# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1907763'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-04-03 deposited with the CCDC.	2019-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H38 N8 Ni2 O13'
_chemical_formula_weight         764.00

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   5.1874(4)
_cell_length_b                   34.715(3)
_cell_length_c                   18.1886(15)
_cell_angle_alpha                90
_cell_angle_beta                 90.275(2)
_cell_angle_gamma                90
_cell_volume                     3275.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    292(2)
_cell_measurement_reflns_used    104175
_cell_measurement_theta_min      2.086
_cell_measurement_theta_max      28.369

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_F_000             1592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .33
_exptl_crystal_size_min          .10
_exptl_absorpt_coefficient_mu    1.224
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  .662
_exptl_absorpt_correction_T_max  .885
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      292(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            104175
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.086
_diffrn_reflns_theta_max         28.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8159
_reflns_number_gt                5916
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0859P)²+7.5016P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8159
_refine_ls_number_parameters     404
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0806
_refine_ls_wR_factor_ref         0.2110
_refine_ls_wR_factor_gt          0.1946
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.144
_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 0.79255(11) 0.79472(2) 0.85695(3) 0.03319(17) Uani 1 1 d . . . . .
Ni2 Ni 0.31907(12) 0.51878(2) 0.73182(4) 0.0449(2) Uani 1 1 d . . . . .
O1A O 1.0285(6) 0.75605(9) 0.84722(17) 0.0384(7) Uani 1 1 d . . . . .
O2A O 1.3889(8) 0.70558(11) 0.8626(2) 0.0544(10) Uani 1 1 d . . . . .
O1B O 0.5560(7) 0.55028(11) 0.7762(2) 0.0505(9) Uani 1 1 d . . . . .
N1A N 0.7999(8) 0.81062(11) 0.7602(2) 0.0377(9) Uani 1 1 d . . . . .
N2A N 0.5808(7) 0.83795(11) 0.8744(2) 0.0375(9) Uani 1 1 d . . . . .
H2A H 0.694933 0.859786 0.884838 0.045 Uiso 1 1 calc R U . . .
N1B N 0.3116(8) 0.54398(12) 0.6435(2) 0.0446(10) Uani 1 1 d . . . . .
N3A N 0.7187(8) 0.77972(12) 0.9561(2) 0.0426(9) Uani 1 1 d . . . . .
H3AA H 0.614094 0.759398 0.955988 0.051 Uiso 1 1 calc R U . . .
H3AB H 0.864104 0.773134 0.979025 0.051 Uiso 1 1 calc R U . . .
O4 O 0.5079(10) 0.58354(17) 0.3529(3) 0.0869(15) Uani 1 1 d . . . . .
N2B N 0.1002(9) 0.48206(13) 0.6871(3) 0.0549(12) Uani 1 1 d . . . . .
H2B H 0.210399 0.462730 0.663685 0.066 Uiso 1 1 calc R U . . .
N4 N 0.5120(10) 0.58277(14) 0.4194(3) 0.0560(12) Uani 1 1 d . . . . .
O2B O 0.9190(9) 0.58149(15) 0.8526(2) 0.0715(13) Uani 1 1 d . . . . .
O6 O 0.3792(11) 0.60500(15) 0.4548(3) 0.0921(18) Uani 1 1 d . . . . .
C1A C 1.1560(9) 0.74776(13) 0.7874(3) 0.0354(10) Uani 1 1 d . . . . .
C7A C 0.9276(10) 0.79501(15) 0.7084(3) 0.0452(12) Uani 1 1 d . . . . .
H7A H 0.898036 0.803946 0.660918 0.054 Uiso 1 1 calc R U . . .
C6B C 0.6363(10) 0.59168(14) 0.6725(3) 0.0436(11) Uani 1 1 d . . . . .
C6A C 1.1136(10) 0.76470(14) 0.7177(3) 0.0400(11) Uani 1 1 d . . . . .
C1B C 0.6823(9) 0.57816(15) 0.7437(3) 0.0428(11) Uani 1 1 d . . . . .
C3A C 1.5005(10) 0.71012(15) 0.7329(3) 0.0484(13) Uani 1 1 d . . . . .
H3A H 1.631988 0.692055 0.737642 0.058 Uiso 1 1 calc R U . . .
C2A C 1.3572(9) 0.71975(14) 0.7931(3) 0.0405(11) Uani 1 1 d . . . . .
C7B C 0.4438(10) 0.57439(16) 0.6268(3) 0.0479(12) Uani 1 1 d . . . . .
H7B H 0.410675 0.585875 0.581576 0.057 Uiso 1 1 calc R U . . .
N3B N 0.2646(11) 0.49127(17) 0.8209(3) 0.0696(15) Uani 1 1 d . . . . .
H3BA H 0.415513 0.486367 0.842408 0.084 Uiso 1 1 calc R U . . .
H3BB H 0.171291 0.505553 0.851494 0.084 Uiso 1 1 calc R U . . .
C4A C 1.4529(12) 0.72686(17) 0.6649(3) 0.0543(14) Uani 1 1 d . . . . .
H4A H 1.551188 0.719887 0.624399 0.065 Uiso 1 1 calc R U . . .
C5A C 1.2632(11) 0.75336(17) 0.6577(3) 0.0481(13) Uani 1 1 d . . . . .
H5A H 1.231490 0.764270 0.611834 0.058 Uiso 1 1 calc R U . . .
C2B C 0.8885(10) 0.59604(16) 0.7843(3) 0.0487(13) Uani 1 1 d . . . . .
C11A C 0.5954(11) 0.81205(16) 0.9951(3) 0.0493(13) Uani 1 1 d . . . . .
H11A H 0.724729 0.829892 1.013300 0.059 Uiso 1 1 calc R U . . .
H11B H 0.496095 0.802637 1.036409 0.059 Uiso 1 1 calc R U . . .
C8A C 0.6363(11) 0.84453(16) 0.7446(3) 0.0518(13) Uani 1 1 d . . . . .
H8AA H 0.549957 0.841582 0.697475 0.062 Uiso 1 1 calc R U . . .
H8AB H 0.740127 0.867754 0.743196 0.062 Uiso 1 1 calc R U . . .
C10A C 0.4236(10) 0.83143(17) 0.9406(3) 0.0509(13) Uani 1 1 d . . . . .
H10A H 0.276536 0.815235 0.929053 0.061 Uiso 1 1 calc R U . . .
H10B H 0.361431 0.855726 0.959977 0.061 Uiso 1 1 calc R U . . .
C5B C 0.7846(11) 0.62163(16) 0.6430(4) 0.0551(14) Uani 1 1 d . . . . .
H5B H 0.749408 0.630452 0.595697 0.066 Uiso 1 1 calc R U . . .
C9A C 0.4410(10) 0.84686(16) 0.8058(3) 0.0503(13) Uani 1 1 d . . . . .
H9AA H 0.366902 0.872483 0.808199 0.060 Uiso 1 1 calc R U . . .
H9AB H 0.303236 0.828432 0.797767 0.060 Uiso 1 1 calc R U . . .
C3B C 1.0287(11) 0.62505(16) 0.7529(4) 0.0573(15) Uani 1 1 d . . . . .
H3B H 1.161252 0.636355 0.779887 0.069 Uiso 1 1 calc R U . . .
C12A C 1.5987(11) 0.67972(16) 0.8751(4) 0.0554(14) Uani 1 1 d . . . . .
H12A H 1.573797 0.656817 0.846321 0.083 Uiso 1 1 calc R U . . .
H12B H 1.606166 0.673050 0.926262 0.083 Uiso 1 1 calc R U . . .
H12C H 1.757125 0.691908 0.861049 0.083 Uiso 1 1 calc R U . . .
O5 O 0.6520(14) 0.5603(2) 0.4521(4) 0.131(3) Uani 1 1 d . . . . .
C8B C 0.1383(11) 0.52659(17) 0.5884(3) 0.0571(15) Uani 1 1 d . . . . .
H8BA H 0.236734 0.511515 0.553480 0.069 Uiso 1 1 calc R U . . .
H8BB H 0.046287 0.546540 0.561715 0.069 Uiso 1 1 calc R U . . .
C9B C -0.0468(11) 0.50144(18) 0.6282(4) 0.0580(15) Uani 1 1 d . . . . .
H9BA H -0.185068 0.516734 0.648937 0.070 Uiso 1 1 calc R U . . .
H9BB H -0.121278 0.482595 0.594936 0.070 Uiso 1 1 calc R U . . .
C4B C 0.9804(12) 0.63806(17) 0.6827(4) 0.0610(16) Uani 1 1 d . . . . .
H4B H 1.079300 0.657721 0.662579 0.073 Uiso 1 1 calc R U . . .
C10B C -0.0514(13) 0.4622(2) 0.7440(4) 0.073(2) Uani 1 1 d . . . . .
H10C H -0.121190 0.438218 0.725016 0.088 Uiso 1 1 calc R U . . .
H10D H -0.193017 0.478274 0.760193 0.088 Uiso 1 1 calc R U . . .
C12B C 1.1155(15) 0.5981(3) 0.8993(4) 0.087(2) Uani 1 1 d . . . . .
H12D H 1.280385 0.595609 0.876073 0.130 Uiso 1 1 calc R U . . .
H12E H 1.118392 0.584819 0.945638 0.130 Uiso 1 1 calc R U . . .
H12F H 1.078272 0.624838 0.907323 0.130 Uiso 1 1 calc R U . . .
C11B C 0.1282(16) 0.4546(2) 0.8055(5) 0.090(2) Uani 1 1 d . . . . .
H11C H 0.250383 0.434633 0.792119 0.107 Uiso 1 1 calc R U . . .
H11D H 0.034214 0.446111 0.848584 0.107 Uiso 1 1 calc R U . . .
N2 N 0.453(3) 0.3874(5) 0.9243(11) 0.252(8) Uiso 1 1 d D U . . .
O3 O 0.355(5) 0.3674(7) 0.8773(14) 0.458(16) Uiso 1 1 d D U . . .
O1 O 0.602(3) 0.4123(4) 0.9019(8) 0.247(6) Uiso 1 1 d D U . . .
O2 O 0.382(6) 0.3855(9) 0.9864(13) 0.60(2) Uiso 1 1 d D U . . .
O7 O 0.1915(9) 0.73941(14) 0.9972(2) 0.0681(12) Uani 1 1 d G . . . .
H7C H 0.157697 0.736564 0.951729 0.102 Uiso 1 1 d G U . . .
H7D H 0.177590 0.716911 1.015174 0.102 Uiso 1 1 d G U . . .
O8 O 0.700(4) 0.5165(6) 0.9266(12) 0.378(11) Uiso 1 1 d . . . . .
O9 O -0.0688(19) 0.33326(19) 0.9490(4) 0.142(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
Ni1 O1A 1.826(3) . ?
Ni1 N1A 1.844(4) . ?
Ni1 N2A 1.887(4) . ?
Ni1 N3A 1.917(4) . ?
Ni2 N1B 1.830(5) . ?
Ni2 O1B 1.830(4) . ?
Ni2 N2B 1.889(4) . ?
Ni2 N3B 1.903(5) . ?
O1A C1A 1.308(5) . ?
O2A C2A 1.365(6) . ?
O2A C12A 1.428(6) . ?
O1B C1B 1.311(6) . ?
N1A C7A 1.275(7) . ?
N1A C8A 1.478(6) . ?
N2A C9A 1.472(7) . ?
N2A C10A 1.475(7) . ?
N2A H2A 0.9800 . ?
N1B C7B 1.295(7) . ?
N1B C8B 1.472(7) . ?
N3A C11A 1.475(7) . ?
N3A H3AA 0.8900 . ?
N3A H3AB 0.8900 . ?
O4 N4 1.210(7) . ?
N2B C9B 1.474(8) . ?
N2B C10B 1.475(9) . ?
N2B H2B 0.9800 . ?
N4 O5 1.219(7) . ?
N4 O6 1.220(7) . ?
O2B C2B 1.350(7) . ?
O2B C12B 1.444(7) . ?
C1A C6A 1.414(7) . ?
C1A C2A 1.430(7) . ?
C7A C6A 1.437(7) . ?
C7A H7A 0.9300 . ?
C6B C1B 1.396(8) . ?
C6B C5B 1.402(8) . ?
C6B C7B 1.429(8) . ?
C6A C5A 1.399(7) . ?
C1B C2B 1.438(7) . ?
C3A C2A 1.368(7) . ?
C3A C4A 1.388(8) . ?
C3A H3A 0.9300 . ?
C7B H7B 0.9300 . ?
N3B C11B 1.484(9) . ?
N3B H3BA 0.8900 . ?
N3B H3BB 0.8900 . ?
C4A C5A 1.353(8) . ?
C4A H4A 0.9300 . ?
C5A H5A 0.9300 . ?
C2B C3B 1.369(8) . ?
C11A C10A 1.490(8) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C8A C9A 1.512(8) . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C10A H10A 0.9700 . ?
C10A H10B 0.9700 . ?
C5B C4B 1.368(9) . ?
C5B H5B 0.9300 . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C3B C4B 1.376(9) . ?
C3B H3B 0.9300 . ?
C12A H12A 0.9600 . ?
C12A H12B 0.9600 . ?
C12A H12C 0.9600 . ?
C8B C9B 1.488(9) . ?
C8B H8BA 0.9700 . ?
C8B H8BB 0.9700 . ?
C9B H9BA 0.9700 . ?
C9B H9BB 0.9700 . ?
C4B H4B 0.9300 . ?
C10B C11B 1.476(10) . ?
C10B H10C 0.9700 . ?
C10B H10D 0.9700 . ?
C12B H12D 0.9600 . ?
C12B H12E 0.9600 . ?
C12B H12F 0.9600 . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
N2 O2 1.190(13) . ?
N2 O3 1.212(13) . ?
N2 O1 1.231(12) . ?
O7 H7C 0.8503 . ?
O7 H7D 0.8499 . ?

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
O1A Ni1 N1A 96.35(16) . . ?
O1A Ni1 N2A 172.67(17) . . ?
N1A Ni1 N2A 86.40(17) . . ?
O1A Ni1 N3A 91.63(16) . . ?
N1A Ni1 N3A 169.58(18) . . ?
N2A Ni1 N3A 86.50(18) . . ?
N1B Ni2 O1B 96.48(18) . . ?
N1B Ni2 N2B 86.2(2) . . ?
O1B Ni2 N2B 173.98(19) . . ?
N1B Ni2 N3B 170.1(2) . . ?
O1B Ni2 N3B 91.5(2) . . ?
N2B Ni2 N3B 86.4(2) . . ?
C1A O1A Ni1 125.8(3) . . ?
C2A O2A C12A 117.5(4) . . ?
C1B O1B Ni2 125.4(3) . . ?
C7A N1A C8A 119.7(4) . . ?
C7A N1A Ni1 126.2(4) . . ?
C8A N1A Ni1 114.1(3) . . ?
C9A N2A C10A 116.9(4) . . ?
C9A N2A Ni1 108.0(3) . . ?
C10A N2A Ni1 109.9(3) . . ?
C9A N2A H2A 107.2 . . ?
C10A N2A H2A 107.2 . . ?
Ni1 N2A H2A 107.2 . . ?
C7B N1B C8B 119.8(5) . . ?
C7B N1B Ni2 125.9(4) . . ?
C8B N1B Ni2 114.3(4) . . ?
C11A N3A Ni1 109.5(3) . . ?
C11A N3A H3AA 109.8 . . ?
Ni1 N3A H3AA 109.8 . . ?
C11A N3A H3AB 109.8 . . ?
Ni1 N3A H3AB 109.8 . . ?
H3AA N3A H3AB 108.2 . . ?
C9B N2B C10B 116.6(5) . . ?
C9B N2B Ni2 108.2(4) . . ?
C10B N2B Ni2 109.5(4) . . ?
C9B N2B H2B 107.4 . . ?
C10B N2B H2B 107.4 . . ?
Ni2 N2B H2B 107.4 . . ?
O4 N4 O5 120.6(6) . . ?
O4 N4 O6 120.4(6) . . ?
O5 N4 O6 118.9(6) . . ?
C2B O2B C12B 118.1(5) . . ?
O1A C1A C6A 125.2(4) . . ?
O1A C1A C2A 117.5(4) . . ?
C6A C1A C2A 117.3(4) . . ?
N1A C7A C6A 125.1(5) . . ?
N1A C7A H7A 117.4 . . ?
C6A C7A H7A 117.4 . . ?
C1B C6B C5B 120.9(5) . . ?
C1B C6B C7B 120.9(5) . . ?
C5B C6B C7B 118.1(5) . . ?
C5A C6A C1A 119.9(5) . . ?
C5A C6A C7A 119.3(5) . . ?
C1A C6A C7A 120.8(4) . . ?
O1B C1B C6B 125.6(5) . . ?
O1B C1B C2B 117.4(5) . . ?
C6B C1B C2B 117.0(5) . . ?
C2A C3A C4A 121.0(5) . . ?
C2A C3A H3A 119.5 . . ?
C4A C3A H3A 119.5 . . ?
O2A C2A C3A 126.1(5) . . ?
O2A C2A C1A 113.4(4) . . ?
C3A C2A C1A 120.5(5) . . ?
N1B C7B C6B 125.2(5) . . ?
N1B C7B H7B 117.4 . . ?
C6B C7B H7B 117.4 . . ?
C11B N3B Ni2 110.1(5) . . ?
C11B N3B H3BA 109.6 . . ?
Ni2 N3B H3BA 109.6 . . ?
C11B N3B H3BB 109.6 . . ?
Ni2 N3B H3BB 109.6 . . ?
H3BA N3B H3BB 108.2 . . ?
C5A C4A C3A 119.8(5) . . ?
C5A C4A H4A 120.1 . . ?
C3A C4A H4A 120.1 . . ?
C4A C5A C6A 121.4(5) . . ?
C4A C5A H5A 119.3 . . ?
C6A C5A H5A 119.3 . . ?
O2B C2B C3B 126.8(5) . . ?
O2B C2B C1B 113.3(5) . . ?
C3B C2B C1B 119.9(6) . . ?
N3A C11A C10A 106.4(4) . . ?
N3A C11A H11A 110.4 . . ?
C10A C11A H11A 110.4 . . ?
N3A C11A H11B 110.4 . . ?
C10A C11A H11B 110.4 . . ?
H11A C11A H11B 108.6 . . ?
N1A C8A C9A 106.7(4) . . ?
N1A C8A H8AA 110.4 . . ?
C9A C8A H8AA 110.4 . . ?
N1A C8A H8AB 110.4 . . ?
C9A C8A H8AB 110.4 . . ?
H8AA C8A H8AB 108.6 . . ?
N2A C10A C11A 106.3(4) . . ?
N2A C10A H10A 110.5 . . ?
C11A C10A H10A 110.5 . . ?
N2A C10A H10B 110.5 . . ?
C11A C10A H10B 110.5 . . ?
H10A C10A H10B 108.7 . . ?
C4B C5B C6B 120.9(6) . . ?
C4B C5B H5B 119.5 . . ?
C6B C5B H5B 119.5 . . ?
N2A C9A C8A 106.5(4) . . ?
N2A C9A H9AA 110.4 . . ?
C8A C9A H9AA 110.4 . . ?
N2A C9A H9AB 110.4 . . ?
C8A C9A H9AB 110.4 . . ?
H9AA C9A H9AB 108.6 . . ?
C2B C3B C4B 122.3(6) . . ?
C2B C3B H3B 118.9 . . ?
C4B C3B H3B 118.9 . . ?
O2A C12A H12A 109.5 . . ?
O2A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
O2A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
N1B C8B C9B 107.6(5) . . ?
N1B C8B H8BA 110.2 . . ?
C9B C8B H8BA 110.2 . . ?
N1B C8B H8BB 110.2 . . ?
C9B C8B H8BB 110.2 . . ?
H8BA C8B H8BB 108.5 . . ?
N2B C9B C8B 106.8(4) . . ?
N2B C9B H9BA 110.4 . . ?
C8B C9B H9BA 110.4 . . ?
N2B C9B H9BB 110.4 . . ?
C8B C9B H9BB 110.4 . . ?
H9BA C9B H9BB 108.6 . . ?
C5B C4B C3B 119.0(6) . . ?
C5B C4B H4B 120.5 . . ?
C3B C4B H4B 120.5 . . ?
N2B C10B C11B 106.2(5) . . ?
N2B C10B H10C 110.5 . . ?
C11B C10B H10C 110.5 . . ?
N2B C10B H10D 110.5 . . ?
C11B C10B H10D 110.5 . . ?
H10C C10B H10D 108.7 . . ?
O2B C12B H12D 109.5 . . ?
O2B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
O2B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C10B C11B N3B 106.7(6) . . ?
C10B C11B H11C 110.4 . . ?
N3B C11B H11C 110.4 . . ?
C10B C11B H11D 110.4 . . ?
N3B C11B H11D 110.4 . . ?
H11C C11B H11D 108.6 . . ?
O2 N2 O3 120(2) . . ?
O2 N2 O1 123(2) . . ?
O3 N2 O1 115.6(19) . . ?
H7C O7 H7D 104.5 . . ?

_refine_diff_density_max         1.280
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.105

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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1907766'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-04-03 deposited with the CCDC.	2019-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H64 N8 Ni6 O25'
_chemical_formula_weight         1601.41

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

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

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

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

_cell_length_a                   20.212(11)
_cell_length_b                   22.656(11)
_cell_length_c                   16.048(8)
_cell_angle_alpha                90
_cell_angle_beta                 121.342(10)
_cell_angle_gamma                90
_cell_volume                     6276(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    13643
_cell_measurement_theta_min      1.483
_cell_measurement_theta_max      24.249

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_F_000             3296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          .49
_exptl_crystal_size_mid          .34
_exptl_crystal_size_min          .11
_exptl_absorpt_coefficient_mu    1.853
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  .474
_exptl_absorpt_correction_T_max  .816
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13643
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.483
_diffrn_reflns_theta_max         24.249
_diffrn_reflns_theta_full        24.249
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.933
_reflns_number_total             4749
_reflns_number_gt                2408
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1002P)²+7.8897P] 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         4749
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.2121
_refine_ls_wR_factor_gt          0.1596
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_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
Ni4 Ni 0.500000 0.28899(7) 0.750000 0.0423(4) Uani 1 2 d S T P . .
Ni2 Ni 0.52359(7) 0.35965(5) 0.60098(8) 0.0501(4) Uani 1 1 d . . . . .
Ni3 Ni 0.51381(7) 0.22578(5) 0.58687(8) 0.0514(4) Uani 1 1 d . . . . .
Ni1 Ni 0.500000 0.42392(7) 0.750000 0.0520(5) Uani 1 2 d S T P . .
O8 O 0.5675(3) 0.2878(2) 0.6931(4) 0.0415(14) Uani 1 1 d . . . . .
H8 H 0.623702 0.285004 0.737560 0.050 Uiso 1 1 calc R U . . .
O9 O 0.4483(3) 0.3587(2) 0.6522(4) 0.0431(14) Uani 1 1 d . . . . .
H9 H 0.392129 0.359196 0.606464 0.052 Uiso 1 1 calc R U . . .
O6 O 0.4679(3) 0.2968(2) 0.5035(4) 0.0521(16) Uani 1 1 d . . . . .
O2 O 0.4375(3) 0.2285(3) 0.6333(4) 0.0469(15) Uani 1 1 d . . . . .
O1 O 0.5624(4) 0.4277(2) 0.6894(4) 0.0549(16) Uani 1 1 d . . . . .
O4 O 0.3052(4) 0.2531(3) 0.6211(4) 0.0676(19) Uani 1 1 d . . . . .
O3 O 0.5916(4) 0.4900(3) 0.8379(5) 0.0660(18) Uani 1 1 d . . . . .
N1 N 0.6198(5) 0.3628(3) 0.5900(5) 0.054(2) Uani 1 1 d . . . . .
O5 O 0.4598(5) 0.4192(3) 0.4848(6) 0.084(2) Uani 1 1 d . . . . .
N2 N 0.6096(4) 0.2147(4) 0.5684(5) 0.061(2) Uani 1 1 d . . . . .
H2 H 0.589143 0.198728 0.502708 0.073 Uiso 1 1 calc R U . . .
O7 O 0.4373(4) 0.1959(3) 0.4190(5) 0.080(2) Uani 1 1 d . . . . .
N3 N 0.5323(5) 0.1427(4) 0.6262(6) 0.063(2) Uani 1 1 d . . . . .
C27 C 0.4355(5) 0.2985(4) 0.4089(6) 0.053(2) Uani 1 1 d . . . . .
N4 N 0.6545(8) 0.1213(5) 0.4172(7) 0.082(3) Uani 1 1 d . . . . .
C2 C 0.6522(6) 0.4829(4) 0.8228(7) 0.059(3) Uani 1 1 d . . . . .
C1 C 0.6343(6) 0.4484(4) 0.7427(7) 0.055(2) Uani 1 1 d . . . . .
C7 C 0.6784(6) 0.3965(4) 0.6432(7) 0.061(3) Uani 1 1 d . . . . .
H7 H 0.718581 0.394780 0.631073 0.074 Uiso 1 1 calc R U . . .
C26 C 0.4178(5) 0.2457(5) 0.3561(7) 0.064(3) Uani 1 1 d . . . . .
C8 C 0.6295(6) 0.3209(5) 0.5287(7) 0.069(3) Uani 1 1 d . . . . .
H8A H 0.662790 0.338092 0.508251 0.083 Uiso 1 1 calc R U . . .
H8B H 0.579543 0.313086 0.470679 0.083 Uiso 1 1 calc R U . . .
C18 C 0.3939(6) 0.1847(5) 0.6274(6) 0.056(2) Uani 1 1 d . . . . .
C3 C 0.7262(6) 0.5060(4) 0.8820(7) 0.070(3) Uani 1 1 d . . . . .
H3 H 0.739106 0.527666 0.937688 0.084 Uiso 1 1 calc R U . . .
O12 O 0.5923(7) 0.1350(5) 0.4030(7) 0.147(5) Uani 1 1 d . . . . .
C6 C 0.6893(6) 0.4361(4) 0.7182(7) 0.058(2) Uani 1 1 d . . . . .
C12 C 0.4840(8) 0.1086(4) 0.6313(7) 0.070(3) Uani 1 1 d . . . . .
H12 H 0.495923 0.068579 0.638655 0.084 Uiso 1 1 calc R U . . .
O11 O 0.6609(6) 0.0793(5) 0.3747(8) 0.137(4) Uani 1 1 d . . . . .
C13 C 0.4139(7) 0.1248(5) 0.6271(7) 0.068(3) Uani 1 1 d . . . . .
C22 C 0.4146(6) 0.3509(5) 0.3565(7) 0.068(3) Uani 1 1 d . . . . .
C17 C 0.3215(6) 0.1955(5) 0.6192(7) 0.066(3) Uani 1 1 d . . . . .
C9 C 0.6651(6) 0.2624(5) 0.5820(8) 0.072(3) Uani 1 1 d . . . . .
H9A H 0.698799 0.247641 0.560462 0.086 Uiso 1 1 calc R U . . .
H9B H 0.697225 0.270689 0.651202 0.086 Uiso 1 1 calc R U . . .
C5 C 0.7623(6) 0.4621(5) 0.7758(9) 0.073(3) Uani 1 1 d . . . . .
H5 H 0.799948 0.456575 0.759743 0.088 Uiso 1 1 calc R U . . .
C11 C 0.5986(6) 0.1169(5) 0.6248(7) 0.073(3) Uani 1 1 d . . . . .
H11A H 0.580806 0.096853 0.563315 0.088 Uiso 1 1 calc R U . . .
H11B H 0.624850 0.088413 0.677176 0.088 Uiso 1 1 calc R U . . .
C10 C 0.6537(7) 0.1665(5) 0.6377(8) 0.082(3) Uani 1 1 d . . . . .
H10A H 0.679260 0.181305 0.704060 0.099 Uiso 1 1 calc R U . . .
H10B H 0.693078 0.151857 0.625668 0.099 Uiso 1 1 calc R U . . .
C25 C 0.3873(7) 0.2458(6) 0.2599(8) 0.092(4) Uani 1 1 d . . . . .
H25 H 0.379081 0.210369 0.226718 0.110 Uiso 1 1 calc R U . . .
C20 C 0.2310(5) 0.2682(5) 0.6070(7) 0.080(3) Uani 1 1 d . . . . .
H20A H 0.190865 0.256414 0.542766 0.120 Uiso 1 1 calc R U . . .
H20B H 0.228392 0.310053 0.614027 0.120 Uiso 1 1 calc R U . . .
H20C H 0.224182 0.248162 0.654718 0.120 Uiso 1 1 calc R U . . .
C21 C 0.4258(7) 0.4076(6) 0.4015(10) 0.095(4) Uani 1 1 d . . . . .
H21 H 0.403185 0.439340 0.359029 0.114 Uiso 1 1 calc R U . . .
O10 O 0.7090(7) 0.1484(5) 0.4724(9) 0.169(5) Uani 1 1 d . . . . .
C4 C 0.7788(7) 0.4956(5) 0.8553(10) 0.087(4) Uani 1 1 d . . . . .
H4 H 0.828058 0.511910 0.892552 0.105 Uiso 1 1 calc R U . . .
C16 C 0.2731(7) 0.1494(6) 0.6085(8) 0.088(4) Uani 1 1 d . . . . .
H16 H 0.224854 0.157169 0.600137 0.105 Uiso 1 1 calc R U . . .
C19 C 0.6037(7) 0.5234(5) 0.9179(9) 0.096(4) Uani 1 1 d . . . . .
H19A H 0.635192 0.501398 0.976826 0.144 Uiso 1 1 calc R U . . .
H19B H 0.554752 0.532216 0.911363 0.144 Uiso 1 1 calc R U . . .
H19C H 0.629521 0.559561 0.920545 0.144 Uiso 1 1 calc R U . . .
C24 C 0.3678(8) 0.2990(8) 0.2091(9) 0.107(5) Uani 1 1 d . . . . .
H24 H 0.346011 0.298808 0.141848 0.128 Uiso 1 1 calc R U . . .
C14 C 0.3638(9) 0.0777(5) 0.6194(8) 0.092(4) Uani 1 1 d . . . . .
H14 H 0.378018 0.038482 0.621003 0.111 Uiso 1 1 calc R U . . .
C23 C 0.3798(7) 0.3497(7) 0.2557(9) 0.096(4) Uani 1 1 d . . . . .
H23 H 0.364923 0.384835 0.220649 0.115 Uiso 1 1 calc R U . . .
C15 C 0.2958(9) 0.0917(7) 0.6100(9) 0.105(5) Uani 1 1 d . . . . .
H15 H 0.262629 0.061460 0.604129 0.126 Uiso 1 1 calc R U . . .
C28 C 0.4134(8) 0.1424(5) 0.3734(10) 0.120(5) Uani 1 1 d . . . . .
H28A H 0.364951 0.147016 0.312943 0.180 Uiso 1 1 calc R U . . .
H28B H 0.406846 0.115316 0.414612 0.180 Uiso 1 1 calc R U . . .
H28C H 0.451531 0.127166 0.360503 0.180 Uiso 1 1 calc R U . . .
O13 O 0.500000 0.9634(11) 0.750000 0.285(11) Uiso 1 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni4 O8 1.998(5) 2_656 ?
Ni4 O8 1.998(5) . ?
Ni4 O9 2.083(5) . ?
Ni4 O9 2.083(5) 2_656 ?
Ni4 O2 2.126(6) 2_656 ?
Ni4 O2 2.126(6) . ?
Ni2 O1 1.961(6) . ?
Ni2 O6 1.978(6) . ?
Ni2 N1 2.043(8) . ?
Ni2 O8 2.063(5) . ?
Ni2 O9 2.073(5) . ?
Ni2 O5 2.112(7) . ?
Ni3 N3 1.959(8) . ?
Ni3 O6 1.986(5) . ?
Ni3 O2 2.033(6) . ?
Ni3 O8 2.033(5) . ?
Ni3 N2 2.120(8) . ?
Ni3 O7 2.402(7) . ?
Ni1 O1 1.955(6) 2_656 ?
Ni1 O1 1.955(6) . ?
Ni1 O9 2.008(5) 2_656 ?
Ni1 O9 2.009(5) . ?
Ni1 O3 2.223(6) 2_656 ?
Ni1 O3 2.223(6) . ?
O8 H8 0.9800 . ?
O9 H9 0.9800 . ?
O6 C27 1.304(9) . ?
O2 C18 1.298(10) . ?
O1 C1 1.330(10) . ?
O4 C17 1.349(12) . ?
O4 C20 1.436(10) . ?
O3 C2 1.377(11) . ?
O3 C19 1.398(11) . ?
N1 C7 1.290(11) . ?
N1 C8 1.451(11) . ?
O5 C21 1.172(13) . ?
N2 C10 1.480(12) . ?
N2 C9 1.490(12) . ?
N2 H2 0.9800 . ?
O7 C28 1.370(12) . ?
O7 C26 1.425(12) . ?
N3 C12 1.280(12) . ?
N3 C11 1.472(11) . ?
C27 C22 1.388(13) . ?
C27 C26 1.401(12) . ?
N4 O10 1.166(12) . ?
N4 O12 1.196(12) . ?
N4 O11 1.217(12) . ?
C2 C1 1.383(13) . ?
C2 C3 1.390(13) . ?
C1 C6 1.387(12) . ?
C7 C6 1.422(13) . ?
C7 H7 0.9300 . ?
C26 C25 1.331(14) . ?
C8 C9 1.537(13) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C18 C13 1.416(13) . ?
C18 C17 1.422(13) . ?
C3 C4 1.358(14) . ?
C3 H3 0.9300 . ?
C6 C5 1.400(13) . ?
C12 C13 1.431(14) . ?
C12 H12 0.9300 . ?
C13 C14 1.431(14) . ?
C22 C23 1.388(14) . ?
C22 C21 1.433(16) . ?
C17 C16 1.379(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C5 C4 1.369(14) . ?
C5 H5 0.9300 . ?
C11 C10 1.519(14) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C25 C24 1.391(17) . ?
C25 H25 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21 0.9300 . ?
C4 H4 0.9300 . ?
C16 C15 1.381(17) . ?
C16 H16 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C24 C23 1.323(17) . ?
C24 H24 0.9300 . ?
C14 C15 1.339(16) . ?
C14 H14 0.9300 . ?
C23 H23 0.9300 . ?
C15 H15 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?

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
O8 Ni4 O8 178.5(3) 2_656 . ?
O8 Ni4 O9 99.2(2) 2_656 . ?
O8 Ni4 O9 82.0(2) . . ?
O8 Ni4 O9 82.0(2) 2_656 2_656 ?
O8 Ni4 O9 99.2(2) . 2_656 ?
O9 Ni4 O9 81.5(3) . 2_656 ?
O8 Ni4 O2 79.8(2) 2_656 2_656 ?
O8 Ni4 O2 99.2(2) . 2_656 ?
O9 Ni4 O2 170.9(2) . 2_656 ?
O9 Ni4 O2 89.4(2) 2_656 2_656 ?
O8 Ni4 O2 99.2(2) 2_656 . ?
O8 Ni4 O2 79.8(2) . . ?
O9 Ni4 O2 89.4(2) . . ?
O9 Ni4 O2 170.9(2) 2_656 . ?
O2 Ni4 O2 99.7(3) 2_656 . ?
O1 Ni2 O6 170.8(2) . . ?
O1 Ni2 N1 89.7(3) . . ?
O6 Ni2 N1 97.6(3) . . ?
O1 Ni2 O8 103.9(2) . . ?
O6 Ni2 O8 81.6(2) . . ?
N1 Ni2 O8 90.9(2) . . ?
O1 Ni2 O9 79.7(2) . . ?
O6 Ni2 O9 94.2(2) . . ?
N1 Ni2 O9 164.4(3) . . ?
O8 Ni2 O9 80.7(2) . . ?
O1 Ni2 O5 88.1(3) . . ?
O6 Ni2 O5 85.8(3) . . ?
N1 Ni2 O5 94.2(3) . . ?
O8 Ni2 O5 167.0(3) . . ?
O9 Ni2 O5 96.9(3) . . ?
N3 Ni3 O6 159.9(3) . . ?
N3 Ni3 O2 88.0(3) . . ?
O6 Ni3 O2 92.6(2) . . ?
N3 Ni3 O8 117.7(3) . . ?
O6 Ni3 O8 82.2(2) . . ?
O2 Ni3 O8 81.2(2) . . ?
N3 Ni3 N2 84.0(3) . . ?
O6 Ni3 N2 98.2(3) . . ?
O2 Ni3 N2 167.6(3) . . ?
O8 Ni3 N2 94.1(3) . . ?
N3 Ni3 O7 89.7(3) . . ?
O6 Ni3 O7 70.7(3) . . ?
O2 Ni3 O7 104.5(2) . . ?
O8 Ni3 O7 152.4(3) . . ?
N2 Ni3 O7 85.0(3) . . ?
O1 Ni1 O1 175.0(3) 2_656 . ?
O1 Ni1 O9 81.5(2) 2_656 2_656 ?
O1 Ni1 O9 102.3(2) . 2_656 ?
O1 Ni1 O9 102.3(2) 2_656 . ?
O1 Ni1 O9 81.5(2) . . ?
O9 Ni1 O9 85.2(3) 2_656 . ?
O1 Ni1 O3 75.3(3) 2_656 2_656 ?
O1 Ni1 O3 101.2(2) . 2_656 ?
O9 Ni1 O3 156.2(2) 2_656 2_656 ?
O9 Ni1 O3 94.4(2) . 2_656 ?
O1 Ni1 O3 101.2(2) 2_656 . ?
O1 Ni1 O3 75.3(3) . . ?
O9 Ni1 O3 94.4(2) 2_656 . ?
O9 Ni1 O3 156.2(2) . . ?
O3 Ni1 O3 95.3(3) 2_656 . ?
Ni4 O8 Ni3 101.5(2) . . ?
Ni4 O8 Ni2 100.1(2) . . ?
Ni3 O8 Ni2 95.8(2) . . ?
Ni4 O8 H8 118.5 . . ?
Ni3 O8 H8 118.5 . . ?
Ni2 O8 H8 118.5 . . ?
Ni1 O9 Ni2 96.4(2) . . ?
Ni1 O9 Ni4 96.7(2) . . ?
Ni2 O9 Ni4 97.0(2) . . ?
Ni1 O9 H9 120.4 . . ?
Ni2 O9 H9 120.4 . . ?
Ni4 O9 H9 120.4 . . ?
C27 O6 Ni2 129.3(6) . . ?
C27 O6 Ni3 125.8(6) . . ?
Ni2 O6 Ni3 100.2(2) . . ?
C18 O2 Ni3 124.4(6) . . ?
C18 O2 Ni4 128.9(5) . . ?
Ni3 O2 Ni4 97.2(2) . . ?
C1 O1 Ni1 117.8(6) . . ?
C1 O1 Ni2 129.4(6) . . ?
Ni1 O1 Ni2 101.9(3) . . ?
C17 O4 C20 118.2(8) . . ?
C2 O3 C19 118.6(8) . . ?
C2 O3 Ni1 109.4(5) . . ?
C19 O3 Ni1 129.6(6) . . ?
C7 N1 C8 115.8(8) . . ?
C7 N1 Ni2 123.4(7) . . ?
C8 N1 Ni2 120.4(7) . . ?
C21 O5 Ni2 126.2(9) . . ?
C10 N2 C9 108.2(8) . . ?
C10 N2 Ni3 102.7(6) . . ?
C9 N2 Ni3 124.4(6) . . ?
C10 N2 H2 106.8 . . ?
C9 N2 H2 106.8 . . ?
Ni3 N2 H2 106.8 . . ?
C28 O7 C26 115.6(9) . . ?
C28 O7 Ni3 133.8(8) . . ?
C26 O7 Ni3 110.6(6) . . ?
C12 N3 C11 119.5(10) . . ?
C12 N3 Ni3 125.2(8) . . ?
C11 N3 Ni3 113.5(7) . . ?
O6 C27 C22 122.8(9) . . ?
O6 C27 C26 119.6(9) . . ?
C22 C27 C26 117.6(9) . . ?
O10 N4 O12 119.5(13) . . ?
O10 N4 O11 120.3(14) . . ?
O12 N4 O11 120.2(13) . . ?
O3 C2 C1 113.7(9) . . ?
O3 C2 C3 125.1(10) . . ?
C1 C2 C3 121.2(10) . . ?
O1 C1 C2 117.9(9) . . ?
O1 C1 C6 121.0(9) . . ?
C2 C1 C6 121.1(10) . . ?
N1 C7 C6 128.2(9) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
C25 C26 C27 121.2(11) . . ?
C25 C26 O7 127.9(11) . . ?
C27 C26 O7 111.0(8) . . ?
N1 C8 C9 112.1(8) . . ?
N1 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
N1 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
O2 C18 C13 123.3(10) . . ?
O2 C18 C17 120.1(9) . . ?
C13 C18 C17 116.5(10) . . ?
C4 C3 C2 117.4(11) . . ?
C4 C3 H3 121.3 . . ?
C2 C3 H3 121.3 . . ?
C1 C6 C5 117.0(10) . . ?
C1 C6 C7 124.9(9) . . ?
C5 C6 C7 118.0(10) . . ?
N3 C12 C13 127.7(10) . . ?
N3 C12 H12 116.1 . . ?
C13 C12 H12 116.1 . . ?
C18 C13 C12 121.5(10) . . ?
C18 C13 C14 121.6(12) . . ?
C12 C13 C14 116.9(11) . . ?
C27 C22 C23 120.0(11) . . ?
C27 C22 C21 122.9(9) . . ?
C23 C22 C21 117.1(11) . . ?
O4 C17 C16 124.8(11) . . ?
O4 C17 C18 114.6(9) . . ?
C16 C17 C18 120.6(12) . . ?
N2 C9 C8 116.5(8) . . ?
N2 C9 H9A 108.2 . . ?
C8 C9 H9A 108.2 . . ?
N2 C9 H9B 108.2 . . ?
C8 C9 H9B 108.2 . . ?
H9A C9 H9B 107.3 . . ?
C4 C5 C6 120.7(10) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
N3 C11 C10 108.3(9) . . ?
N3 C11 H11A 110.0 . . ?
C10 C11 H11A 110.0 . . ?
N3 C11 H11B 110.0 . . ?
C10 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
N2 C10 C11 109.3(9) . . ?
N2 C10 H10A 109.8 . . ?
C11 C10 H10A 109.8 . . ?
N2 C10 H10B 109.8 . . ?
C11 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
C26 C25 C24 120.0(12) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O5 C21 C22 128.4(12) . . ?
O5 C21 H21 115.8 . . ?
C22 C21 H21 115.8 . . ?
C3 C4 C5 122.6(10) . . ?
C3 C4 H4 118.7 . . ?
C5 C4 H4 118.7 . . ?
C17 C16 C15 120.5(12) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
O3 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C23 C24 C25 120.5(11) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C15 C14 C13 118.1(13) . . ?
C15 C14 H14 121.0 . . ?
C13 C14 H14 121.0 . . ?
C24 C23 C22 120.6(12) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C14 C15 C16 122.6(12) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
O7 C28 H28A 109.5 . . ?
O7 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O7 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_refine_diff_density_max         1.119
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.101
# start Validation Reply Form
_vrf_PLAT029_I                   
;
PROBLEM: diffrn_measured_fraction_theta_full value Low . 0.933 Why
RESPONSE:This alert comes from the overall poor diffraction quality
of the crystal.
;
# end Validation Reply Form

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1907765'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-04-03 deposited with the CCDC.	2019-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 N8 Ni4 O17'
_chemical_formula_weight         1187.69

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

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

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

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

_cell_length_a                   13.838(4)
_cell_length_b                   29.260(9)
_cell_length_c                   14.867(4)
_cell_angle_alpha                90
_cell_angle_beta                 116.548(4)
_cell_angle_gamma                90
_cell_volume                     5385(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9473
_cell_measurement_theta_min      1.392
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_F_000             2456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .12
_exptl_absorpt_coefficient_mu    1.450
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  .654
_exptl_absorpt_correction_T_max  .840
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37759
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.392
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9473
_reflns_number_gt                6223
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1224P)²+36.5811P] 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         9473
_refine_ls_number_parameters     654
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0924
_refine_ls_wR_factor_ref         0.2922
_refine_ls_wR_factor_gt          0.2634
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.088
_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
O17 O 0.311(3) 0.5844(12) 0.009(3) 0.258(17) Uiso 0.78(3) 1 d . . P A 1
C43 C 0.233(4) 0.5978(16) 0.047(4) 0.219(19) Uiso 0.78(3) 1 d . . P A 1
C43A C 0.296(9) 0.583(4) 0.092(8) 0.12(3) Uiso 0.22(3) 1 d . . P A 2
O17A O 0.319(5) 0.546(2) 0.080(4) 0.12(3) Uiso 0.22(3) 1 d . . P A 2
Ni4 Ni 0.26238(10) 0.62541(4) 0.44656(9) 0.0442(3) Uani 1 1 d . . . . .
Ni3 Ni 0.06902(10) 0.68592(4) 0.42553(9) 0.0475(4) Uani 1 1 d . . . . .
Ni2 Ni 0.47369(10) 0.63297(4) 0.64764(9) 0.0463(3) Uani 1 1 d . . . . .
Ni1 Ni 0.27841(10) 0.69077(4) 0.61934(9) 0.0439(3) Uani 1 1 d . . . . .
O9 O 0.3133(5) 0.62196(19) 0.5973(4) 0.0420(14) Uani 1 1 d . . . . .
O10 O 0.2297(5) 0.69168(19) 0.4614(4) 0.0402(14) Uani 1 1 d . . . . .
O2 O 0.4326(5) 0.6311(2) 0.4979(5) 0.0456(15) Uani 1 1 d . . . . .
O1 O 0.1262(5) 0.6802(2) 0.5723(5) 0.0516(16) Uani 1 1 d . . . . .
O5 O 0.4309(5) 0.6971(2) 0.6525(5) 0.0491(15) Uani 1 1 d . . . . .
O6 O 0.0956(5) 0.6197(2) 0.4017(5) 0.0533(17) Uani 1 1 d . . . . .
O3 O -0.0744(6) 0.6606(3) 0.4536(6) 0.067(2) Uani 1 1 d . . . . .
O7 O 0.6145(6) 0.6778(2) 0.6611(6) 0.0631(19) Uani 1 1 d . . . . .
O4 O 0.4367(6) 0.6602(2) 0.3245(5) 0.065(2) Uani 1 1 d . . . . .
N1 N 0.3030(7) 0.6743(3) 0.7631(6) 0.053(2) Uani 1 1 d . . . . .
N4 N 0.2659(7) 0.7612(3) 0.6171(6) 0.053(2) Uani 1 1 d . . . . .
N3 N 0.5323(7) 0.5705(3) 0.6625(6) 0.053(2) Uani 1 1 d . . . . .
O12 O 0.2720(7) 0.5563(2) 0.4170(7) 0.076(2) Uani 1 1 d . U . . .
N5 N 0.0160(7) 0.7538(3) 0.4346(6) 0.055(2) Uani 1 1 d . . . . .
H5 H -0.031693 0.750031 0.466918 0.066 Uiso 1 1 calc R U . . .
N2 N 0.5431(7) 0.6306(3) 0.8064(6) 0.054(2) Uani 1 1 d . . . . .
H2 H 0.591537 0.657060 0.829472 0.065 Uiso 1 1 calc R U . . .
C26 C 0.4446(8) 0.7773(3) 0.6295(7) 0.051(2) Uani 1 1 d . . . . .
N6 N 0.0009(8) 0.6982(3) 0.2797(7) 0.066(2) Uani 1 1 d . . . . .
N8 N 0.7688(10) 0.7130(4) 0.9495(8) 0.078(3) Uani 1 1 d . . . . .
C21 C 0.4839(8) 0.7329(3) 0.6428(7) 0.049(2) Uani 1 1 d . . . . .
O8 O 0.0764(8) 0.5317(3) 0.4197(9) 0.100(3) Uani 1 1 d . . . . .
C18 C 0.4849(8) 0.6066(3) 0.4607(7) 0.048(2) Uani 1 1 d . . . . .
C27 C 0.3384(9) 0.7886(3) 0.6202(7) 0.056(3) Uani 1 1 d . . . . .
H27 H 0.321592 0.819549 0.616137 0.067 Uiso 1 1 calc R U . . .
C13 C 0.5460(8) 0.5664(3) 0.5077(8) 0.052(2) Uani 1 1 d . . . . .
O11 O 0.2329(7) 0.6279(4) 0.2959(6) 0.092(3) Uani 1 1 d . . . . .
C22 C 0.5871(8) 0.7235(4) 0.6465(7) 0.055(3) Uani 1 1 d . . . . .
C1 C 0.0691(8) 0.6594(3) 0.6147(8) 0.050(2) Uani 1 1 d . . . . .
C17 C 0.4894(9) 0.6210(3) 0.3711(8) 0.055(3) Uani 1 1 d . . . . .
C2 C -0.0379(9) 0.6485(4) 0.5525(9) 0.060(3) Uani 1 1 d . . . . .
C42 C 0.2665(9) 0.7232(3) 0.4113(8) 0.057(3) Uani 1 1 d . . . . .
H42A H 0.339785 0.716120 0.425801 0.085 Uiso 1 1 calc R U . . .
H42B H 0.263177 0.753604 0.434029 0.085 Uiso 1 1 calc R U . . .
H42C H 0.221593 0.721256 0.340135 0.085 Uiso 1 1 calc R U . . .
C25 C 0.5100(10) 0.8126(3) 0.6207(8) 0.060(3) Uani 1 1 d . . . . .
H25 H 0.485869 0.842689 0.612999 0.072 Uiso 1 1 calc R U . . .
O16 O 0.8270(9) 0.7438(4) 0.9962(8) 0.116(4) Uani 1 1 d . . . . .
C12 C 0.5613(8) 0.5495(3) 0.6041(8) 0.055(3) Uani 1 1 d . . . . .
H12 H 0.594652 0.521194 0.624814 0.066 Uiso 1 1 calc R U . . .
C41 C 0.2720(9) 0.5818(3) 0.6268(8) 0.060(3) Uani 1 1 d . . . . .
H41A H 0.194660 0.581156 0.590438 0.090 Uiso 1 1 calc R U . . .
H41B H 0.293020 0.582979 0.697678 0.090 Uiso 1 1 calc R U . . .
H41C H 0.301250 0.554677 0.611832 0.090 Uiso 1 1 calc R U . . .
C14 C 0.5986(9) 0.5417(4) 0.4612(9) 0.067(3) Uani 1 1 d . . . . .
H14 H 0.635062 0.514976 0.491279 0.080 Uiso 1 1 calc R U . . .
C38 C 0.0276(9) 0.5972(4) 0.3191(9) 0.065(3) Uani 1 1 d . . . . .
C28 C 0.1615(9) 0.7832(3) 0.5992(8) 0.058(3) Uani 1 1 d . . . . .
H28A H 0.176732 0.811641 0.636529 0.070 Uiso 1 1 calc R U . . .
H28B H 0.123753 0.763340 0.625292 0.070 Uiso 1 1 calc R U . . .
C16 C 0.5426(10) 0.5958(4) 0.3272(9) 0.072(3) Uani 1 1 d . . . . .
H16 H 0.541395 0.605620 0.267233 0.086 Uiso 1 1 calc R U . . .
C30 C -0.0568(9) 0.7667(4) 0.3302(8) 0.066(3) Uani 1 1 d . . . . .
H30A H -0.060015 0.799701 0.324239 0.079 Uiso 1 1 calc R U . . .
H30B H -0.129076 0.755566 0.312771 0.079 Uiso 1 1 calc R U . . .
C9 C 0.4780(9) 0.6326(4) 0.8633(8) 0.063(3) Uani 1 1 d . . . . .
H9A H 0.526244 0.628984 0.934337 0.075 Uiso 1 1 calc R U . . .
H9B H 0.428275 0.607007 0.843031 0.075 Uiso 1 1 calc R U . . .
C31 C -0.0181(9) 0.7469(4) 0.2578(8) 0.068(3) Uani 1 1 d . . . . .
H31A H -0.072256 0.751386 0.188958 0.081 Uiso 1 1 calc R U . . .
H31B H 0.048074 0.761838 0.266480 0.081 Uiso 1 1 calc R U . . .
C15 C 0.5978(11) 0.5558(4) 0.3731(9) 0.073(3) Uani 1 1 d . . . . .
H15 H 0.633526 0.538897 0.344118 0.088 Uiso 1 1 calc R U . . .
C11 C 0.5610(11) 0.5515(4) 0.7632(8) 0.073(3) Uani 1 1 d . . . . .
H11A H 0.610193 0.525945 0.776992 0.087 Uiso 1 1 calc R U . . .
H11B H 0.496798 0.541053 0.767748 0.087 Uiso 1 1 calc R U . . .
C23 C 0.6479(9) 0.7585(4) 0.6364(8) 0.063(3) Uani 1 1 d . . . . .
H23 H 0.714586 0.752233 0.638091 0.076 Uiso 1 1 calc R U . . .
C20 C 0.5039(12) 0.6999(4) 0.3695(9) 0.081(4) Uani 1 1 d . . . . .
H20A H 0.530083 0.698924 0.441097 0.121 Uiso 1 1 calc R U . . .
H20B H 0.462114 0.727205 0.343411 0.121 Uiso 1 1 calc R U . . .
H20C H 0.563994 0.699898 0.353628 0.121 Uiso 1 1 calc R U . . .
C33 C -0.0351(10) 0.6189(4) 0.2270(10) 0.075(3) Uani 1 1 d . . . . .
C29 C 0.0874(9) 0.7931(4) 0.4885(9) 0.067(3) Uani 1 1 d . . . . .
H29A H 0.042722 0.819369 0.484012 0.081 Uiso 1 1 calc R U . . .
H29B H 0.131446 0.800950 0.455068 0.081 Uiso 1 1 calc R U . . .
C32 C -0.0390(11) 0.6671(5) 0.2108(9) 0.079(4) Uani 1 1 d . . . . .
H32 H -0.073543 0.677166 0.144496 0.095 Uiso 1 1 calc R U . . .
C8 C 0.4137(9) 0.6765(4) 0.8492(8) 0.065(3) Uani 1 1 d . . . . .
H8A H 0.407460 0.682889 0.910391 0.078 Uiso 1 1 calc R U . . .
H8B H 0.452919 0.701582 0.838080 0.078 Uiso 1 1 calc R U . . .
C10 C 0.6149(10) 0.5901(4) 0.8378(8) 0.073(3) Uani 1 1 d . . . . .
H10A H 0.627741 0.580668 0.904719 0.087 Uiso 1 1 calc R U . . .
H10B H 0.683829 0.597624 0.839198 0.087 Uiso 1 1 calc R U . . .
O14 O 0.6724(11) 0.7169(5) 0.9085(12) 0.160(6) Uani 1 1 d . . . . .
C24 C 0.6104(11) 0.8029(4) 0.6236(9) 0.077(4) Uani 1 1 d . . . . .
H24 H 0.651860 0.826419 0.616822 0.092 Uiso 1 1 calc R U . . .
C5 C 0.0532(11) 0.6272(4) 0.7554(10) 0.072(3) Uani 1 1 d . . . . .
H5A H 0.083319 0.619751 0.823285 0.086 Uiso 1 1 calc R U . . .
O13 O 0.2419(12) 0.5396(6) 0.2372(11) 0.163(6) Uani 1 1 d . U . . .
C4 C -0.0501(12) 0.6172(4) 0.6971(12) 0.083(4) Uani 1 1 d . . . . .
H4 H -0.090372 0.602893 0.724980 0.099 Uiso 1 1 calc R U . . .
C3 C -0.0997(10) 0.6280(4) 0.5927(11) 0.075(3) Uani 1 1 d . . . . .
H3 H -0.172225 0.621429 0.552511 0.091 Uiso 1 1 calc R U . . .
C37 C 0.0174(11) 0.5498(4) 0.3264(12) 0.083(4) Uani 1 1 d . . . . .
C19 C -0.1813(11) 0.6519(5) 0.3862(11) 0.095(4) Uani 1 1 d . . . . .
H19A H -0.195168 0.619698 0.385137 0.142 Uiso 1 1 calc R U . . .
H19B H -0.194247 0.661760 0.320211 0.142 Uiso 1 1 calc R U . . .
H19C H -0.228287 0.668169 0.406828 0.142 Uiso 1 1 calc R U . . .
C39 C 0.7106(10) 0.6636(5) 0.6563(13) 0.096(5) Uani 1 1 d . . . . .
H39A H 0.717619 0.679881 0.603471 0.144 Uiso 1 1 calc R U . . .
H39B H 0.706993 0.631360 0.642880 0.144 Uiso 1 1 calc R U . . .
H39C H 0.772017 0.669898 0.719272 0.144 Uiso 1 1 calc R U . . .
C34 C -0.1002(14) 0.5933(7) 0.1418(14) 0.124(6) Uani 1 1 d . . . . .
H34 H -0.139075 0.607558 0.080134 0.149 Uiso 1 1 calc R U . . .
O15 O 0.8019(14) 0.6773(5) 0.9403(13) 0.198(9) Uani 1 1 d . . . . .
C36 C -0.0466(18) 0.5242(7) 0.2434(19) 0.139(8) Uani 1 1 d . . . . .
H36 H -0.049896 0.492627 0.249337 0.167 Uiso 1 1 calc R U . . .
C35 C -0.1064(19) 0.5449(8) 0.151(2) 0.158(9) Uani 1 1 d . . . . .
H35 H -0.149993 0.527435 0.095109 0.190 Uiso 1 1 calc R U . . .
C40 C 0.0812(18) 0.4841(6) 0.4357(16) 0.154(8) Uani 1 1 d . . . . .
H40A H 0.009784 0.472596 0.416735 0.231 Uiso 1 1 calc R U . . .
H40B H 0.126111 0.477780 0.505542 0.231 Uiso 1 1 calc R U . . .
H40C H 0.111056 0.469621 0.395822 0.231 Uiso 1 1 calc R U . . .
N7 N 0.2537(16) 0.5696(9) 0.321(2) 0.192(8) Uani 1 1 d . U . . .
C6 C 0.1180(10) 0.6488(4) 0.7174(9) 0.060(3) Uani 1 1 d . . . . .
C7 C 0.2302(10) 0.6579(4) 0.7847(8) 0.059(3) Uani 1 1 d . . . . .
H7 H 0.252121 0.651044 0.852105 0.071 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O17 C43 1.48(5) . ?
C43A O17A 1.17(11) . ?
Ni4 O10 2.025(6) . ?
Ni4 O9 2.029(6) . ?
Ni4 O12 2.086(7) . ?
Ni4 O11 2.090(8) . ?
Ni4 O6 2.103(7) . ?
Ni4 O2 2.134(6) . ?
Ni4 N7 2.45(3) . ?
Ni3 O1 1.968(6) . ?
Ni3 N6 1.973(10) . ?
Ni3 O6 2.032(6) . ?
Ni3 O10 2.049(6) . ?
Ni3 N5 2.142(8) . ?
Ni3 O3 2.324(7) . ?
Ni2 N3 1.971(8) . ?
Ni2 O5 1.978(6) . ?
Ni2 O9 2.026(6) . ?
Ni2 O2 2.038(6) . ?
Ni2 N2 2.115(8) . ?
Ni2 O7 2.282(7) . ?
Ni1 O1 1.925(7) . ?
Ni1 O5 1.950(6) . ?
Ni1 N1 2.066(8) . ?
Ni1 N4 2.067(8) . ?
Ni1 O9 2.130(6) . ?
Ni1 O10 2.134(6) . ?
O9 C41 1.459(11) . ?
O10 C42 1.415(11) . ?
O2 C18 1.304(11) . ?
O1 C1 1.355(11) . ?
O5 C21 1.323(11) . ?
O6 C38 1.339(13) . ?
O3 C2 1.371(13) . ?
O3 C19 1.390(14) . ?
O7 C22 1.381(12) . ?
O7 C39 1.425(13) . ?
O4 C17 1.371(12) . ?
O4 C20 1.451(14) . ?
N1 C7 1.279(14) . ?
N1 C8 1.495(14) . ?
N4 C27 1.269(13) . ?
N4 C28 1.493(13) . ?
N3 C12 1.268(13) . ?
N3 C11 1.476(13) . ?
O12 N7 1.39(3) . ?
N5 C30 1.473(12) . ?
N5 C29 1.495(14) . ?
N5 H5 0.9800 . ?
N2 C10 1.482(13) . ?
N2 C9 1.487(14) . ?
N2 H2 0.9800 . ?
C26 C21 1.389(14) . ?
C26 C25 1.417(14) . ?
C26 C27 1.451(15) . ?
N6 C32 1.295(15) . ?
N6 C31 1.457(14) . ?
N8 O15 1.174(17) . ?
N8 O14 1.199(15) . ?
N8 O16 1.202(13) . ?
C21 C22 1.430(14) . ?
O8 C37 1.363(17) . ?
O8 C40 1.409(17) . ?
C18 C17 1.425(14) . ?
C18 C13 1.434(13) . ?
C27 H27 0.9300 . ?
C13 C14 1.408(14) . ?
C13 C12 1.440(14) . ?
O11 N7 1.74(3) . ?
C22 C23 1.376(15) . ?
C1 C2 1.387(15) . ?
C1 C6 1.401(15) . ?
C17 C16 1.392(15) . ?
C2 C3 1.381(16) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C25 C24 1.400(17) . ?
C25 H25 0.9300 . ?
C12 H12 0.9300 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C14 C15 1.367(16) . ?
C14 H14 0.9300 . ?
C38 C37 1.404(16) . ?
C38 C33 1.402(17) . ?
C28 C29 1.529(14) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C16 C15 1.398(16) . ?
C16 H16 0.9300 . ?
C30 C31 1.515(15) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C9 C8 1.523(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C15 H15 0.9300 . ?
C11 C10 1.523(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C23 C24 1.380(17) . ?
C23 H23 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C33 C34 1.399(19) . ?
C33 C32 1.430(17) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C32 H32 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C24 H24 0.9300 . ?
C5 C4 1.331(18) . ?
C5 C6 1.404(15) . ?
C5 H5A 0.9300 . ?
O13 N7 1.47(2) . ?
C4 C3 1.424(19) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C37 C36 1.38(2) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C34 C35 1.43(3) . ?
C34 H34 0.9300 . ?
C36 C35 1.39(3) . ?
C36 H36 0.9300 . ?
C35 H35 0.9300 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C6 C7 1.448(16) . ?
C7 H7 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Ni4 O9 84.9(2) . . ?
O10 Ni4 O12 171.6(3) . . ?
O9 Ni4 O12 99.3(3) . . ?
O10 Ni4 O11 97.9(4) . . ?
O9 Ni4 O11 171.9(3) . . ?
O12 Ni4 O11 78.9(4) . . ?
O10 Ni4 O6 81.0(2) . . ?
O9 Ni4 O6 97.9(3) . . ?
O12 Ni4 O6 91.2(3) . . ?
O11 Ni4 O6 90.1(3) . . ?
O10 Ni4 O2 98.6(2) . . ?
O9 Ni4 O2 80.0(2) . . ?
O12 Ni4 O2 89.3(3) . . ?
O11 Ni4 O2 92.1(3) . . ?
O6 Ni4 O2 177.9(3) . . ?
O10 Ni4 N7 141.8(7) . . ?
O9 Ni4 N7 133.3(7) . . ?
O12 Ni4 N7 34.7(6) . . ?
O11 Ni4 N7 44.3(7) . . ?
O6 Ni4 N7 91.9(5) . . ?
O2 Ni4 N7 89.7(5) . . ?
O1 Ni3 N6 172.7(3) . . ?
O1 Ni3 O6 95.7(3) . . ?
N6 Ni3 O6 91.0(3) . . ?
O1 Ni3 O10 82.4(3) . . ?
N6 Ni3 O10 101.6(3) . . ?
O6 Ni3 O10 82.2(2) . . ?
O1 Ni3 N5 89.3(3) . . ?
N6 Ni3 N5 83.7(4) . . ?
O6 Ni3 N5 171.3(3) . . ?
O10 Ni3 N5 105.7(3) . . ?
O1 Ni3 O3 74.1(3) . . ?
N6 Ni3 O3 103.2(3) . . ?
O6 Ni3 O3 87.9(3) . . ?
O10 Ni3 O3 153.4(3) . . ?
N5 Ni3 O3 86.5(3) . . ?
N3 Ni2 O5 171.8(3) . . ?
N3 Ni2 O9 102.8(3) . . ?
O5 Ni2 O9 82.4(2) . . ?
N3 Ni2 O2 89.9(3) . . ?
O5 Ni2 O2 97.1(3) . . ?
O9 Ni2 O2 82.4(2) . . ?
N3 Ni2 N2 83.5(3) . . ?
O5 Ni2 N2 89.1(3) . . ?
O9 Ni2 N2 106.4(3) . . ?
O2 Ni2 N2 169.9(3) . . ?
N3 Ni2 O7 103.3(3) . . ?
O5 Ni2 O7 73.1(3) . . ?
O9 Ni2 O7 151.1(2) . . ?
O2 Ni2 O7 85.5(3) . . ?
N2 Ni2 O7 88.7(3) . . ?
O1 Ni1 O5 172.9(3) . . ?
O1 Ni1 N1 89.2(3) . . ?
O5 Ni1 N1 95.8(3) . . ?
O1 Ni1 N4 94.8(3) . . ?
O5 Ni1 N4 89.0(3) . . ?
N1 Ni1 N4 102.9(3) . . ?
O1 Ni1 O9 94.6(3) . . ?
O5 Ni1 O9 80.4(2) . . ?
N1 Ni1 O9 89.8(3) . . ?
N4 Ni1 O9 164.4(3) . . ?
O1 Ni1 O10 81.2(2) . . ?
O5 Ni1 O10 92.9(3) . . ?
N1 Ni1 O10 165.2(3) . . ?
N4 Ni1 O10 89.2(3) . . ?
O9 Ni1 O10 79.9(2) . . ?
C41 O9 Ni2 121.9(6) . . ?
C41 O9 Ni4 112.5(5) . . ?
Ni2 O9 Ni4 100.5(3) . . ?
C41 O9 Ni1 124.7(6) . . ?
Ni2 O9 Ni1 94.5(2) . . ?
Ni4 O9 Ni1 97.6(2) . . ?
C42 O10 Ni4 114.6(5) . . ?
C42 O10 Ni3 121.4(6) . . ?
Ni4 O10 Ni3 99.3(2) . . ?
C42 O10 Ni1 125.2(6) . . ?
Ni4 O10 Ni1 97.6(2) . . ?
Ni3 O10 Ni1 93.3(2) . . ?
C18 O2 Ni2 122.7(6) . . ?
C18 O2 Ni4 122.6(6) . . ?
Ni2 O2 Ni4 96.7(2) . . ?
C1 O1 Ni1 132.3(6) . . ?
C1 O1 Ni3 121.7(6) . . ?
Ni1 O1 Ni3 102.8(3) . . ?
C21 O5 Ni1 129.6(6) . . ?
C21 O5 Ni2 123.9(6) . . ?
Ni1 O5 Ni2 102.0(3) . . ?
C38 O6 Ni3 121.4(7) . . ?
C38 O6 Ni4 123.5(6) . . ?
Ni3 O6 Ni4 97.3(3) . . ?
C2 O3 C19 119.2(10) . . ?
C2 O3 Ni3 109.9(7) . . ?
C19 O3 Ni3 130.4(8) . . ?
C22 O7 C39 118.1(9) . . ?
C22 O7 Ni2 112.3(6) . . ?
C39 O7 Ni2 127.4(7) . . ?
C17 O4 C20 110.5(9) . . ?
C7 N1 C8 115.0(9) . . ?
C7 N1 Ni1 124.3(7) . . ?
C8 N1 Ni1 120.5(7) . . ?
C27 N4 C28 114.9(9) . . ?
C27 N4 Ni1 124.8(7) . . ?
C28 N4 Ni1 120.0(7) . . ?
C12 N3 C11 119.2(9) . . ?
C12 N3 Ni2 127.9(7) . . ?
C11 N3 Ni2 111.9(7) . . ?
N7 O12 Ni4 86.9(11) . . ?
C30 N5 C29 110.1(8) . . ?
C30 N5 Ni3 105.2(6) . . ?
C29 N5 Ni3 125.7(6) . . ?
C30 N5 H5 104.6 . . ?
C29 N5 H5 104.6 . . ?
Ni3 N5 H5 104.6 . . ?
C10 N2 C9 110.1(8) . . ?
C10 N2 Ni2 106.5(6) . . ?
C9 N2 Ni2 123.1(6) . . ?
C10 N2 H2 105.3 . . ?
C9 N2 H2 105.3 . . ?
Ni2 N2 H2 105.3 . . ?
C21 C26 C25 118.0(10) . . ?
C21 C26 C27 122.9(9) . . ?
C25 C26 C27 119.1(10) . . ?
C32 N6 C31 122.6(10) . . ?
C32 N6 Ni3 124.5(9) . . ?
C31 N6 Ni3 112.0(7) . . ?
O15 N8 O14 115.4(15) . . ?
O15 N8 O16 122.7(16) . . ?
O14 N8 O16 121.8(16) . . ?
O5 C21 C26 123.7(9) . . ?
O5 C21 C22 115.9(9) . . ?
C26 C21 C22 120.4(9) . . ?
C37 O8 C40 121.2(13) . . ?
O2 C18 C17 119.9(8) . . ?
O2 C18 C13 124.2(9) . . ?
C17 C18 C13 115.8(9) . . ?
N4 C27 C26 127.6(9) . . ?
N4 C27 H27 116.2 . . ?
C26 C27 H27 116.2 . . ?
C14 C13 C18 120.3(10) . . ?
C14 C13 C12 115.7(9) . . ?
C18 C13 C12 124.1(9) . . ?
N7 O11 Ni4 78.8(10) . . ?
C23 C22 O7 126.9(10) . . ?
C23 C22 C21 120.1(10) . . ?
O7 C22 C21 113.0(9) . . ?
O1 C1 C2 117.6(9) . . ?
O1 C1 C6 120.6(9) . . ?
C2 C1 C6 121.8(10) . . ?
O4 C17 C16 118.7(10) . . ?
O4 C17 C18 119.0(9) . . ?
C16 C17 C18 122.3(10) . . ?
O3 C2 C3 125.0(11) . . ?
O3 C2 C1 115.3(10) . . ?
C3 C2 C1 119.6(11) . . ?
O10 C42 H42A 109.5 . . ?
O10 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O10 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C24 C25 C26 121.0(10) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
N3 C12 C13 124.3(9) . . ?
N3 C12 H12 117.9 . . ?
C13 C12 H12 117.9 . . ?
O9 C41 H41A 109.5 . . ?
O9 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O9 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C15 C14 C13 122.1(10) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
O6 C38 C37 117.9(11) . . ?
O6 C38 C33 123.3(10) . . ?
C37 C38 C33 118.8(11) . . ?
N4 C28 C29 113.8(8) . . ?
N4 C28 H28A 108.8 . . ?
C29 C28 H28A 108.8 . . ?
N4 C28 H28B 108.8 . . ?
C29 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C17 C16 C15 120.2(11) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
N5 C30 C31 111.0(8) . . ?
N5 C30 H30A 109.4 . . ?
C31 C30 H30A 109.4 . . ?
N5 C30 H30B 109.4 . . ?
C31 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
N2 C9 C8 114.8(9) . . ?
N2 C9 H9A 108.6 . . ?
C8 C9 H9A 108.6 . . ?
N2 C9 H9B 108.6 . . ?
C8 C9 H9B 108.6 . . ?
H9A C9 H9B 107.5 . . ?
N6 C31 C30 107.5(9) . . ?
N6 C31 H31A 110.2 . . ?
C30 C31 H31A 110.2 . . ?
N6 C31 H31B 110.2 . . ?
C30 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
C14 C15 C16 119.2(11) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
N3 C11 C10 106.3(9) . . ?
N3 C11 H11A 110.5 . . ?
C10 C11 H11A 110.5 . . ?
N3 C11 H11B 110.5 . . ?
C10 C11 H11B 110.5 . . ?
H11A C11 H11B 108.7 . . ?
C22 C23 C24 120.3(12) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C34 C33 C38 120.6(14) . . ?
C34 C33 C32 114.6(14) . . ?
C38 C33 C32 124.8(11) . . ?
N5 C29 C28 113.3(9) . . ?
N5 C29 H29A 108.9 . . ?
C28 C29 H29A 108.9 . . ?
N5 C29 H29B 108.9 . . ?
C28 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
N6 C32 C33 126.2(12) . . ?
N6 C32 H32 116.9 . . ?
C33 C32 H32 116.9 . . ?
N1 C8 C9 113.3(9) . . ?
N1 C8 H8A 108.9 . . ?
C9 C8 H8A 108.9 . . ?
N1 C8 H8B 108.9 . . ?
C9 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
N2 C10 C11 108.8(9) . . ?
N2 C10 H10A 109.9 . . ?
C11 C10 H10A 109.9 . . ?
N2 C10 H10B 109.9 . . ?
C11 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C23 C24 C25 120.2(11) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C4 C5 C6 122.0(12) . . ?
C4 C5 H5A 119.0 . . ?
C6 C5 H5A 119.0 . . ?
C5 C4 C3 121.0(12) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C2 C3 C4 118.5(12) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
O8 C37 C36 123.6(16) . . ?
O8 C37 C38 115.3(11) . . ?
C36 C37 C38 121.1(17) . . ?
O3 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O7 C39 H39A 109.5 . . ?
O7 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O7 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C33 C34 C35 119.2(19) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C37 C36 C35 120.6(19) . . ?
C37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C36 C35 C34 119.5(18) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
O8 C40 H40A 109.5 . . ?
O8 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O8 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O12 N7 O13 127(2) . . ?
O12 N7 O11 115.3(16) . . ?
O13 N7 O11 117(2) . . ?
O12 N7 Ni4 58.4(10) . . ?
O13 N7 Ni4 174.1(19) . . ?
O11 N7 Ni4 57.0(7) . . ?
C1 C6 C5 117.0(11) . . ?
C1 C6 C7 123.9(10) . . ?
C5 C6 C7 119.1(11) . . ?
N1 C7 C6 128.2(10) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?

_refine_diff_density_max         1.264
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.150
_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 153.7 32.9 ?
2 0.000 0.500 0.000 153.7 32.9 ?
3 0.500 0.000 0.500 208.6 32.0 ?
4 0.500 0.500 1.000 208.6 32.0 ?


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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1907764'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh'
;University of Calcutta
India
;
_audit_update_record             
;
2019-04-03 deposited with the CCDC.	2019-06-24 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         ?
_chemical_formula_sum            'C32 H44 N8 Ni2 O13'
_chemical_formula_weight         866.13

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

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

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

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

_cell_length_a                   22.233(4)
_cell_length_b                   7.3217(14)
_cell_length_c                   23.045(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.296(4)
_cell_angle_gamma                90
_cell_volume                     3678.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    86877
_cell_measurement_theta_min      2.186
_cell_measurement_theta_max      25.303

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_F_000             1808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .1
_exptl_absorpt_coefficient_mu    1.100
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  .768
_exptl_absorpt_correction_T_max  .896
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      299(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            86877
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.186
_diffrn_reflns_theta_max         25.303
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6675
_reflns_number_gt                5907
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0437P)²+2.9399P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6675
_refine_ls_number_parameters     503
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.0990
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.89190(2) 0.38440(4) 0.51914(2) 0.03641(10) Uani 1 1 d . . . . .
Ni1 Ni 0.40671(2) 0.19221(5) 0.25000(2) 0.03825(11) Uani 1 1 d . . . . .
O5 O 0.92410(8) 0.3361(3) 0.45362(7) 0.0398(4) Uani 1 1 d . . . . .
O6 O 0.95082(9) 0.2828(3) 0.35065(8) 0.0531(5) Uani 1 1 d . . . . .
O1 O 0.45278(8) 0.2195(3) 0.32419(8) 0.0480(5) Uani 1 1 d . . . . .
O2 O 0.63465(9) 0.0989(3) 0.32176(9) 0.0508(5) Uani 1 1 d . . . . .
H2 H 0.666765 0.113538 0.345754 0.076 Uiso 1 1 calc R U . . .
O3 O 0.53575(10) 0.2432(4) 0.42094(9) 0.0639(6) Uani 1 1 d . . . . .
N2 N 0.36141(10) 0.1688(3) 0.17209(10) 0.0440(5) Uani 1 1 d . . . . .
H2A H 0.353833 0.291665 0.155397 0.053 Uiso 1 1 calc R U . . .
N3 N 0.47820(10) 0.1810(3) 0.21543(9) 0.0380(5) Uani 1 1 d . . . . .
N5 N 0.85495(11) 0.4385(3) 0.58440(9) 0.0457(5) Uani 1 1 d . . . . .
H5A H 0.865455 0.564758 0.596368 0.055 Uiso 1 1 calc R U . . .
N4 N 0.95890(11) 0.3098(3) 0.57394(9) 0.0424(5) Uani 1 1 d . . . . .
N6 N 0.81481(10) 0.4498(3) 0.46990(9) 0.0450(5) Uani 1 1 d . . . . .
H6A H 0.820936 0.532551 0.443381 0.054 Uiso 1 1 calc R U . . .
H6B H 0.797865 0.351613 0.450503 0.054 Uiso 1 1 calc R U . . .
O13 O 0.85885(11) 0.9181(4) 0.86213(10) 0.0703(7) Uani 1 1 d G . . . .
H13A H 0.867895 0.872652 0.830999 0.105 Uiso 1 1 d G U . . .
H13B H 0.880381 1.014655 0.868372 0.105 Uiso 1 1 d G U . . .
O8 O 0.71844(12) 0.1660(3) 0.42089(11) 0.0737(7) Uani 1 1 d . . . . .
O4 O 0.74699(10) 0.1185(4) 0.30160(12) 0.0726(7) Uani 1 1 d . . . . .
O7 O 0.70514(13) -0.1215(3) 0.42743(11) 0.0759(7) Uani 1 1 d . . . . .
N7 N 0.73071(11) 0.0198(4) 0.44734(11) 0.0517(6) Uani 1 1 d . . . . .
N1 N 0.33221(10) 0.1847(3) 0.27348(11) 0.0471(6) Uani 1 1 d . . . . .
C27 C 1.00914(13) 0.2469(4) 0.56278(12) 0.0453(7) Uani 1 1 d . . . . .
H27 H 1.039389 0.213146 0.594848 0.054 Uiso 1 1 calc R U . . .
C12 C 0.53303(11) 0.1893(3) 0.24421(11) 0.0378(6) Uani 1 1 d . . . . .
H12 H 0.536569 0.197797 0.285006 0.045 Uiso 1 1 calc R U . . .
C21 C 0.97857(11) 0.2681(3) 0.45383(11) 0.0361(5) Uani 1 1 d . . . . .
C22 C 0.99521(12) 0.2344(4) 0.39809(12) 0.0412(6) Uani 1 1 d . . . . .
N8 N 0.85295(15) 0.8073(5) 0.70814(16) 0.0709(9) Uani 1 1 d . . . . .
C13 C 0.59164(12) 0.1877(4) 0.22425(12) 0.0404(6) Uani 1 1 d . . . . .
C18 C 0.64286(12) 0.1475(4) 0.26740(12) 0.0420(6) Uani 1 1 d . . . . .
C6 C 0.37057(14) 0.2091(4) 0.37801(14) 0.0520(7) Uani 1 1 d . . . . .
C10 C 0.39959(13) 0.0705(4) 0.13726(12) 0.0497(7) Uani 1 1 d . . . . .
H10A H 0.382046 0.080044 0.095382 0.060 Uiso 1 1 calc R U . . .
H10B H 0.402235 -0.057666 0.148086 0.060 Uiso 1 1 calc R U . . .
C23 C 1.05131(12) 0.1627(4) 0.39437(14) 0.0481(7) Uani 1 1 d . . . . .
H23 H 1.060913 0.140079 0.357528 0.058 Uiso 1 1 calc R U . . .
C17 C 0.70215(13) 0.1566(4) 0.25429(16) 0.0537(8) Uani 1 1 d . . . . .
C11 C 0.46220(14) 0.1565(4) 0.15039(11) 0.0480(7) Uani 1 1 d . . . . .
H11A H 0.491909 0.077968 0.137044 0.058 Uiso 1 1 calc R U . . .
H11B H 0.461663 0.273418 0.130506 0.058 Uiso 1 1 calc R U . . .
C9 C 0.30146(13) 0.0837(4) 0.17343(14) 0.0544(8) Uani 1 1 d . . . . .
H9A H 0.306008 -0.047264 0.179035 0.065 Uiso 1 1 calc R U . . .
H9B H 0.272865 0.106403 0.136601 0.065 Uiso 1 1 calc R U . . .
O9 O 0.76620(16) 0.0211(4) 0.49442(14) 0.1203(13) Uani 1 1 d . . . . .
C30 C 0.78761(15) 0.4279(5) 0.56536(13) 0.0558(8) Uani 1 1 d . . . . .
H30A H 0.767424 0.486808 0.594056 0.067 Uiso 1 1 calc R U . . .
H30B H 0.774292 0.301614 0.561050 0.067 Uiso 1 1 calc R U . . .
C2 C 0.47639(15) 0.2346(4) 0.42785(12) 0.0518(7) Uani 1 1 d . . . . .
C31 C 0.77283(14) 0.5254(5) 0.50679(13) 0.0537(7) Uani 1 1 d . . . . .
H31A H 0.730421 0.504430 0.487939 0.064 Uiso 1 1 calc R U . . .
H31B H 0.779237 0.655804 0.512298 0.064 Uiso 1 1 calc R U . . .
C1 C 0.43286(13) 0.2213(4) 0.37400(12) 0.0443(6) Uani 1 1 d . . . . .
C7 C 0.32341(14) 0.1923(4) 0.32646(15) 0.0552(8) Uani 1 1 d . . . . .
H7 H 0.283116 0.186486 0.331954 0.066 Uiso 1 1 calc R U . . .
C24 C 1.09417(13) 0.1237(4) 0.44599(15) 0.0531(7) Uani 1 1 d . . . . .
H24 H 1.132484 0.077114 0.443459 0.064 Uiso 1 1 calc R U . . .
C29 C 0.88236(18) 0.3184(5) 0.63398(13) 0.0613(9) Uani 1 1 d . . . . .
H29A H 0.866524 0.195083 0.627435 0.074 Uiso 1 1 calc R U . . .
H29B H 0.873300 0.363398 0.670916 0.074 Uiso 1 1 calc R U . . .
C14 C 0.60076(15) 0.2363(4) 0.16723(14) 0.0556(8) Uani 1 1 d . . . . .
H14 H 0.567261 0.264831 0.137619 0.067 Uiso 1 1 calc R U . . .
C16 C 0.70926(16) 0.2019(5) 0.19849(17) 0.0652(9) Uani 1 1 d . . . . .
H16 H 0.748276 0.205920 0.189604 0.078 Uiso 1 1 calc R U . . .
C5 C 0.35367(18) 0.2082(5) 0.43392(17) 0.0689(10) Uani 1 1 d . . . . .
H5 H 0.312449 0.199214 0.436107 0.083 Uiso 1 1 calc R U . . .
C8 C 0.27880(13) 0.1685(5) 0.22411(16) 0.0609(8) Uani 1 1 d . . . . .
H8A H 0.261452 0.288038 0.213070 0.073 Uiso 1 1 calc R U . . .
H8B H 0.247383 0.092575 0.235672 0.073 Uiso 1 1 calc R U . . .
C32 C 0.96083(15) 0.2402(6) 0.29303(13) 0.0656(9) Uani 1 1 d . . . . .
H32A H 0.999804 0.288126 0.288396 0.098 Uiso 1 1 calc R U . . .
H32B H 0.928885 0.293764 0.263916 0.098 Uiso 1 1 calc R U . . .
H32C H 0.960544 0.110080 0.287919 0.098 Uiso 1 1 calc R U . . .
C3 C 0.45802(19) 0.2345(5) 0.48107(14) 0.0696(10) Uani 1 1 d . . . . .
H3 H 0.487219 0.244353 0.515843 0.084 Uiso 1 1 calc R U . . .
C15 C 0.65874(17) 0.2416(5) 0.15547(17) 0.0682(9) Uani 1 1 d . . . . .
H15 H 0.664081 0.272646 0.117676 0.082 Uiso 1 1 calc R U . . .
C28 C 0.95042(17) 0.3218(4) 0.63567(12) 0.0590(8) Uani 1 1 d . . . . .
H28A H 0.968165 0.434111 0.653764 0.071 Uiso 1 1 calc R U . . .
H28B H 0.970191 0.219505 0.658513 0.071 Uiso 1 1 calc R U . . .
C4 C 0.3961(2) 0.2200(6) 0.48403(17) 0.0802(12) Uani 1 1 d . . . . .
H4 H 0.384235 0.218473 0.520554 0.096 Uiso 1 1 calc R U . . .
C20 C 0.58232(18) 0.2541(6) 0.47287(15) 0.0741(10) Uani 1 1 d . . . . .
H20A H 0.577164 0.364272 0.493955 0.111 Uiso 1 1 calc R U . . .
H20B H 0.621849 0.254861 0.462002 0.111 Uiso 1 1 calc R U . . .
H20C H 0.579348 0.150514 0.497692 0.111 Uiso 1 1 calc R U . . .
O10 O 0.82712(18) 0.7232(7) 0.6683(2) 0.166(2) Uani 1 1 d . . . . .
O12 O 0.8452(2) 0.9611(5) 0.7146(2) 0.1466(17) Uani 1 1 d . . . . .
C19 C 0.80954(15) 0.1394(6) 0.2963(2) 0.0917(14) Uani 1 1 d . . . . .
H19A H 0.819235 0.051353 0.268681 0.138 Uiso 1 1 calc R U . . .
H19B H 0.835694 0.120716 0.334236 0.138 Uiso 1 1 calc R U . . .
H19C H 0.815758 0.260329 0.282466 0.138 Uiso 1 1 calc R U . . .
O11 O 0.8901(2) 0.7320(8) 0.7466(3) 0.191(3) Uani 1 1 d . . . . .
C26 C 1.02253(12) 0.2243(3) 0.50496(12) 0.0403(6) Uani 1 1 d . . . . .
C25 C 1.07974(13) 0.1538(4) 0.49958(14) 0.0502(7) Uani 1 1 d . . . . .
H25 H 1.108475 0.127010 0.533599 0.060 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 O5 1.8277(18) . ?
Ni2 N4 1.837(2) . ?
Ni2 N5 1.891(2) . ?
Ni2 N6 1.921(2) . ?
Ni1 O1 1.8238(18) . ?
Ni1 N1 1.841(2) . ?
Ni1 N2 1.886(2) . ?
Ni1 N3 1.914(2) . ?
O5 C21 1.309(3) . ?
O6 C22 1.368(3) . ?
O6 C32 1.423(3) . ?
O1 C1 1.309(3) . ?
O2 C18 1.349(3) . ?
O2 H2 0.8200 . ?
O3 C2 1.361(4) . ?
O3 C20 1.423(4) . ?
N2 C10 1.466(4) . ?
N2 C9 1.477(4) . ?
N2 H2A 0.9800 . ?
N3 C12 1.270(3) . ?
N3 C11 1.482(3) . ?
N5 C29 1.476(4) . ?
N5 C30 1.477(4) . ?
N5 H5A 0.9800 . ?
N4 C27 1.280(4) . ?
N4 C28 1.474(4) . ?
N6 C31 1.487(4) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
O13 H13A 0.8500 . ?
O13 H13B 0.8498 . ?
O8 N7 1.235(3) . ?
O4 C17 1.354(4) . ?
O4 C19 1.428(4) . ?
O7 N7 1.226(3) . ?
N7 O9 1.210(3) . ?
N1 C7 1.275(4) . ?
N1 C8 1.480(4) . ?
C27 C26 1.431(4) . ?
C27 H27 0.9300 . ?
C12 C13 1.465(4) . ?
C12 H12 0.9300 . ?
C21 C26 1.413(3) . ?
C21 C22 1.426(4) . ?
C22 C23 1.371(4) . ?
N8 O12 1.153(4) . ?
N8 O10 1.160(4) . ?
N8 O11 1.219(5) . ?
C13 C18 1.389(4) . ?
C13 C14 1.414(4) . ?
C18 C17 1.410(4) . ?
C6 C1 1.409(4) . ?
C6 C5 1.411(4) . ?
C6 C7 1.427(5) . ?
C10 C11 1.503(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C23 C24 1.400(4) . ?
C23 H23 0.9300 . ?
C17 C16 1.367(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C9 C8 1.495(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C30 C31 1.505(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C2 C3 1.367(4) . ?
C2 C1 1.420(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C7 H7 0.9300 . ?
C24 C25 1.353(5) . ?
C24 H24 0.9300 . ?
C29 C28 1.506(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C14 C15 1.369(5) . ?
C14 H14 0.9300 . ?
C16 C15 1.376(5) . ?
C16 H16 0.9300 . ?
C5 C4 1.343(5) . ?
C5 H5 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C3 C4 1.396(5) . ?
C3 H3 0.9300 . ?
C15 H15 0.9300 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C4 H4 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C26 C25 1.401(4) . ?
C25 H25 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Ni2 N4 96.56(9) . . ?
O5 Ni2 N5 177.13(9) . . ?
N4 Ni2 N5 86.31(10) . . ?
O5 Ni2 N6 90.50(8) . . ?
N4 Ni2 N6 171.62(10) . . ?
N5 Ni2 N6 86.64(10) . . ?
O1 Ni1 N1 95.75(10) . . ?
O1 Ni1 N2 177.79(9) . . ?
N1 Ni1 N2 86.21(11) . . ?
O1 Ni1 N3 92.02(8) . . ?
N1 Ni1 N3 171.55(10) . . ?
N2 Ni1 N3 86.10(10) . . ?
C21 O5 Ni2 125.63(16) . . ?
C22 O6 C32 118.0(2) . . ?
C1 O1 Ni1 126.78(18) . . ?
C18 O2 H2 109.5 . . ?
C2 O3 C20 117.8(3) . . ?
C10 N2 C9 115.2(2) . . ?
C10 N2 Ni1 107.90(16) . . ?
C9 N2 Ni1 109.52(18) . . ?
C10 N2 H2A 108.0 . . ?
C9 N2 H2A 108.0 . . ?
Ni1 N2 H2A 108.0 . . ?
C12 N3 C11 123.3(2) . . ?
C12 N3 Ni1 124.81(18) . . ?
C11 N3 Ni1 111.83(17) . . ?
C29 N5 C30 116.1(2) . . ?
C29 N5 Ni2 108.26(18) . . ?
C30 N5 Ni2 109.00(17) . . ?
C29 N5 H5A 107.7 . . ?
C30 N5 H5A 107.7 . . ?
Ni2 N5 H5A 107.7 . . ?
C27 N4 C28 119.8(2) . . ?
C27 N4 Ni2 126.21(19) . . ?
C28 N4 Ni2 113.9(2) . . ?
C31 N6 Ni2 110.01(17) . . ?
C31 N6 H6A 109.7 . . ?
Ni2 N6 H6A 109.7 . . ?
C31 N6 H6B 109.7 . . ?
Ni2 N6 H6B 109.7 . . ?
H6A N6 H6B 108.2 . . ?
H13A O13 H13B 104.5 . . ?
C17 O4 C19 119.0(3) . . ?
O9 N7 O7 121.0(3) . . ?
O9 N7 O8 118.5(3) . . ?
O7 N7 O8 120.4(2) . . ?
C7 N1 C8 119.3(3) . . ?
C7 N1 Ni1 126.6(2) . . ?
C8 N1 Ni1 114.1(2) . . ?
N4 C27 C26 125.3(2) . . ?
N4 C27 H27 117.4 . . ?
C26 C27 H27 117.4 . . ?
N3 C12 C13 131.1(2) . . ?
N3 C12 H12 114.4 . . ?
C13 C12 H12 114.4 . . ?
O5 C21 C26 125.3(2) . . ?
O5 C21 C22 117.8(2) . . ?
C26 C21 C22 116.9(2) . . ?
O6 C22 C23 124.9(3) . . ?
O6 C22 C21 113.6(2) . . ?
C23 C22 C21 121.5(2) . . ?
O12 N8 O10 123.8(6) . . ?
O12 N8 O11 116.4(5) . . ?
O10 N8 O11 119.7(5) . . ?
C18 C13 C14 118.2(3) . . ?
C18 C13 C12 115.6(2) . . ?
C14 C13 C12 126.0(3) . . ?
O2 C18 C13 118.7(2) . . ?
O2 C18 C17 120.9(3) . . ?
C13 C18 C17 120.4(3) . . ?
C1 C6 C5 120.1(3) . . ?
C1 C6 C7 121.5(3) . . ?
C5 C6 C7 118.4(3) . . ?
N2 C10 C11 107.3(2) . . ?
N2 C10 H10A 110.3 . . ?
C11 C10 H10A 110.3 . . ?
N2 C10 H10B 110.3 . . ?
C11 C10 H10B 110.3 . . ?
H10A C10 H10B 108.5 . . ?
C22 C23 C24 120.1(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
O4 C17 C16 127.2(3) . . ?
O4 C17 C18 112.9(3) . . ?
C16 C17 C18 119.9(3) . . ?
N3 C11 C10 106.5(2) . . ?
N3 C11 H11A 110.4 . . ?
C10 C11 H11A 110.4 . . ?
N3 C11 H11B 110.4 . . ?
C10 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
N2 C9 C8 106.5(2) . . ?
N2 C9 H9A 110.4 . . ?
C8 C9 H9A 110.4 . . ?
N2 C9 H9B 110.4 . . ?
C8 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
N5 C30 C31 105.8(2) . . ?
N5 C30 H30A 110.6 . . ?
C31 C30 H30A 110.6 . . ?
N5 C30 H30B 110.6 . . ?
C31 C30 H30B 110.6 . . ?
H30A C30 H30B 108.7 . . ?
O3 C2 C3 124.9(3) . . ?
O3 C2 C1 114.3(2) . . ?
C3 C2 C1 120.8(3) . . ?
N6 C31 C30 106.5(2) . . ?
N6 C31 H31A 110.4 . . ?
C30 C31 H31A 110.4 . . ?
N6 C31 H31B 110.4 . . ?
C30 C31 H31B 110.4 . . ?
H31A C31 H31B 108.6 . . ?
O1 C1 C6 124.3(3) . . ?
O1 C1 C2 118.5(3) . . ?
C6 C1 C2 117.2(3) . . ?
N1 C7 C6 125.1(3) . . ?
N1 C7 H7 117.4 . . ?
C6 C7 H7 117.4 . . ?
C25 C24 C23 119.9(3) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
N5 C29 C28 105.7(2) . . ?
N5 C29 H29A 110.6 . . ?
C28 C29 H29A 110.6 . . ?
N5 C29 H29B 110.6 . . ?
C28 C29 H29B 110.6 . . ?
H29A C29 H29B 108.7 . . ?
C15 C14 C13 120.2(3) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C17 C16 C15 120.0(3) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
N1 C8 C9 107.0(2) . . ?
N1 C8 H8A 110.3 . . ?
C9 C8 H8A 110.3 . . ?
N1 C8 H8B 110.3 . . ?
C9 C8 H8B 110.3 . . ?
H8A C8 H8B 108.6 . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C2 C3 C4 121.0(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C14 C15 C16 121.3(3) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
N4 C28 C29 107.0(2) . . ?
N4 C28 H28A 110.3 . . ?
C29 C28 H28A 110.3 . . ?
N4 C28 H28B 110.3 . . ?
C29 C28 H28B 110.3 . . ?
H28A C28 H28B 108.6 . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 C26 C21 120.1(3) . . ?
C25 C26 C27 118.9(2) . . ?
C21 C26 C27 121.0(2) . . ?
C24 C25 C26 121.5(3) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?

_refine_diff_density_max         0.524
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.069

