# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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 2036426'
loop_
_audit_author_name
_audit_author_address
'Shouvik Chattopadhyay' 'Jadavpur University, kolkata'
_audit_update_record             
;
2021-01-20 deposited with the CCDC.	2021-01-22 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            'C27 H44 N10 Ni2 O6'
_chemical_formula_weight         722.14

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                   11.7035(3)
_cell_length_b                   11.3841(3)
_cell_length_c                   25.2520(7)
_cell_angle_alpha                90
_cell_angle_beta                 94.1940(10)
_cell_angle_gamma                90
_cell_volume                     3355.41(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    897
_cell_measurement_theta_min      2.05
_cell_measurement_theta_max      28.91

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_F_000             1520.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    1.176
_shelx_estimated_absorpt_T_min   0.53
_shelx_estimated_absorpt_T_max   0.973
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_T_max  0.775
_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_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25134
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.869
_diffrn_reflns_theta_max         24.817
_diffrn_reflns_theta_full        24.817
_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             5786
_reflns_number_gt                4626
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL, PLATON, WINGX (Ferrugia, 2012)'
_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)+(0.0573P)²+0.1270P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5786
_refine_ls_number_parameters     428
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_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 0.11389(3) 0.57817(3) 0.31700(2) 0.03355(13) Uani 1 1 d . . . . .
Ni2 Ni 0.21141(3) 0.72282(3) 0.41556(2) 0.03121(13) Uani 1 1 d . . . . .
N1 N 0.1302(2) 0.7556(2) 0.33973(10) 0.0383(6) Uani 1 1 d . . . . .
N2 N 0.1300(2) 0.8413(3) 0.31373(11) 0.0482(7) Uani 1 1 d . . . . .
N3 N 0.1285(3) 0.9246(3) 0.28787(18) 0.1035(15) Uani 1 1 d . . . . .
N4 N -0.0534(2) 0.5599(3) 0.34180(12) 0.0525(7) Uani 1 1 d . . . . .
N5 N -0.0828(2) 0.4717(3) 0.36124(12) 0.0552(8) Uani 1 1 d . . . . .
N6 N -0.1141(3) 0.3863(4) 0.38028(18) 0.0967(13) Uani 1 1 d . . . . .
O1 O 0.28956(18) 0.6000(2) 0.29554(9) 0.0501(6) Uani 1 1 d D . . . .
O11 O 0.17789(16) 0.55925(15) 0.39227(7) 0.0324(5) Uani 1 1 d . . . . .
C12 C 0.2163(2) 0.4629(2) 0.41628(11) 0.0300(6) Uani 1 1 d . . . . .
C13 C 0.2743(2) 0.4729(3) 0.46700(12) 0.0377(7) Uani 1 1 d . . . . .
C14 C 0.3091(3) 0.3745(3) 0.49562(13) 0.0499(9) Uani 1 1 d . . . . .
H14 H 0.344894 0.382134 0.529557 0.060 Uiso 1 1 calc R U . . .
C15 C 0.2903(3) 0.2634(3) 0.47334(15) 0.0590(10) Uani 1 1 d . . . . .
H15 H 0.313102 0.196850 0.492698 0.071 Uiso 1 1 calc R U . . .
C16 C 0.2391(3) 0.2516(3) 0.42387(14) 0.0517(9) Uani 1 1 d . . . . .
H16 H 0.228134 0.176866 0.409471 0.062 Uiso 1 1 calc R U . . .
C17 C 0.2022(2) 0.3503(2) 0.39379(12) 0.0366(7) Uani 1 1 d . . . . .
C18 C 0.1515(2) 0.3282(3) 0.34045(13) 0.0400(7) Uani 1 1 d . . . . .
H18 H 0.139651 0.250088 0.330806 0.048 Uiso 1 1 calc R U . . .
N19 N 0.1215(2) 0.4056(2) 0.30556(10) 0.0389(6) Uani 1 1 d . . . . .
C20 C 0.0752(3) 0.3720(3) 0.25239(14) 0.0600(10) Uani 1 1 d . . . . .
H20A H 0.137908 0.352417 0.230878 0.072 Uiso 1 1 calc R U . . .
H20B H 0.027801 0.302632 0.254824 0.072 Uiso 1 1 calc R U . . .
C21 C 0.0096(6) 0.4629(4) 0.22755(19) 0.138(3) Uani 1 1 d . . . . .
H21A H -0.068054 0.455335 0.238224 0.166 Uiso 1 1 calc R U . . .
H21B H 0.006519 0.449331 0.189553 0.166 Uiso 1 1 calc R U . . .
N22 N 0.0455(2) 0.5842(2) 0.23707(10) 0.0485(7) Uani 1 1 d . . . . .
O131 O 0.28973(18) 0.58687(17) 0.48546(8) 0.0431(5) Uani 1 1 d . . . . .
C132 C 0.3614(4) 0.5982(4) 0.53401(19) 0.0932(16) Uani 1 1 d . . . . .
H13A H 0.323303 0.561342 0.562519 0.112 Uiso 1 1 calc R U . . .
H13B H 0.432440 0.556138 0.530220 0.112 Uiso 1 1 calc R U . . .
C133 C 0.3873(4) 0.7145(4) 0.54825(19) 0.0933(15) Uani 1 1 d . . . . .
H13C H 0.425115 0.751918 0.520271 0.140 Uiso 1 1 calc R U . . .
H13D H 0.436829 0.715466 0.580290 0.140 Uiso 1 1 calc R U . . .
H13E H 0.317859 0.755933 0.553958 0.140 Uiso 1 1 calc R U . . .
C221 C 0.1239(4) 0.6228(5) 0.19895(16) 0.1068(18) Uani 1 1 d . . . . .
H22A H 0.086220 0.620209 0.163901 0.160 Uiso 1 1 calc R U . . .
H22B H 0.189574 0.572049 0.200576 0.160 Uiso 1 1 calc R U . . .
H22C H 0.147962 0.701803 0.207061 0.160 Uiso 1 1 calc R U . . .
C222 C -0.0575(4) 0.6587(5) 0.22953(17) 0.1044(17) Uani 1 1 d . . . . .
H22D H -0.034896 0.739360 0.226473 0.157 Uiso 1 1 calc R U . . .
H22E H -0.102906 0.650023 0.259435 0.157 Uiso 1 1 calc R U . . .
H22F H -0.101676 0.635285 0.197755 0.157 Uiso 1 1 calc R U . . .
O31 O 0.36578(16) 0.70746(16) 0.38765(8) 0.0392(5) Uani 1 1 d . . . . .
C32 C 0.4525(3) 0.7789(2) 0.39410(11) 0.0347(7) Uani 1 1 d . . . . .
C33 C 0.5576(3) 0.7450(3) 0.37358(12) 0.0400(8) Uani 1 1 d . . . . .
C34 C 0.6529(3) 0.8165(3) 0.37811(13) 0.0506(9) Uani 1 1 d . . . . .
H34 H 0.720654 0.792620 0.364292 0.061 Uiso 1 1 calc R U . . .
C35 C 0.6469(3) 0.9253(3) 0.40367(14) 0.0540(10) Uani 1 1 d . . . . .
H35 H 0.711088 0.973660 0.406997 0.065 Uiso 1 1 calc R U . . .
C36 C 0.5489(3) 0.9601(3) 0.42339(12) 0.0465(8) Uani 1 1 d . . . . .
H36 H 0.546119 1.032999 0.439905 0.056 Uiso 1 1 calc R U . . .
C37 C 0.4500(3) 0.8889(2) 0.41966(11) 0.0361(7) Uani 1 1 d . . . . .
C38 C 0.3498(3) 0.9331(3) 0.44257(12) 0.0425(8) Uani 1 1 d . . . . .
H38 H 0.356050 1.007054 0.458191 0.051 Uiso 1 1 calc R U . . .
N39 N 0.2524(2) 0.8814(2) 0.44378(10) 0.0394(6) Uani 1 1 d . . . . .
C40 C 0.1607(3) 0.9387(3) 0.47100(15) 0.0555(10) Uani 1 1 d . . . . .
H40A H 0.111286 0.983244 0.445852 0.067 Uiso 1 1 calc R U . . .
H40B H 0.192992 0.991915 0.498099 0.067 Uiso 1 1 calc R U . . .
C41 C 0.0930(3) 0.8423(3) 0.49600(13) 0.0525(9) Uani 1 1 d . . . . .
H41A H 0.139741 0.806571 0.524960 0.063 Uiso 1 1 calc R U . . .
H41B H 0.025682 0.875813 0.510396 0.063 Uiso 1 1 calc R U . . .
N42 N 0.0579(2) 0.7521(2) 0.45626(10) 0.0390(6) Uani 1 1 d . . . . .
O331 O 0.55354(17) 0.6377(2) 0.34898(9) 0.0518(6) Uani 1 1 d . . . . .
C332 C 0.6531(3) 0.5953(3) 0.32681(16) 0.0630(10) Uani 1 1 d . . . . .
H33A H 0.716300 0.591691 0.353865 0.076 Uiso 1 1 calc R U . . .
H33B H 0.674492 0.647455 0.298803 0.076 Uiso 1 1 calc R U . . .
C333 C 0.6279(3) 0.4760(4) 0.30495(17) 0.0814(13) Uani 1 1 d . . . . .
H33C H 0.606903 0.424989 0.332934 0.122 Uiso 1 1 calc R U . . .
H33D H 0.694620 0.445376 0.289802 0.122 Uiso 1 1 calc R U . . .
H33E H 0.565755 0.480509 0.278006 0.122 Uiso 1 1 calc R U . . .
C421 C 0.0197(3) 0.6453(3) 0.48351(14) 0.0573(9) Uani 1 1 d . . . . .
H42D H -0.044426 0.664366 0.503535 0.086 Uiso 1 1 calc R U . . .
H42E H 0.081368 0.616143 0.507051 0.086 Uiso 1 1 calc R U . . .
H42F H -0.002493 0.586349 0.457613 0.086 Uiso 1 1 calc R U . . .
C422 C -0.0403(3) 0.7957(3) 0.42178(14) 0.0556(9) Uani 1 1 d . . . . .
H42A H -0.063724 0.736495 0.396155 0.083 Uiso 1 1 calc R U . . .
H42B H -0.018301 0.865395 0.403726 0.083 Uiso 1 1 calc R U . . .
H42C H -0.102842 0.813447 0.443033 0.083 Uiso 1 1 calc R U . . .
C1S C -0.1224(11) 0.0985(13) 0.3310(5) 0.084(4) Uiso 0.5 1 d . . P A 1
H1S1 H -0.188929 0.139870 0.316455 0.125 Uiso 0.5 1 calc R U P A 1
H1S2 H -0.134823 0.015418 0.327279 0.125 Uiso 0.5 1 calc R U P A 1
H1S3 H -0.057259 0.120766 0.312212 0.125 Uiso 0.5 1 calc R U P A 1
O1S O -0.1045(11) 0.1232(8) 0.3782(4) 0.121(3) Uiso 0.5 1 d . . P A 1
H1S H -0.102442 0.194810 0.381703 0.181 Uiso 0.5 1 calc R U P A 1
O2S O -0.1900(12) 0.1646(12) 0.3690(5) 0.085(3) Uiso 0.25 1 d . . P B 2
H2S H -0.191216 0.230961 0.381515 0.127 Uiso 0.25 1 calc R U P B 2
C2S C -0.142(3) 0.168(3) 0.3201(13) 0.172(15) Uiso 0.25 1 d . . P B 2
H2S1 H -0.165149 0.100146 0.299663 0.258 Uiso 0.25 1 calc R U P B 2
H2S2 H -0.059868 0.169620 0.325703 0.258 Uiso 0.25 1 calc R U P B 2
H2S3 H -0.167480 0.237787 0.301187 0.258 Uiso 0.25 1 calc R U P B 2
O3S O -0.0375(15) 0.1249(16) 0.3779(7) 0.109(5) Uiso 0.25 1 d . . P C 3
H3S H -0.056774 0.194068 0.378641 0.163 Uiso 0.25 1 calc R U P C 3
C3S C -0.079(3) 0.078(2) 0.3345(12) 0.099(9) Uiso 0.25 1 d . . P C 3
H1 H 0.325(4) 0.546(3) 0.2819(19) 0.148 Uiso 1 1 d D U . . .
H2 H 0.329(4) 0.628(4) 0.3220(14) 0.148 Uiso 1 1 d D U . . .
H3S1 H -0.163612 0.053995 0.338570 0.148 Uiso 0.25 1 d . U P D 3
H3S2 H -0.043536 -0.000938 0.328012 0.148 Uiso 0.25 1 d . U P E 3
H3S3 H -0.080997 0.121428 0.303534 0.148 Uiso 0.25 1 d . U P F 3


_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 N19 1.989(2) . ?
Ni1 O11 2.0030(19) . ?
Ni1 N1 2.105(2) . ?
Ni1 N4 2.109(3) . ?
Ni1 N22 2.117(3) . ?
Ni1 O1 2.178(2) . ?
Ni2 O11 1.9833(18) . ?
Ni2 N39 1.986(2) . ?
Ni2 O31 1.9943(19) . ?
Ni2 N1 2.108(3) . ?
Ni2 N42 2.160(2) . ?
Ni2 O131 2.473(2) . ?
N1 N2 1.176(3) . ?
N2 N3 1.151(4) . ?
N4 N5 1.179(4) . ?
N5 N6 1.157(4) . ?
O1 H1 0.832(18) . ?
O1 H2 0.845(19) . ?
O11 C12 1.317(3) . ?
C12 C17 1.406(4) . ?
C12 C13 1.410(4) . ?
C13 C14 1.378(4) . ?
C13 O131 1.386(3) . ?
C14 C15 1.396(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.352(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.407(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.454(4) . ?
C18 N19 1.277(4) . ?
C18 H18 0.9300 . ?
N19 C20 1.461(4) . ?
C20 C21 1.408(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N22 1.458(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
N22 C221 1.446(5) . ?
N22 C222 1.475(5) . ?
O131 C132 1.440(4) . ?
C132 C133 1.399(5) . ?
C132 H13A 0.9700 . ?
C132 H13B 0.9700 . ?
C133 H13C 0.9600 . ?
C133 H13D 0.9600 . ?
C133 H13E 0.9600 . ?
C221 H22A 0.9600 . ?
C221 H22B 0.9600 . ?
C221 H22C 0.9600 . ?
C222 H22D 0.9600 . ?
C222 H22E 0.9600 . ?
C222 H22F 0.9600 . ?
O31 C32 1.302(3) . ?
C32 C37 1.410(4) . ?
C32 C33 1.422(4) . ?
C33 O331 1.370(4) . ?
C33 C34 1.378(4) . ?
C34 C35 1.401(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.344(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.411(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.436(4) . ?
C38 N39 1.286(4) . ?
C38 H38 0.9300 . ?
N39 C40 1.469(4) . ?
C40 C41 1.517(5) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 N42 1.473(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
N42 C422 1.476(4) . ?
N42 C421 1.482(4) . ?
O331 C332 1.415(4) . ?
C332 C333 1.488(5) . ?
C332 H33A 0.9700 . ?
C332 H33B 0.9700 . ?
C333 H33C 0.9600 . ?
C333 H33D 0.9600 . ?
C333 H33E 0.9600 . ?
C421 H42D 0.9600 . ?
C421 H42E 0.9600 . ?
C421 H42F 0.9600 . ?
C422 H42A 0.9600 . ?
C422 H42B 0.9600 . ?
C422 H42C 0.9600 . ?
C1S O1S 1.229(14) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
O1S H1S 0.8200 . ?
O2S C2S 1.39(3) . ?
O2S H2S 0.8200 . ?
C2S H2S1 0.9600 . ?
C2S H2S2 0.9600 . ?
C2S H2S3 0.9600 . ?
O3S C3S 1.29(3) . ?
O3S H3S 0.8200 . ?
C3S H3S1 1.04(3) . ?
C3S H3S2 1.00(3) . ?
C3S H3S3 0.93(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N19 Ni1 O11 90.80(9) . . ?
N19 Ni1 N1 169.61(10) . . ?
O11 Ni1 N1 79.89(9) . . ?
N19 Ni1 N4 89.90(11) . . ?
O11 Ni1 N4 89.91(10) . . ?
N1 Ni1 N4 94.65(11) . . ?
N19 Ni1 N22 84.90(10) . . ?
O11 Ni1 N22 175.67(9) . . ?
N1 Ni1 N22 104.44(10) . . ?
N4 Ni1 N22 89.54(11) . . ?
N19 Ni1 O1 91.34(9) . . ?
O11 Ni1 O1 87.37(8) . . ?
N1 Ni1 O1 83.69(9) . . ?
N4 Ni1 O1 177.03(10) . . ?
N22 Ni1 O1 93.26(10) . . ?
O11 Ni2 O131 71.27(7) . . ?
N39 Ni2 O131 104.20(8) . . ?
O31 Ni2 O131 84.22(8) . . ?
N1 Ni2 O131 151.43(8) . . ?
N42 Ni2 O131 91.99(8) . . ?
O11 Ni2 N39 175.44(9) . . ?
O11 Ni2 O31 88.71(8) . . ?
N39 Ni2 O31 90.30(9) . . ?
O11 Ni2 N1 80.24(9) . . ?
N39 Ni2 N1 104.25(10) . . ?
O31 Ni2 N1 93.14(9) . . ?
O11 Ni2 N42 97.62(9) . . ?
N39 Ni2 N42 82.90(10) . . ?
O31 Ni2 N42 171.19(9) . . ?
N1 Ni2 N42 93.97(10) . . ?
N2 N1 Ni1 130.4(2) . . ?
N2 N1 Ni2 129.5(2) . . ?
Ni1 N1 Ni2 95.95(10) . . ?
N3 N2 N1 179.0(4) . . ?
N5 N4 Ni1 120.8(2) . . ?
N6 N5 N4 178.4(4) . . ?
Ni1 O1 H1 121(4) . . ?
Ni1 O1 H2 108(3) . . ?
H1 O1 H2 111(3) . . ?
C12 O11 Ni2 126.34(17) . . ?
C12 O11 Ni1 128.16(17) . . ?
Ni2 O11 Ni1 103.44(8) . . ?
O11 C12 C17 123.2(3) . . ?
O11 C12 C13 118.5(2) . . ?
C17 C12 C13 118.3(3) . . ?
C14 C13 O131 123.9(3) . . ?
C14 C13 C12 121.0(3) . . ?
O131 C13 C12 115.0(2) . . ?
C13 C14 C15 119.6(3) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 120.6(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 121.1(3) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C12 C17 C16 119.2(3) . . ?
C12 C17 C18 124.0(3) . . ?
C16 C17 C18 116.8(3) . . ?
N19 C18 C17 126.4(3) . . ?
N19 C18 H18 116.8 . . ?
C17 C18 H18 116.8 . . ?
C18 N19 C20 121.2(3) . . ?
C18 N19 Ni1 126.4(2) . . ?
C20 N19 Ni1 112.0(2) . . ?
C21 C20 N19 111.7(3) . . ?
C21 C20 H20A 109.3 . . ?
N19 C20 H20A 109.3 . . ?
C21 C20 H20B 109.3 . . ?
N19 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
C20 C21 N22 118.7(4) . . ?
C20 C21 H21A 107.6 . . ?
N22 C21 H21A 107.6 . . ?
C20 C21 H21B 107.6 . . ?
N22 C21 H21B 107.6 . . ?
H21A C21 H21B 107.1 . . ?
C221 N22 C21 111.6(4) . . ?
C221 N22 C222 106.9(3) . . ?
C21 N22 C222 107.5(4) . . ?
C221 N22 Ni1 115.5(2) . . ?
C21 N22 Ni1 102.2(2) . . ?
C222 N22 Ni1 113.0(2) . . ?
C13 O131 C132 115.1(3) . . ?
C133 C132 O131 113.9(4) . . ?
C133 C132 H13A 108.8 . . ?
O131 C132 H13A 108.8 . . ?
C133 C132 H13B 108.8 . . ?
O131 C132 H13B 108.8 . . ?
H13A C132 H13B 107.7 . . ?
C132 C133 H13C 109.5 . . ?
C132 C133 H13D 109.5 . . ?
H13C C133 H13D 109.5 . . ?
C132 C133 H13E 109.5 . . ?
H13C C133 H13E 109.5 . . ?
H13D C133 H13E 109.5 . . ?
N22 C221 H22A 109.5 . . ?
N22 C221 H22B 109.5 . . ?
H22A C221 H22B 109.5 . . ?
N22 C221 H22C 109.5 . . ?
H22A C221 H22C 109.5 . . ?
H22B C221 H22C 109.5 . . ?
N22 C222 H22D 109.5 . . ?
N22 C222 H22E 109.5 . . ?
H22D C222 H22E 109.5 . . ?
N22 C222 H22F 109.5 . . ?
H22D C222 H22F 109.5 . . ?
H22E C222 H22F 109.5 . . ?
C32 O31 Ni2 128.27(18) . . ?
O31 C32 C37 124.7(3) . . ?
O31 C32 C33 118.2(3) . . ?
C37 C32 C33 117.1(3) . . ?
O331 C33 C34 124.4(3) . . ?
O331 C33 C32 113.9(3) . . ?
C34 C33 C32 121.7(3) . . ?
C33 C34 C35 119.5(3) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C36 C35 C34 120.3(3) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C37 121.6(3) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 H36 119.2 . . ?
C32 C37 C36 119.7(3) . . ?
C32 C37 C38 122.8(3) . . ?
C36 C37 C38 117.5(3) . . ?
N39 C38 C37 126.9(3) . . ?
N39 C38 H38 116.6 . . ?
C37 C38 H38 116.6 . . ?
C38 N39 C40 119.1(3) . . ?
C38 N39 Ni2 126.8(2) . . ?
C40 N39 Ni2 113.9(2) . . ?
N39 C40 C41 107.1(2) . . ?
N39 C40 H40A 110.3 . . ?
C41 C40 H40A 110.3 . . ?
N39 C40 H40B 110.3 . . ?
C41 C40 H40B 110.3 . . ?
H40A C40 H40B 108.5 . . ?
N42 C41 C40 110.4(3) . . ?
N42 C41 H41A 109.6 . . ?
C40 C41 H41A 109.6 . . ?
N42 C41 H41B 109.6 . . ?
C40 C41 H41B 109.6 . . ?
H41A C41 H41B 108.1 . . ?
C41 N42 C422 109.5(2) . . ?
C41 N42 C421 109.5(3) . . ?
C422 N42 C421 107.5(3) . . ?
C41 N42 Ni2 103.35(19) . . ?
C422 N42 Ni2 114.21(19) . . ?
C421 N42 Ni2 112.56(19) . . ?
C33 O331 C332 118.8(3) . . ?
O331 C332 C333 108.1(3) . . ?
O331 C332 H33A 110.1 . . ?
C333 C332 H33A 110.1 . . ?
O331 C332 H33B 110.1 . . ?
C333 C332 H33B 110.1 . . ?
H33A C332 H33B 108.4 . . ?
C332 C333 H33C 109.5 . . ?
C332 C333 H33D 109.5 . . ?
H33C C333 H33D 109.5 . . ?
C332 C333 H33E 109.5 . . ?
H33C C333 H33E 109.5 . . ?
H33D C333 H33E 109.5 . . ?
N42 C421 H42D 109.5 . . ?
N42 C421 H42E 109.5 . . ?
H42D C421 H42E 109.5 . . ?
N42 C421 H42F 109.5 . . ?
H42D C421 H42F 109.5 . . ?
H42E C421 H42F 109.5 . . ?
N42 C422 H42A 109.5 . . ?
N42 C422 H42B 109.5 . . ?
H42A C422 H42B 109.5 . . ?
N42 C422 H42C 109.5 . . ?
H42A C422 H42C 109.5 . . ?
H42B C422 H42C 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C1S O1S H1S 109.5 . . ?
C2S O2S H2S 109.5 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C3S O3S H3S 109.5 . . ?
O3S C3S H3S1 109(2) . . ?
O3S C3S H3S2 112(3) . . ?
H3S1 C3S H3S2 101(3) . . ?
O3S C3S H3S3 119(3) . . ?
H3S1 C3S H3S3 105(3) . . ?
H3S2 C3S H3S3 109(3) . . ?

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
C222 H22E N4 0.96 2.35 3.047(6) 128.7 .
C41 H41A O1S 0.97 2.63 3.193(10) 117.0 3_566
C421 H42E O131 0.96 2.56 3.226(4) 126.7 .
C422 H42A N4 0.96 2.44 3.356(5) 158.9 .
O1S H1S N6 0.82 2.18 2.998(10) 171.5 .
O2S H2S N6 0.82 1.99 2.684(14) 142.5 .
O3S H3S N6 0.82 2.29 3.110(19) 178.9 .
O1 H1 N3 0.832(18) 2.33(3) 3.105(4) 155(5) 2_545
O1 H2 O31 0.845(19) 1.91(2) 2.720(3) 160(5) .
C3S H3S2 N3 1.00(3) 2.469(5) 3.28(3) 137.1(18) 1_545

_refine_diff_density_max         0.725
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.062



####################################################################### 
# 
# 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 2049044'
loop_
_audit_author_name
_audit_author_address
'Shouvik Chattopadhyay' 'Jadavpur University, kolkata'
_audit_update_record             
;
2021-01-20 deposited with the CCDC.	2021-01-22 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            'C26 H40 N10 Ni2 O5'
_chemical_formula_weight         690.10

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

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

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

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

_cell_length_a                   11.5492(4)
_cell_length_b                   12.4240(3)
_cell_length_c                   21.6851(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3111.54(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10054
_cell_measurement_theta_min      3.41
_cell_measurement_theta_max      25.00
_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_F_000             1448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    1.263
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_T_max  1.000

_diffrn_ambient_temperature      150(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       'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            10054
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.41
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             5144
_reflns_number_gt                4990
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.781
_reflns_Friedel_fraction_max     0.974
_reflns_Friedel_fraction_full    0.974

_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       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL, PLATON, WINGX (Ferrugia, 2012)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0238P)²+0.1817P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.062(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5144
_refine_ls_number_parameters     405
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0560
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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
Ni2 Ni 0.13843(4) 0.88981(3) 0.16417(2) 0.01153(12) Uani 1 1 d . . . . .
Ni1 Ni 0.18140(4) 0.75538(3) 0.04233(2) 0.01136(12) Uani 1 1 d . . . . .
N4 N 0.3433(3) 0.6905(2) 0.06280(13) 0.0151(7) Uani 1 1 d . . . . .
N5 N 0.3732(3) 0.6649(2) 0.11380(14) 0.0168(7) Uani 1 1 d . . . . .
N6 N 0.4049(3) 0.6401(3) 0.16227(17) 0.0287(8) Uani 1 1 d . . . . .
N1 N 0.1200(3) 0.7277(2) 0.13631(13) 0.0133(7) Uani 1 1 d . . . . .
N2 N 0.0318(3) 0.6807(2) 0.14861(13) 0.0145(7) Uani 1 1 d . . . . .
N3 N -0.0519(3) 0.6338(2) 0.16099(16) 0.0233(8) Uani 1 1 d . . . . .
O11 O 0.2239(2) 0.89707(18) 0.08382(10) 0.0122(5) Uani 1 1 d . . . . .
C12 C 0.2292(3) 0.9920(3) 0.05719(16) 0.0121(8) Uani 1 1 d . . . . .
C17 C 0.2435(3) 1.0078(3) -0.00674(17) 0.0128(8) Uani 1 1 d . . . . .
C16 C 0.2484(3) 1.1132(3) -0.02989(16) 0.0178(8) Uani 1 1 d . . . . .
H16 H 0.259316 1.123499 -0.071969 0.021 Uiso 1 1 calc R U . . .
C15 C 0.2376(4) 1.2012(3) 0.00743(18) 0.0196(9) Uani 1 1 d . . . . .
H15 H 0.240757 1.270141 -0.009171 0.024 Uiso 1 1 calc R U . . .
C14 C 0.2217(4) 1.1867(3) 0.07083(17) 0.0166(9) Uani 1 1 d . . . . .
H14 H 0.214035 1.246172 0.096557 0.020 Uiso 1 1 calc R U . . .
C13 C 0.2173(3) 1.0850(3) 0.09499(17) 0.0137(8) Uani 1 1 d . . . . .
C18 C 0.2458(3) 0.9201(3) -0.05111(17) 0.0156(8) Uani 1 1 d . . . . .
H18 H 0.258393 0.938274 -0.092160 0.019 Uiso 1 1 calc R U . . .
O131 O 0.1970(2) 1.06105(17) 0.15664(11) 0.0147(6) Uani 1 1 d . . . . .
C132 C 0.1567(4) 1.1466(3) 0.19650(17) 0.0191(9) Uani 1 1 d . . . . .
H13B H 0.111249 1.115888 0.229726 0.023 Uiso 1 1 calc R U . . .
H13A H 0.106895 1.194424 0.173146 0.023 Uiso 1 1 calc R U . . .
C133 C 0.2554(4) 1.2105(3) 0.22345(19) 0.0264(10) Uani 1 1 d . . . . .
H13C H 0.306835 1.162926 0.245036 0.040 Uiso 1 1 calc R U . . .
H13D H 0.225364 1.263201 0.251590 0.040 Uiso 1 1 calc R U . . .
H13E H 0.296732 1.246004 0.190890 0.040 Uiso 1 1 calc R U . . .
N19 N 0.2321(3) 0.8206(2) -0.03894(14) 0.0139(7) Uani 1 1 d . . . . .
C20 C 0.2282(3) 0.7418(3) -0.08962(16) 0.0174(8) Uani 1 1 d . . . . .
H20A H 0.300766 0.702612 -0.091902 0.021 Uiso 1 1 calc R U . . .
H20B H 0.215778 0.778152 -0.128632 0.021 Uiso 1 1 calc R U . . .
C21 C 0.1299(4) 0.6655(3) -0.07659(16) 0.0166(8) Uani 1 1 d . . . . .
H21A H 0.056659 0.703283 -0.079731 0.020 Uiso 1 1 calc R U . . .
H21B H 0.130038 0.607584 -0.106618 0.020 Uiso 1 1 calc R U . . .
N22 N 0.1436(3) 0.6206(2) -0.01361(13) 0.0144(7) Uani 1 1 d D . . . .
H22 H 0.208(2) 0.582(3) -0.0116(18) 0.017 Uiso 1 1 d D U . . .
C221 C 0.0468(4) 0.5483(3) 0.00338(19) 0.0235(10) Uani 1 1 d . . . . .
H22A H 0.023620 0.506719 -0.032397 0.028 Uiso 1 1 calc R U . . .
H22B H -0.019019 0.591045 0.016496 0.028 Uiso 1 1 calc R U . . .
C222 C 0.0817(4) 0.4729(3) 0.0547(2) 0.0303(11) Uani 1 1 d . . . . .
H22C H 0.136395 0.421331 0.039297 0.045 Uiso 1 1 calc R U . . .
H22D H 0.014406 0.436002 0.069866 0.045 Uiso 1 1 calc R U . . .
H22E H 0.116335 0.513388 0.087571 0.045 Uiso 1 1 calc R U . . .
O31 O -0.0075(2) 0.94129(18) 0.12255(11) 0.0138(6) Uani 1 1 d . . . . .
C32 C -0.0947(3) 0.9911(3) 0.14762(17) 0.0134(8) Uani 1 1 d . . . . .
C37 C -0.1186(3) 0.9910(3) 0.21205(17) 0.0142(8) Uani 1 1 d . . . . .
C36 C -0.2185(3) 1.0422(3) 0.23517(17) 0.0169(9) Uani 1 1 d . . . . .
H36 H -0.232791 1.040959 0.277372 0.020 Uiso 1 1 calc R U . . .
C35 C -0.2950(3) 1.0937(3) 0.19714(18) 0.0179(9) Uani 1 1 d . . . . .
H35 H -0.360951 1.126471 0.213054 0.021 Uiso 1 1 calc R U . . .
C34 C -0.2719(3) 1.0962(3) 0.13350(18) 0.0174(9) Uani 1 1 d . . . . .
H34 H -0.322819 1.131567 0.107177 0.021 Uiso 1 1 calc R U . . .
C33 C -0.1750(3) 1.0471(3) 0.10960(16) 0.0143(8) Uani 1 1 d . . . . .
C38 C -0.0444(3) 0.9366(3) 0.25609(18) 0.0151(9) Uani 1 1 d . . . . .
H38 H -0.069198 0.934708 0.296874 0.018 Uiso 1 1 calc R U . . .
O331 O -0.1626(2) 1.04429(17) 0.04578(12) 0.0165(6) Uani 1 1 d . . . . .
C332 C -0.0615(3) 1.1007(3) 0.02213(17) 0.0202(9) Uani 1 1 d . . . . .
H33A H 0.008550 1.071216 0.040122 0.024 Uiso 1 1 calc R U . . .
H33B H -0.065840 1.176565 0.032342 0.024 Uiso 1 1 calc R U . . .
C333 C -0.0605(4) 1.0857(3) -0.04699(18) 0.0244(9) Uani 1 1 d . . . . .
H33D H -0.046394 1.011433 -0.056532 0.037 Uiso 1 1 calc R U . . .
H33E H -0.000396 1.129293 -0.064685 0.037 Uiso 1 1 calc R U . . .
H33C H -0.133989 1.107015 -0.063677 0.037 Uiso 1 1 calc R U . . .
N39 N 0.0521(3) 0.8910(2) 0.24383(13) 0.0139(7) Uani 1 1 d . . . . .
C40 C 0.1203(3) 0.8414(3) 0.29308(16) 0.0174(9) Uani 1 1 d . . . . .
H40A H 0.114251 0.763590 0.290839 0.021 Uiso 1 1 calc R U . . .
H40B H 0.091831 0.864576 0.333014 0.021 Uiso 1 1 calc R U . . .
C41 C 0.2447(3) 0.8758(3) 0.28478(17) 0.0167(8) Uani 1 1 d . . . . .
H41A H 0.252180 0.952140 0.293302 0.020 Uiso 1 1 calc R U . . .
H41B H 0.293814 0.836924 0.313437 0.020 Uiso 1 1 calc R U . . .
N42 N 0.2817(3) 0.8532(2) 0.22072(14) 0.0137(7) Uani 1 1 d D . . . .
H42 H 0.290(3) 0.7872(19) 0.2165(18) 0.016 Uiso 1 1 d D U . . .
C421 C 0.3942(3) 0.9020(3) 0.20441(18) 0.0199(9) Uani 1 1 d . . . . .
H42A H 0.387130 0.979612 0.207299 0.024 Uiso 1 1 calc R U . . .
H42B H 0.411563 0.884495 0.161812 0.024 Uiso 1 1 calc R U . . .
C422 C 0.4951(4) 0.8663(3) 0.2443(2) 0.0293(10) Uani 1 1 d . . . . .
H42C H 0.483076 0.890254 0.285891 0.044 Uiso 1 1 calc R U . . .
H42D H 0.565566 0.896806 0.228602 0.044 Uiso 1 1 calc R U . . .
H42E H 0.500575 0.789179 0.243631 0.044 Uiso 1 1 calc R U . . .
O1 O 0.0127(2) 0.8118(2) 0.02766(12) 0.0216(7) Uani 1 1 d D . . . .
H1 H 0.002(4) 0.863(3) 0.0528(14) 0.026 Uiso 1 1 d D U . . .
H2 H -0.032(3) 0.818(3) -0.0042(13) 0.026 Uiso 1 1 d D 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 N39 1.994(3) . ?
Ni2 O11 2.005(2) . ?
Ni2 O31 2.016(3) . ?
Ni2 N42 2.109(3) . ?
Ni2 N1 2.113(3) . ?
Ni2 O131 2.238(2) . ?
Ni1 N19 2.026(3) . ?
Ni1 O11 2.037(2) . ?
Ni1 N4 2.084(3) . ?
Ni1 O1 2.094(3) . ?
Ni1 N22 2.113(3) . ?
Ni1 N1 2.185(3) . ?
N4 N5 1.201(4) . ?
N5 N6 1.155(4) . ?
N1 N2 1.205(4) . ?
N2 N3 1.160(4) . ?
O11 C12 1.314(4) . ?
C12 C17 1.410(5) . ?
C12 C13 1.424(5) . ?
C17 C16 1.404(5) . ?
C17 C18 1.454(5) . ?
C16 C15 1.365(5) . ?
C16 H16 0.9300 . ?
C15 C14 1.399(5) . ?
C15 H15 0.9300 . ?
C14 C13 1.368(5) . ?
C14 H14 0.9300 . ?
C13 O131 1.390(4) . ?
C18 N19 1.274(4) . ?
C18 H18 0.9300 . ?
O131 C132 1.447(4) . ?
C132 C133 1.506(5) . ?
C132 H13B 0.9700 . ?
C132 H13A 0.9700 . ?
C133 H13C 0.9600 . ?
C133 H13D 0.9600 . ?
C133 H13E 0.9600 . ?
N19 C20 1.473(4) . ?
C20 C21 1.506(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N22 1.483(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
N22 C221 1.480(5) . ?
N22 H22 0.89(2) . ?
C221 C222 1.509(6) . ?
C221 H22A 0.9700 . ?
C221 H22B 0.9700 . ?
C222 H22C 0.9600 . ?
C222 H22D 0.9600 . ?
C222 H22E 0.9600 . ?
O31 C32 1.301(4) . ?
C32 C33 1.423(5) . ?
C32 C37 1.424(5) . ?
C37 C36 1.410(5) . ?
C37 C38 1.450(5) . ?
C36 C35 1.367(5) . ?
C36 H36 0.9300 . ?
C35 C34 1.406(5) . ?
C35 H35 0.9300 . ?
C34 C33 1.376(5) . ?
C34 H34 0.9300 . ?
C33 O331 1.392(4) . ?
C38 N39 1.278(4) . ?
C38 H38 0.9300 . ?
O331 C332 1.455(4) . ?
C332 C333 1.510(5) . ?
C332 H33A 0.9700 . ?
C332 H33B 0.9700 . ?
C333 H33D 0.9600 . ?
C333 H33E 0.9600 . ?
C333 H33C 0.9600 . ?
N39 C40 1.463(5) . ?
C40 C41 1.511(5) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 N42 1.480(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
N42 C421 1.477(5) . ?
N42 H42 0.83(2) . ?
C421 C422 1.518(6) . ?
C421 H42A 0.9700 . ?
C421 H42B 0.9700 . ?
C422 H42C 0.9600 . ?
C422 H42D 0.9600 . ?
C422 H42E 0.9600 . ?
O1 H1 0.84(2) . ?
O1 H2 0.87(2) . ?

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
N39 Ni2 O11 176.98(11) . . ?
N39 Ni2 O31 88.16(11) . . ?
O11 Ni2 O31 90.48(10) . . ?
N39 Ni2 N42 83.67(12) . . ?
O11 Ni2 N42 97.40(11) . . ?
O31 Ni2 N42 169.91(11) . . ?
N39 Ni2 N1 101.78(12) . . ?
O11 Ni2 N1 81.03(10) . . ?
O31 Ni2 N1 95.17(11) . . ?
N42 Ni2 N1 92.29(11) . . ?
N39 Ni2 O131 101.96(10) . . ?
O11 Ni2 O131 75.23(9) . . ?
O31 Ni2 O131 85.31(9) . . ?
N42 Ni2 O131 90.58(10) . . ?
N1 Ni2 O131 156.26(10) . . ?
N19 Ni1 O11 88.22(10) . . ?
N19 Ni1 N4 94.62(12) . . ?
O11 Ni1 N4 91.36(10) . . ?
N19 Ni1 O1 90.16(12) . . ?
O11 Ni1 O1 90.14(10) . . ?
N4 Ni1 O1 175.03(11) . . ?
N19 Ni1 N22 82.94(11) . . ?
O11 Ni1 N22 171.14(10) . . ?
N4 Ni1 N22 90.08(12) . . ?
O1 Ni1 N22 89.16(12) . . ?
N19 Ni1 N1 165.47(10) . . ?
O11 Ni1 N1 78.60(10) . . ?
N4 Ni1 N1 91.83(11) . . ?
O1 Ni1 N1 83.82(11) . . ?
N22 Ni1 N1 110.10(11) . . ?
N5 N4 Ni1 123.8(3) . . ?
N6 N5 N4 178.1(4) . . ?
N2 N1 Ni2 119.0(2) . . ?
N2 N1 Ni1 123.9(2) . . ?
Ni2 N1 Ni1 94.82(11) . . ?
N3 N2 N1 178.7(4) . . ?
C12 O11 Ni2 116.4(2) . . ?
C12 O11 Ni1 126.3(2) . . ?
Ni2 O11 Ni1 103.07(10) . . ?
O11 C12 C17 124.3(3) . . ?
O11 C12 C13 118.1(3) . . ?
C17 C12 C13 117.6(3) . . ?
C16 C17 C12 119.1(3) . . ?
C16 C17 C18 117.5(3) . . ?
C12 C17 C18 123.2(3) . . ?
C15 C16 C17 122.1(3) . . ?
C15 C16 H16 119.0 . . ?
C17 C16 H16 119.0 . . ?
C16 C15 C14 119.5(3) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C13 C14 C15 120.0(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C13 O131 124.9(3) . . ?
C14 C13 C12 121.7(3) . . ?
O131 C13 C12 113.3(3) . . ?
N19 C18 C17 126.0(3) . . ?
N19 C18 H18 117.0 . . ?
C17 C18 H18 117.0 . . ?
C13 O131 C132 118.1(3) . . ?
C13 O131 Ni2 108.97(19) . . ?
C132 O131 Ni2 123.9(2) . . ?
O131 C132 C133 112.1(3) . . ?
O131 C132 H13B 109.2 . . ?
C133 C132 H13B 109.2 . . ?
O131 C132 H13A 109.2 . . ?
C133 C132 H13A 109.2 . . ?
H13B C132 H13A 107.9 . . ?
C132 C133 H13C 109.5 . . ?
C132 C133 H13D 109.5 . . ?
H13C C133 H13D 109.5 . . ?
C132 C133 H13E 109.5 . . ?
H13C C133 H13E 109.5 . . ?
H13D C133 H13E 109.5 . . ?
C18 N19 C20 119.6(3) . . ?
C18 N19 Ni1 127.2(3) . . ?
C20 N19 Ni1 112.0(2) . . ?
N19 C20 C21 107.5(3) . . ?
N19 C20 H20A 110.2 . . ?
C21 C20 H20A 110.2 . . ?
N19 C20 H20B 110.2 . . ?
C21 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
N22 C21 C20 109.2(3) . . ?
N22 C21 H21A 109.8 . . ?
C20 C21 H21A 109.8 . . ?
N22 C21 H21B 109.8 . . ?
C20 C21 H21B 109.8 . . ?
H21A C21 H21B 108.3 . . ?
C221 N22 C21 112.1(3) . . ?
C221 N22 Ni1 119.6(2) . . ?
C21 N22 Ni1 104.6(2) . . ?
C221 N22 H22 107(2) . . ?
C21 N22 H22 110(3) . . ?
Ni1 N22 H22 103(2) . . ?
N22 C221 C222 111.0(3) . . ?
N22 C221 H22A 109.4 . . ?
C222 C221 H22A 109.4 . . ?
N22 C221 H22B 109.4 . . ?
C222 C221 H22B 109.4 . . ?
H22A C221 H22B 108.0 . . ?
C221 C222 H22C 109.5 . . ?
C221 C222 H22D 109.5 . . ?
H22C C222 H22D 109.5 . . ?
C221 C222 H22E 109.5 . . ?
H22C C222 H22E 109.5 . . ?
H22D C222 H22E 109.5 . . ?
C32 O31 Ni2 127.6(2) . . ?
O31 C32 C33 119.7(3) . . ?
O31 C32 C37 124.1(3) . . ?
C33 C32 C37 116.2(3) . . ?
C36 C37 C32 120.5(3) . . ?
C36 C37 C38 117.4(3) . . ?
C32 C37 C38 122.1(3) . . ?
C35 C36 C37 121.7(4) . . ?
C35 C36 H36 119.1 . . ?
C37 C36 H36 119.1 . . ?
C36 C35 C34 118.7(4) . . ?
C36 C35 H35 120.7 . . ?
C34 C35 H35 120.7 . . ?
C33 C34 C35 120.9(4) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 H34 119.5 . . ?
C34 C33 O331 118.0(3) . . ?
C34 C33 C32 121.9(3) . . ?
O331 C33 C32 119.8(3) . . ?
N39 C38 C37 125.8(3) . . ?
N39 C38 H38 117.1 . . ?
C37 C38 H38 117.1 . . ?
C33 O331 C332 114.9(3) . . ?
O331 C332 C333 107.3(3) . . ?
O331 C332 H33A 110.3 . . ?
C333 C332 H33A 110.3 . . ?
O331 C332 H33B 110.3 . . ?
C333 C332 H33B 110.3 . . ?
H33A C332 H33B 108.5 . . ?
C332 C333 H33D 109.5 . . ?
C332 C333 H33E 109.5 . . ?
H33D C333 H33E 109.5 . . ?
C332 C333 H33C 109.5 . . ?
H33D C333 H33C 109.5 . . ?
H33E C333 H33C 109.5 . . ?
C38 N39 C40 120.3(3) . . ?
C38 N39 Ni2 128.2(3) . . ?
C40 N39 Ni2 111.1(2) . . ?
N39 C40 C41 107.8(3) . . ?
N39 C40 H40A 110.1 . . ?
C41 C40 H40A 110.1 . . ?
N39 C40 H40B 110.1 . . ?
C41 C40 H40B 110.1 . . ?
H40A C40 H40B 108.5 . . ?
N42 C41 C40 109.4(3) . . ?
N42 C41 H41A 109.8 . . ?
C40 C41 H41A 109.8 . . ?
N42 C41 H41B 109.8 . . ?
C40 C41 H41B 109.8 . . ?
H41A C41 H41B 108.2 . . ?
C421 N42 C41 113.6(3) . . ?
C421 N42 Ni2 117.6(2) . . ?
C41 N42 Ni2 106.2(2) . . ?
C421 N42 H42 106(3) . . ?
C41 N42 H42 109(3) . . ?
Ni2 N42 H42 104(3) . . ?
N42 C421 C422 114.8(3) . . ?
N42 C421 H42A 108.6 . . ?
C422 C421 H42A 108.6 . . ?
N42 C421 H42B 108.6 . . ?
C422 C421 H42B 108.6 . . ?
H42A C421 H42B 107.5 . . ?
C421 C422 H42C 109.5 . . ?
C421 C422 H42D 109.5 . . ?
H42C C422 H42D 109.5 . . ?
C421 C422 H42E 109.5 . . ?
H42C C422 H42E 109.5 . . ?
H42D C422 H42E 109.5 . . ?
Ni1 O1 H1 107(3) . . ?
Ni1 O1 H2 135(3) . . ?
H1 O1 H2 111(3) . . ?

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
N22 H22 O331 0.89(2) 2.29(3) 3.114(4) 155(3) 4_565
N42 H42 N6 0.83(2) 2.55(3) 3.263(4) 145(3) .
O1 H1 O31 0.84(2) 1.80(2) 2.623(3) 163(4) .
O1 H2 N4 0.87(2) 1.92(2) 2.771(4) 165(4) 4_465

_refine_diff_density_max         0.318
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.050



