C29 C25 C26 C27 177.7(10) . . . . ?
C25 C26 C27 C28 -0.2(13) . . . . ?
C26 C27 C28 O5 -174.7(7) . . . . ?
C26 C27 C28 C23 3.1(11) . . . . ?
N2 C23 C28 O5 -6.7(9) . . . . ?
C24 C23 C28 O5 175.6(7) . . . . ?
N2 C23 C28 C27 175.4(6) . . . . ?
C24 C23 C28 C27 -2.3(11) . . . . ?
C8 C7 N1 C6 -177.6(6) . . . . ?
C8 C7 N1 Ni1 -4.2(9) . . . . ?
C5 C6 N1 C7 8.3(9) . . . . ?
C1 C6 N1 C7 -174.1(5) . . . . ?
C5 C6 N1 Ni1 -165.9(5) . . . . ?
C1 C6 N1 Ni1 11.6(6) . . . . ?
C20 C22 N2 C23 176.7(8) . . . . ?
C20 C22 N2 Ni2 -3.8(14) . . . . ?
C28 C23 N2 C22 166.7(8) . . . . ?
C24 C23 N2 C22 -15.7(14) . . . . ?
C28 C23 N2 Ni2 -12.9(8) . . . . ?
C24 C23 N2 Ni2 164.7(7) . . . . ?
C11 C12 O1 C14 0.2(11) . . . . ?
C13 C12 O1 C14 179.9(7) . . . . ?
C8 C13 O2 Ni1 -15.2(8) . . . . ?
C12 C13 O2 Ni1 165.5(4) . . . . ?
C34 C33 O3 Ni1 -108.6(7) . . . . ?
C2 C1 O4 Ni1 158.9(5) . . . . ?
C6 C1 O4 Ni1 -22.8(6) . . . . ?
C2 C1 O4 Ni2 32.8(8) . . . . ?
C6 C1 O4 Ni2 -149.0(4) . . . . ?
C2 C1 O4 Ni1 -91.1(6) . . . 3_656 ?
C6 C1 O4 Ni1 87.2(5) . . . 3_656 ?
C27 C28 O5 Ni1 -37.0(9) . . . 3_656 ?
C23 C28 O5 Ni1 145.2(5) . . . 3_656 ?
C27 C28 O5 Ni2 -160.4(5) . . . . ?
C23 C28 O5 Ni2 21.8(7) . . . . ?
C27 C28 O5 Ni2 89.6(6) . . . 3_656 ?
C23 C28 O5 Ni2 -88.2(6) . . . 3_656 ?
C32 C31 O6 Ni2 113.5(9) . . . . ?
C20 C21 O7 Ni2 12.1(10) . . . . ?
C16 C21 O7 Ni2 -165.3(5) . . . . ?
C17 C16 O8 C30 -1.9(11) . . . . ?
C21 C16 O8 C30 174.8(7) . . . . ?
O10 C36 C37 C38 -34(6) . . . . ?
O10 C39 C38 C37 -7(8) . . . . ?
C36 C37 C38 C39 25(7) . . . . ?
C38 C39 O10 C36 -15(8) . . . . ?
C37 C36 O10 C39 32(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
_geom_hbond_publ_flag
C2 H2 O6 0.95 2.53 3.270(9) 135.1 . yes
C27 H27 O3 0.95 2.46 3.215(8) 136.2 3_656 yes
C30 H30A O1 0.98 2.56 3.514(10) 164.9 8_456 yes
O3 H3A O7 0.84 2.05 2.816(6) 150.6 . yes
O3 H3A O8 0.84 2.50 3.201(6) 141.2 . yes
O6 H6A O1 0.84 2.43 3.083(7) 135.6 3_656 yes
O6 H6A O2 0.84 1.97 2.721(6) 148.6 3_656 yes
C35 H35B O9^a 0.98 1.45 2.05(4) 113.5 4_566 yes

_refine_diff_density_max         0.403
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.064



# start Validation Reply Form
_vrf_PLAT260_shelx               
;
PROBLEM: Large Average Ueq of Residue Including       O10      0.358 Check 
RESPONSE: The atom belongs to the solvent molecule which is disordered
around 2 fold axis of rotation. Hence large value of Ueq is expected.
;
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Bond Without Acceptor  O9       --H9A      .     Please Check 
RESPONSE:  Methanol solvent is found to be disordered around 2 fold axis
of rotation. Hence the refined position of H may not be in a geometry to
show H-bond interaction

;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE:  These reflections are affected by the beamstop and hence omitted 
from refinement

;
# end Validation Reply Form

