# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1425683'
loop_
_audit_author_name
_audit_author_address
'Bipul Sarma'
;Tezpur University
India
;
_audit_update_record             
;
2019-07-01 deposited with the CCDC.	2019-08-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H21 N7 Ni O5 S2'
_chemical_formula_weight         622.32

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'
S S 0.1246 0.1234 '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                   10.3308(2)
_cell_length_b                   11.4554(3)
_cell_length_c                   23.6689(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2801.06(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4617
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      25.99

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    0.890
_shelx_estimated_absorpt_T_min   0.764
_shelx_estimated_absorpt_T_max   0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7638
_exptl_absorpt_correction_T_max  0.8282
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13706
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.721
_diffrn_reflns_theta_max         27.710
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.950
_reflns_number_total             6128
_reflns_number_gt                5280
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.686
_reflns_Friedel_fraction_max     0.869
_reflns_Friedel_fraction_full    0.892

_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    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2008 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and  goodness of fit S are based on F², conventional R-factors R are based  on F, with F set to zero for negative F². The threshold expression of  F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is  not relevant to the choice of reflections for refinement.  R-factors based  on F² are statistically about twice as large as those based on F, and R-  factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0708P)²] 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 
;
 Flack x determined using 1819 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6128
_refine_ls_number_parameters     371
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1348
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.005
_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
H3A H 1.068(8) 0.672(4) 0.193(4) 0.07(3) Uiso 1 1 d D . . . .
H5A H 0.704(19) 0.141(14) 0.057(10) 0.35(13) Uiso 1 1 d D . . . .
Ni1 Ni 0.86615(7) 0.42687(6) 0.12761(3) 0.01568(18) Uani 1 1 d . . . . .
S1 S 0.91835(16) 0.53747(14) -0.06280(6) 0.0265(4) Uani 1 1 d . . . . .
S2 S 0.78004(15) 0.35036(15) 0.32150(6) 0.0259(4) Uani 1 1 d . . . . .
O2 O 0.9432(4) 0.2038(4) 0.11844(16) 0.0223(9) Uani 1 1 d . . . . .
O3 O 0.7945(4) 0.8615(4) 0.45252(17) 0.0307(11) Uani 1 1 d . . . . .
O1 O 1.0751(4) 0.4110(3) 0.16195(16) 0.0195(8) Uani 1 1 d . . . . .
N1 N 0.7069(4) 0.5252(4) 0.11611(17) 0.0150(9) Uani 1 1 d . . . . .
N4 N 0.7313(4) 0.3131(4) 0.08497(18) 0.0168(10) Uani 1 1 d . . . . .
N7 N 0.8094(5) 0.3741(4) 0.2045(2) 0.0212(11) Uani 1 1 d . . . . .
N6 N 0.9388(4) 0.4634(4) 0.05006(19) 0.0196(10) Uani 1 1 d . . . . .
N2 N 0.9176(4) 0.5882(4) 0.16123(19) 0.0174(10) Uani 1 1 d . . . . .
C1 C 0.8701(6) 0.1506(5) 0.0867(2) 0.0174(11) Uani 1 1 d . . . . .
C15 C 0.7062(5) 0.6332(5) 0.1368(2) 0.0157(11) Uani 1 1 d . . . . .
C9 C 0.6196(5) 0.3570(5) 0.0716(2) 0.0171(11) Uani 1 1 d . . . . .
N3 N 1.0381(4) 0.6011(4) 0.1843(2) 0.0175(10) Uani 1 1 d D . . . .
C22 C 1.3669(6) 0.5837(6) 0.2929(2) 0.0277(13) Uani 1 1 d . . . . .
H22 H 1.3775 0.6340 0.3233 0.033 Uiso 1 1 calc R U . . .
C17 C 0.8535(6) 0.7887(5) 0.1868(2) 0.0230(13) Uani 1 1 d . . . . .
H17A H 0.8802 0.7811 0.2255 0.035 Uiso 1 1 calc R U . . .
H17B H 0.7742 0.8323 0.1851 0.035 Uiso 1 1 calc R U . . .
H17C H 0.9193 0.8289 0.1658 0.035 Uiso 1 1 calc R U . . .
C7 C 0.7943(6) -0.0479(5) 0.0527(2) 0.0233(13) Uani 1 1 d . . . . .
H7 H 0.7087 -0.0226 0.0534 0.028 Uiso 1 1 calc R U . . .
C3 C 1.0219(6) -0.0108(5) 0.0672(2) 0.0226(13) Uani 1 1 d . . . . .
H3 H 1.0885 0.0393 0.0777 0.027 Uiso 1 1 calc R U . . .
N5 N 0.7582(4) 0.2005(4) 0.0666(2) 0.0167(10) Uani 1 1 d D . . . .
C19 C 1.1121(5) 0.5008(5) 0.1852(2) 0.0181(12) Uani 1 1 d . . . . .
C16 C 0.8330(5) 0.6713(5) 0.1623(2) 0.0168(12) Uani 1 1 d . . . . .
C14 C 0.5934(5) 0.7019(5) 0.1350(2) 0.0221(12) Uani 1 1 d . . . . .
H14 H 0.5924 0.7771 0.1498 0.027 Uiso 1 1 calc R U . . .
C11 C 0.6020(5) 0.4792(5) 0.0922(2) 0.0168(11) Uani 1 1 d . . . . .
C20 C 1.2358(5) 0.5083(5) 0.2171(2) 0.0167(11) Uani 1 1 d . . . . .
C12 C 0.4868(5) 0.5426(5) 0.0885(2) 0.0204(12) Uani 1 1 d . . . . .
H12 H 0.4137 0.5106 0.0716 0.025 Uiso 1 1 calc R U . . .
C2 C 0.8939(5) 0.0288(5) 0.0679(2) 0.0170(11) Uani 1 1 d . . . . .
C25 C 1.3359(5) 0.4321(5) 0.2032(2) 0.0197(12) Uani 1 1 d . . . . .
H25 H 1.3251 0.3797 0.1735 0.024 Uiso 1 1 calc R U . . .
C21 C 1.2506(5) 0.5845(6) 0.2628(2) 0.0235(13) Uani 1 1 d . . . . .
H21 H 1.1840 0.6349 0.2731 0.028 Uiso 1 1 calc R U . . .
C24 C 1.4516(5) 0.4337(6) 0.2330(2) 0.0248(13) Uani 1 1 d . . . . .
H24 H 1.5190 0.3842 0.2228 0.030 Uiso 1 1 calc R U . . .
C13 C 0.4845(6) 0.6542(5) 0.1106(2) 0.0241(13) Uani 1 1 d . . . . .
H13 H 0.4086 0.6976 0.1090 0.029 Uiso 1 1 calc R U . . .
C4 C 1.0504(7) -0.1248(6) 0.0509(3) 0.0296(15) Uani 1 1 d . . . . .
H4 H 1.1356 -0.1507 0.0502 0.035 Uiso 1 1 calc R U . . .
C5 C 0.9503(7) -0.1991(6) 0.0358(3) 0.0342(16) Uani 1 1 d . . . . .
H5 H 0.9684 -0.2754 0.0250 0.041 Uiso 1 1 calc R U . . .
C10 C 0.5189(6) 0.2946(6) 0.0394(3) 0.0260(14) Uani 1 1 d . . . . .
H10A H 0.5422 0.2927 0.0002 0.039 Uiso 1 1 calc R U . . .
H10B H 0.4375 0.3341 0.0438 0.039 Uiso 1 1 calc R U . . .
H10C H 0.5113 0.2162 0.0534 0.039 Uiso 1 1 calc R U . . .
C6 C 0.8226(7) -0.1600(6) 0.0369(2) 0.0280(14) Uani 1 1 d . . . . .
H6 H 0.7560 -0.2104 0.0267 0.034 Uiso 1 1 calc R U . . .
C23 C 1.4658(6) 0.5096(6) 0.2781(3) 0.0296(15) Uani 1 1 d . . . . .
H23 H 1.5427 0.5104 0.2985 0.036 Uiso 1 1 calc R U . . .
C27 C 0.7967(5) 0.3646(5) 0.2524(2) 0.0189(12) Uani 1 1 d . . . . .
C26 C 0.9288(5) 0.4943(5) 0.0026(2) 0.0179(12) Uani 1 1 d . . . . .
O4 O 0.7100(7) 0.6944(5) 0.3765(2) 0.0633(17) Uani 1 1 d . . . . .
O5 O 0.1168(7) 0.1266(6) 0.1994(3) 0.0721(19) 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 N7 2.006(5) . ?
Ni1 N1 2.013(4) . ?
Ni1 N6 2.027(5) . ?
Ni1 N2 2.081(5) . ?
Ni1 N4 2.158(5) . ?
Ni1 O1 2.314(4) . ?
S1 C26 1.629(6) . ?
S2 C27 1.652(6) . ?
O2 C1 1.227(6) . ?
O1 C19 1.228(6) . ?
N1 C15 1.329(7) . ?
N1 C11 1.331(7) . ?
N4 C9 1.299(7) . ?
N4 N5 1.389(6) . ?
N7 C27 1.147(7) . ?
N6 C26 1.182(7) . ?
N2 C16 1.293(7) . ?
N2 N3 1.367(6) . ?
C1 N5 1.375(7) . ?
C1 C2 1.485(7) . ?
C15 C14 1.406(7) . ?
C15 C16 1.507(7) . ?
C9 C10 1.475(8) . ?
C9 C11 1.493(8) . ?
N3 C19 1.380(7) . ?
N3 H3A 0.89(3) . ?
C22 C23 1.374(9) . ?
C22 C21 1.396(8) . ?
C22 H22 0.9300 . ?
C17 C16 1.481(8) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C7 C6 1.369(8) . ?
C7 C2 1.400(8) . ?
C7 H7 0.9300 . ?
C3 C4 1.392(8) . ?
C3 C2 1.398(7) . ?
C3 H3 0.9300 . ?
N5 H5A 0.92(3) . ?
C19 C20 1.487(7) . ?
C14 C13 1.377(8) . ?
C14 H14 0.9300 . ?
C11 C12 1.397(8) . ?
C20 C25 1.393(8) . ?
C20 C21 1.398(8) . ?
C12 C13 1.381(8) . ?
C12 H12 0.9300 . ?
C25 C24 1.388(7) . ?
C25 H25 0.9300 . ?
C21 H21 0.9300 . ?
C24 C23 1.384(8) . ?
C24 H24 0.9300 . ?
C13 H13 0.9300 . ?
C4 C5 1.387(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(9) . ?
C5 H5 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C6 H6 0.9300 . ?
C23 H23 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
N7 Ni1 N1 93.02(18) . . ?
N7 Ni1 N6 172.9(2) . . ?
N1 Ni1 N6 93.72(18) . . ?
N7 Ni1 N2 89.73(19) . . ?
N1 Ni1 N2 76.30(18) . . ?
N6 Ni1 N2 93.93(19) . . ?
N7 Ni1 N4 93.08(18) . . ?
N1 Ni1 N4 75.38(18) . . ?
N6 Ni1 N4 86.57(18) . . ?
N2 Ni1 N4 151.65(18) . . ?
N7 Ni1 O1 85.99(16) . . ?
N1 Ni1 O1 148.67(17) . . ?
N6 Ni1 O1 89.35(16) . . ?
N2 Ni1 O1 72.38(16) . . ?
N4 Ni1 O1 135.95(16) . . ?
C19 O1 Ni1 112.4(3) . . ?
C15 N1 C11 121.3(5) . . ?
C15 N1 Ni1 118.4(4) . . ?
C11 N1 Ni1 120.1(4) . . ?
C9 N4 N5 117.5(5) . . ?
C9 N4 Ni1 116.9(4) . . ?
N5 N4 Ni1 125.3(3) . . ?
C27 N7 Ni1 163.7(5) . . ?
C26 N6 Ni1 152.8(4) . . ?
C16 N2 N3 121.9(5) . . ?
C16 N2 Ni1 119.3(4) . . ?
N3 N2 Ni1 118.7(4) . . ?
O2 C1 N5 121.5(5) . . ?
O2 C1 C2 123.3(5) . . ?
N5 C1 C2 115.2(5) . . ?
N1 C15 C14 120.9(5) . . ?
N1 C15 C16 114.3(5) . . ?
C14 C15 C16 124.7(5) . . ?
N4 C9 C10 124.4(5) . . ?
N4 C9 C11 113.1(5) . . ?
C10 C9 C11 122.5(5) . . ?
N2 N3 C19 114.9(5) . . ?
N2 N3 H3A 120(6) . . ?
C19 N3 H3A 124(6) . . ?
C23 C22 C21 121.0(6) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C6 C7 C2 120.1(6) . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
C4 C3 C2 120.5(6) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C1 N5 N4 116.5(5) . . ?
C1 N5 H5A 107(10) . . ?
N4 N5 H5A 131(10) . . ?
O1 C19 N3 121.2(5) . . ?
O1 C19 C20 123.0(5) . . ?
N3 C19 C20 115.8(5) . . ?
N2 C16 C17 125.4(5) . . ?
N2 C16 C15 111.5(5) . . ?
C17 C16 C15 123.0(5) . . ?
C13 C14 C15 117.9(5) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
N1 C11 C12 121.0(5) . . ?
N1 C11 C9 114.3(5) . . ?
C12 C11 C9 124.7(5) . . ?
C25 C20 C21 119.6(5) . . ?
C25 C20 C19 118.7(5) . . ?
C21 C20 C19 121.6(5) . . ?
C13 C12 C11 118.1(5) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C3 C2 C7 119.2(5) . . ?
C3 C2 C1 117.7(5) . . ?
C7 C2 C1 123.0(5) . . ?
C24 C25 C20 120.7(5) . . ?
C24 C25 H25 119.7 . . ?
C20 C25 H25 119.7 . . ?
C22 C21 C20 118.9(5) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C23 C24 C25 119.4(6) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C14 C13 C12 120.8(6) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C5 C4 C3 119.3(6) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.2(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C6 C5 120.6(6) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C22 C23 C24 120.4(6) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
N7 C27 S2 179.4(5) . . ?
N6 C26 S1 178.8(5) . . ?

_refine_diff_density_max         0.676
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.125

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1936571'
loop_
_audit_author_name
_audit_author_address
'Bipul Sarma'
;Tezpur University
India
;
_audit_update_record             
;
2019-06-26 deposited with the CCDC.	2019-08-30 downloaded from the CCDC.
;
_vrf_PLAT029_shelxl              
;
PROBLEM:  _diffrn_measured_fraction_theta_full Low .......      0.963     
RESPONSE: This is a triclinic Molybdenum dataset collected with a four-circle
diffractometer. Some regions of reciprocal space
remain unaccessible, especially at the high 2-Theta
angles that are needed to collect high-resolution
copper data.  Depending on crystal orientation,
sometimes all equivalents of some reflections fall
into this unaccessible region and the completeness
suffers. The data collection strategy was based on
a combination of phi and omega scans spread out
evenly across the accessible reciprocal space
giving rise to a multiplicity of observations
("redundancy".  This underlines that the data
collection strategy employed was adequate.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H15 N9 Ni O4 S2'
_chemical_formula_weight         484.08

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.758(4)
_cell_length_b                   11.248(5)
_cell_length_c                   12.524(6)
_cell_angle_alpha                65.786(6)
_cell_angle_beta                 84.967(7)
_cell_angle_gamma                71.813(6)
_cell_volume                     1067.9(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6073
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      26.99

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_F_000             496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    1.142
_shelx_estimated_absorpt_T_min   0.771
_shelx_estimated_absorpt_T_max   0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8307
_exptl_absorpt_correction_T_max  0.9200
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10441
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.450
_diffrn_reflns_theta_max         28.776
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             5086
_reflns_number_gt                3572
_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    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0625P)²+1.3010P] 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         5086
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1635
_refine_ls_wR_factor_gt          0.1493
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
C1 C 0.1937(5) 0.1589(4) 0.1891(3) 0.0314(9) Uani 1 1 d . . . . .
C2 C 0.2073(5) 0.2879(5) 0.1233(4) 0.0440(11) Uani 1 1 d . . . . .
H2 H 0.1243 0.3656 0.1187 0.053 Uiso 1 1 calc R U . . .
C3 C 0.3470(6) 0.2997(5) 0.0639(4) 0.0470(11) Uani 1 1 d . . . . .
H3 H 0.3574 0.3858 0.0181 0.056 Uiso 1 1 calc R U . . .
C4 C 0.4697(5) 0.1845(5) 0.0728(4) 0.0407(10) Uani 1 1 d . . . . .
H4 H 0.5637 0.1914 0.0334 0.049 Uiso 1 1 calc R U . . .
C5 C 0.4511(5) 0.0578(4) 0.1415(3) 0.0310(8) Uani 1 1 d . . . . .
C6 C 0.0526(5) 0.1306(4) 0.2573(4) 0.0360(9) Uani 1 1 d . . . . .
C7 C -0.0837(6) 0.2429(5) 0.2692(5) 0.0492(12) Uani 1 1 d . . . . .
H7A H -0.1637 0.2053 0.3160 0.074 Uiso 1 1 calc R U . . .
H7B H -0.1305 0.3076 0.1930 0.074 Uiso 1 1 calc R U . . .
H7C H -0.0448 0.2880 0.3064 0.074 Uiso 1 1 calc R U . . .
C8 C 0.5759(5) -0.0753(4) 0.1648(4) 0.0331(9) Uani 1 1 d . . . . .
C9 C 0.7416(5) -0.0843(5) 0.1213(4) 0.0475(12) Uani 1 1 d . . . . .
H9A H 0.8039 -0.1787 0.1449 0.071 Uiso 1 1 calc R U . . .
H9B H 0.7917 -0.0409 0.1536 0.071 Uiso 1 1 calc R U . . .
H9C H 0.7357 -0.0392 0.0373 0.071 Uiso 1 1 calc R U . . .
C10 C -0.0523(5) -0.1702(5) 0.4195(4) 0.0390(10) Uani 1 1 d . . . . .
C11 C 0.5622(5) -0.4102(4) 0.3365(4) 0.0342(9) Uani 1 1 d . . . . .
C12 C 0.4087(5) -0.1538(4) 0.5272(4) 0.0315(8) Uani 1 1 d . . . . .
C13 C 0.1754(5) -0.2185(5) 0.1071(4) 0.0407(10) Uani 1 1 d . . . . .
N1 N 0.3126(4) 0.0469(3) 0.1959(3) 0.0295(7) Uani 1 1 d . . . . .
N2 N 0.0618(4) 0.0026(4) 0.3055(3) 0.0340(8) Uani 1 1 d . . . . .
N3 N -0.0653(4) -0.0339(4) 0.3674(3) 0.0397(9) Uani 1 1 d . . . . .
N4 N 0.5265(4) -0.1791(3) 0.2292(3) 0.0312(7) Uani 1 1 d . . . . .
N5 N 0.6250(4) -0.3087(4) 0.2615(3) 0.0371(8) Uani 1 1 d . . . . .
N6 N 0.6641(5) -0.5369(4) 0.3709(4) 0.0484(11) Uani 1 1 d . . . . .
N7 N -0.1884(6) -0.1982(6) 0.4614(5) 0.0655(15) Uani 1 1 d . . . . .
N8 N 0.3690(4) -0.1574(4) 0.4436(3) 0.0391(8) Uani 1 1 d . . . . .
N9 N 0.1999(4) -0.1696(4) 0.1655(3) 0.0406(8) Uani 1 1 d . . . . .
O1 O 0.0774(3) -0.2588(3) 0.4270(3) 0.0461(8) Uani 1 1 d . . . . .
O2 O 0.4218(3) -0.3827(3) 0.3663(3) 0.0412(7) Uani 1 1 d . . . . .
O102 O -0.0465(4) -0.4455(4) 0.2413(4) 0.0607(10) Uani 1 1 d . . . . .
O103 O 0.1755(5) -0.5109(4) 0.4148(4) 0.0701(11) Uani 1 1 d . . . . .
S1 S 0.46271(15) -0.14843(15) 0.64636(11) 0.0521(3) Uani 1 1 d . . . . .
S2 S 0.1438(2) -0.28599(19) 0.02052(13) 0.0710(5) Uani 1 1 d . . . . .
Ni01 Ni 0.29042(6) -0.14125(5) 0.29158(4) 0.03226(17) Uani 1 1 d . . . . .
H3D H -0.156(6) 0.030(5) 0.353(4) 0.050(14) Uiso 1 1 d . . . . .
H5D H 0.723(6) -0.329(5) 0.245(4) 0.056(15) Uiso 1 1 d . . . . .
H6D H 0.646(6) -0.604(5) 0.425(4) 0.038(13) Uiso 1 1 d . . . . .
H6E H 0.776(14) -0.553(12) 0.335(10) 0.22(5) Uiso 1 1 d . . . . .
H7D H -0.262(6) -0.135(5) 0.450(4) 0.044(15) Uiso 1 1 d . . . . .
H7E H -0.177(7) -0.295(7) 0.515(5) 0.078(19) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.338(5) . ?
C1 C2 1.381(6) . ?
C1 C6 1.482(5) . ?
C2 C3 1.389(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.353(5) . ?
C5 C8 1.482(6) . ?
C6 N2 1.290(5) . ?
C6 C7 1.492(6) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N4 1.298(5) . ?
C8 C9 1.492(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O1 1.236(5) . ?
C10 N7 1.336(6) . ?
C10 N3 1.369(6) . ?
C11 O2 1.235(5) . ?
C11 N6 1.335(6) . ?
C11 N5 1.382(5) . ?
C12 N8 1.153(5) . ?
C12 S1 1.633(4) . ?
C13 N9 1.147(5) . ?
C13 S2 1.639(5) . ?
N1 Ni01 2.021(3) . ?
N2 N3 1.372(4) . ?
N2 Ni01 2.192(3) . ?
N3 H3D 0.86(5) . ?
N4 N5 1.352(5) . ?
N4 Ni01 2.123(3) . ?
N5 H5D 0.85(5) . ?
N6 H6D 0.83(5) . ?
N6 H6E 1.04(11) . ?
N7 H7D 0.76(5) . ?
N7 H7E 1.00(6) . ?
N8 Ni01 2.000(4) . ?
N9 Ni01 2.003(4) . ?
O2 Ni01 2.394(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
N1 C1 C2 120.8(4) . . ?
N1 C1 C6 114.2(4) . . ?
C2 C1 C6 124.9(4) . . ?
C1 C2 C3 118.9(4) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 118.8(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.0(4) . . ?
N1 C5 C8 114.0(4) . . ?
C4 C5 C8 125.0(4) . . ?
N2 C6 C1 114.1(3) . . ?
N2 C6 C7 124.6(4) . . ?
C1 C6 C7 121.3(4) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 C5 112.8(3) . . ?
N4 C8 C9 125.1(4) . . ?
C5 C8 C9 122.1(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 C10 N7 123.7(5) . . ?
O1 C10 N3 121.4(4) . . ?
N7 C10 N3 114.9(4) . . ?
O2 C11 N6 124.1(4) . . ?
O2 C11 N5 121.2(4) . . ?
N6 C11 N5 114.7(4) . . ?
N8 C12 S1 179.3(4) . . ?
N9 C13 S2 178.2(4) . . ?
C1 N1 C5 120.4(3) . . ?
C1 N1 Ni01 120.4(3) . . ?
C5 N1 Ni01 119.1(3) . . ?
C6 N2 N3 118.5(3) . . ?
C6 N2 Ni01 116.3(3) . . ?
N3 N2 Ni01 125.0(3) . . ?
C10 N3 N2 117.7(3) . . ?
C10 N3 H3D 123(3) . . ?
N2 N3 H3D 116(3) . . ?
C8 N4 N5 121.2(3) . . ?
C8 N4 Ni01 118.5(3) . . ?
N5 N4 Ni01 120.2(3) . . ?
N4 N5 C11 115.8(3) . . ?
N4 N5 H5D 124(4) . . ?
C11 N5 H5D 120(4) . . ?
C11 N6 H6D 123(3) . . ?
C11 N6 H6E 120(6) . . ?
H6D N6 H6E 117(7) . . ?
C10 N7 H7D 115(4) . . ?
C10 N7 H7E 116(3) . . ?
H7D N7 H7E 128(5) . . ?
C12 N8 Ni01 173.7(4) . . ?
C13 N9 Ni01 162.5(4) . . ?
C11 O2 Ni01 112.1(3) . . ?
N8 Ni01 N9 165.34(15) . . ?
N8 Ni01 N1 95.52(14) . . ?
N9 Ni01 N1 99.03(14) . . ?
N8 Ni01 N4 92.33(14) . . ?
N9 Ni01 N4 93.01(14) . . ?
N1 Ni01 N4 75.46(13) . . ?
N8 Ni01 N2 89.37(14) . . ?
N9 Ni01 N2 92.77(14) . . ?
N1 Ni01 N2 74.67(13) . . ?
N4 Ni01 N2 150.11(13) . . ?
N8 Ni01 O2 84.28(13) . . ?
N9 Ni01 O2 84.66(14) . . ?
N1 Ni01 O2 145.91(11) . . ?
N4 Ni01 O2 70.49(11) . . ?
N2 Ni01 O2 139.29(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.1(7) . . . . ?
C6 C1 C2 C3 179.8(4) . . . . ?
C1 C2 C3 C4 -1.1(7) . . . . ?
C2 C3 C4 C5 0.1(7) . . . . ?
C3 C4 C5 N1 2.2(6) . . . . ?
C3 C4 C5 C8 -176.4(4) . . . . ?
N1 C1 C6 N2 -4.7(5) . . . . ?
C2 C1 C6 N2 175.4(4) . . . . ?
N1 C1 C6 C7 173.9(4) . . . . ?
C2 C1 C6 C7 -6.0(7) . . . . ?
N1 C5 C8 N4 3.2(5) . . . . ?
C4 C5 C8 N4 -178.1(4) . . . . ?
N1 C5 C8 C9 -174.6(4) . . . . ?
C4 C5 C8 C9 4.2(7) . . . . ?
C2 C1 N1 C5 2.4(6) . . . . ?
C6 C1 N1 C5 -177.5(3) . . . . ?
C2 C1 N1 Ni01 -179.5(3) . . . . ?
C6 C1 N1 Ni01 0.6(5) . . . . ?
C4 C5 N1 C1 -3.5(6) . . . . ?
C8 C5 N1 C1 175.3(3) . . . . ?
C4 C5 N1 Ni01 178.4(3) . . . . ?
C8 C5 N1 Ni01 -2.8(4) . . . . ?
C1 C6 N2 N3 -177.9(4) . . . . ?
C7 C6 N2 N3 3.6(6) . . . . ?
C1 C6 N2 Ni01 6.3(5) . . . . ?
C7 C6 N2 Ni01 -172.2(4) . . . . ?
O1 C10 N3 N2 11.4(7) . . . . ?
N7 C10 N3 N2 -169.3(4) . . . . ?
C6 N2 N3 C10 -179.1(4) . . . . ?
Ni01 N2 N3 C10 -3.7(5) . . . . ?
C5 C8 N4 N5 -178.6(3) . . . . ?
C9 C8 N4 N5 -1.0(6) . . . . ?
C5 C8 N4 Ni01 -2.2(5) . . . . ?
C9 C8 N4 Ni01 175.5(3) . . . . ?
C8 N4 N5 C11 175.8(4) . . . . ?
Ni01 N4 N5 C11 -0.6(5) . . . . ?
O2 C11 N5 N4 3.5(6) . . . . ?
N6 C11 N5 N4 -177.4(4) . . . . ?
N6 C11 O2 Ni01 176.8(4) . . . . ?
N5 C11 O2 Ni01 -4.3(5) . . . . ?

_refine_diff_density_max         0.581
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.092

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_squeezed
_database_code_depnum_ccdc_archive 'CCDC 1936566'
loop_
_audit_author_name
_audit_author_address
'Bipul Sarma'
;Tezpur University
India
;
_audit_update_record             
;
2019-06-26 deposited with the CCDC.	2019-08-30 downloaded from the CCDC.
;

_vrf_PLAT601_squeezed            
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        422 Ang**3
RESPONSE: Structure contains disordered water molecules and two nitrate
anions and removed using PLATON SQUEEZE program. The sample diffracted
very weakly because they form bad quality needle crystals. Moreover high
angle reflections are of very poor quality. Low temperature data could
resolve this issue. 
;
_vrf_SHFSU01_squeezed            
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
            Absolute value of the parameter shift to su ratio given   0.336
            Additional refinement cycles may be required.
RESPONSE: The sample diffracted very weakly, and at high angles the
reflections were completely missing. Dispite the poor quality of the data, the
connectivity and gross conformation are not in doubt. 
;
_vrf_PLAT080_squeezed            
;
PROBLEM: Maximum Shift/Error ............................       0.34 Why ?
RESPONSE: The sample diffracted very weakly because these are fine
needle-shaped crystals. High angles reflections are with very poor data
quality. 
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H23 N11 Ni O2'
_chemical_formula_weight         472.17

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   32.1592(12)
_cell_length_b                   32.1592(12)
_cell_length_c                   10.0314(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10374.6(9)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4491
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      21.74

_exptl_crystal_description       Needle
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_F_000             3936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.780
_shelx_estimated_absorpt_T_min   0.794
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   SADABS
_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            37717
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.266
_diffrn_reflns_theta_max         28.411
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6507
_reflns_number_gt                3768
_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    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1153P)²+1.2136P] 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         6507
_refine_ls_number_parameters     314
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.2088
_refine_ls_wR_factor_gt          0.1895
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.336
_refine_ls_shift/su_mean         0.010

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
C3 C 0.17668(17) 0.1385(2) 0.9576(9) 0.127(3) Uani 1 1 d . . . . .
H3 H 0.1934 0.1509 1.0219 0.152 Uiso 1 1 calc R U . . .
C10 C 0.02564(9) 0.01067(9) 0.6844(3) 0.0365(6) Uani 1 1 d . . . . .
C15 C 0.15588(12) 0.01975(11) 0.6304(4) 0.0584(9) Uani 1 1 d . . . . .
H15 H 0.1590 0.0224 0.7222 0.070 Uiso 1 1 calc R U . . .
C1 C 0.12489(11) 0.08958(12) 0.8963(4) 0.0580(9) Uani 1 1 d . . . . .
C8 C 0.15003(15) 0.14996(13) 0.5965(7) 0.0981(19) Uani 1 1 d . . . . .
C6 C 0.09493(10) 0.05562(12) 0.9138(3) 0.0532(8) Uani 1 1 d . . . . .
C14 C 0.00845(13) 0.13950(15) 0.5843(6) 0.0808(13) Uani 1 1 d . . . . .
H14 H 0.0046 0.1308 0.4967 0.097 Uiso 1 1 calc R U . . .
C7 C 0.09148(14) 0.03226(14) 1.0431(4) 0.0742(12) Uani 1 1 d . . . . .
H7A H 0.1185 0.0228 1.0699 0.111 Uiso 1 1 calc R U . . .
H7B H 0.0734 0.0088 1.0316 0.111 Uiso 1 1 calc R U . . .
H7C H 0.0803 0.0503 1.1105 0.111 Uiso 1 1 calc R U . . .
C11 C 0.0834(2) 0.12198(16) 0.3373(5) 0.0914(17) Uani 1 1 d . . . . .
C2 C 0.15069(13) 0.10548(17) 0.9964(6) 0.0914(16) Uani 1 1 d . . . . .
H2 H 0.1507 0.0949 1.0827 0.110 Uiso 1 1 calc R U . . .
C16 C 0.16602(17) 0.00050(14) 0.4234(4) 0.0812(14) Uani 1 1 d . . . . .
H16 H 0.1769 -0.0120 0.3473 0.097 Uiso 1 1 calc R U . . .
C17 C 0.13347(16) 0.02607(13) 0.4313(4) 0.0765(12) Uani 1 1 d . . . . .
H17 H 0.1175 0.0343 0.3585 0.092 Uiso 1 1 calc R U . . .
C12 C 0.03250(15) 0.14444(14) 0.7822(5) 0.0792(12) Uani 1 1 d . . . . .
H12 H 0.0484 0.1409 0.8588 0.095 Uiso 1 1 calc R U . . .
C13 C -0.01368(15) 0.16785(16) 0.6464(7) 0.0954(18) Uani 1 1 d . . . . .
H13 H -0.0353 0.1833 0.6094 0.114 Uiso 1 1 calc R U . . .
C5 C 0.15192(12) 0.13634(12) 0.7359(6) 0.0750(13) Uani 1 1 d . . . . .
C4 C 0.17840(16) 0.1528(2) 0.8350(10) 0.126(3) Uani 1 1 d . . . . .
H4 H 0.1971 0.1738 0.8135 0.151 Uiso 1 1 calc R U . . .
C9 C 0.18001(18) 0.18136(17) 0.5403(9) 0.138(3) Uani 1 1 d . . . . .
H9D H 0.2020 0.1861 0.6031 0.206 Uiso 1 1 calc R U . . .
H9B H 0.1656 0.2070 0.5235 0.206 Uiso 1 1 calc R U . . .
H9C H 0.1915 0.1710 0.4585 0.206 Uiso 1 1 calc R U . . .
N1 N 0.12569(9) 0.10552(9) 0.7700(4) 0.0596(8) Uani 1 1 d . . . . .
N2 N 0.07337(8) 0.04726(8) 0.8081(2) 0.0420(6) Uani 1 1 d . . . . .
N3 N 0.04504(9) 0.01618(8) 0.8058(2) 0.0441(6) Uani 1 1 d . . . . .
N4 N 0.12145(12) 0.13149(10) 0.5284(4) 0.0767(11) Uani 1 1 d . . . . .
N5 N 0.11512(17) 0.14198(14) 0.4008(6) 0.1024(17) Uani 1 1 d . . . . .
N10 N 0.12636(9) 0.03880(8) 0.5597(3) 0.0504(7) Uani 1 1 d . . . . .
N8 N 0.03853(9) 0.12473(10) 0.6709(3) 0.0608(8) Uani 1 1 d . . . . .
N11 N 0.18029(13) -0.00344(11) 0.5545(4) 0.0728(10) Uani 1 1 d . . . . .
N9 N -0.00001(14) 0.17079(14) 0.7715(6) 0.0902(13) Uani 1 1 d . . . . .
N6 N -0.00137(9) -0.02025(9) 0.6782(3) 0.0503(7) Uani 1 1 d D . . . .
N7 N 0.0734(2) 0.13438(17) 0.2134(5) 0.1256(19) Uani 1 1 d D . . . .
Ni1 Ni 0.08465(2) 0.08192(2) 0.62931(4) 0.05377(19) Uani 1 1 d . . . . .
O1 O 0.03380(7) 0.03376(7) 0.58805(19) 0.0480(5) Uani 1 1 d . . . . .
O2 O 0.06475(11) 0.09190(10) 0.3911(3) 0.0896(10) Uani 1 1 d . . . . .
H6B H -0.0127(9) -0.0267(10) 0.5988(14) 0.050(9) Uiso 1 1 d D . . . .
H5A H 0.1252(14) 0.1651(16) 0.389(4) 0.079(14) Uiso 1 1 d . . . . .
H6A H -0.0116(17) -0.011(2) 0.756(3) 0.25(5) Uiso 1 1 d D . . . .
H7E H 0.0830(12) 0.1606(5) 0.206(5) 0.090(16) Uiso 1 1 d D . . . .
H3A H 0.032(3) 0.015(3) 0.874(9) 0.21(4) Uiso 1 1 d . . . . .
H7D H 0.071(3) 0.1155(11) 0.148(3) 0.24(5) Uiso 1 1 d D . . . .
H11A H 0.2024(16) -0.0119(16) 0.581(5) 0.091(17) Uiso 1 1 d . . . . .
H9A H 0.005(2) 0.192(2) 0.829(8) 0.17(3) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C3 C4 1.313(11) . ?
C3 C2 1.407(9) . ?
C3 H3 0.9300 . ?
C10 O1 1.247(3) . ?
C10 N6 1.322(4) . ?
C10 N3 1.380(4) . ?
C10 H6A 1.55(6) . ?
C15 N11 1.324(5) . ?
C15 N10 1.334(5) . ?
C15 H15 0.9300 . ?
C1 N1 1.367(5) . ?
C1 C2 1.399(5) . ?
C1 C6 1.467(5) . ?
C8 N4 1.290(7) . ?
C8 C5 1.467(8) . ?
C8 C9 1.506(6) . ?
C6 N2 1.296(4) . ?
C6 C7 1.503(5) . ?
C14 C13 1.314(7) . ?
C14 N8 1.384(5) . ?
C14 H14 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C11 O2 1.259(6) . ?
C11 N7 1.344(7) . ?
C11 N5 1.365(8) . ?
C2 H2 0.9300 . ?
C16 C17 1.333(6) . ?
C16 N11 1.398(6) . ?
C16 H16 0.9300 . ?
C17 N10 1.371(5) . ?
C17 H17 0.9300 . ?
C12 N8 1.299(5) . ?
C12 N9 1.350(6) . ?
C12 H12 0.9300 . ?
C13 N9 1.332(8) . ?
C13 H13 0.9300 . ?
C5 N1 1.346(5) . ?
C5 C4 1.412(8) . ?
C4 H4 0.9300 . ?
C9 H9D 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
N1 Ni1 2.076(3) . ?
N2 N3 1.353(4) . ?
N2 Ni1 2.142(2) . ?
N3 H3A 0.79(9) . ?
N4 N5 1.339(6) . ?
N4 Ni1 2.229(3) . ?
N5 H5A 0.82(5) . ?
N10 Ni1 2.052(3) . ?
N8 Ni1 2.066(3) . ?
N11 H11A 0.80(5) . ?
N9 H9A 0.90(8) . ?
N6 H6B 0.8999(10) . ?
N6 H6A 0.9003(19) . ?
N7 H7E 0.9001(11) . ?
N7 H7D 0.9001(11) . ?
Ni1 O1 2.290(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
C4 C3 C2 123.2(6) . . ?
C4 C3 H3 118.4 . . ?
C2 C3 H3 118.4 . . ?
O1 C10 N6 123.4(3) . . ?
O1 C10 N3 120.8(3) . . ?
N6 C10 N3 115.8(3) . . ?
O1 C10 H6A 141(2) . . ?
N6 C10 H6A 35.4(13) . . ?
N3 C10 H6A 89.9(16) . . ?
N11 C15 N10 112.0(4) . . ?
N11 C15 H15 124.0 . . ?
N10 C15 H15 124.0 . . ?
N1 C1 C2 121.1(4) . . ?
N1 C1 C6 113.7(3) . . ?
C2 C1 C6 125.1(4) . . ?
N4 C8 C5 113.4(4) . . ?
N4 C8 C9 124.5(7) . . ?
C5 C8 C9 122.1(6) . . ?
N2 C6 C1 114.1(3) . . ?
N2 C6 C7 124.3(3) . . ?
C1 C6 C7 121.6(3) . . ?
C13 C14 N8 108.6(5) . . ?
C13 C14 H14 125.7 . . ?
N8 C14 H14 125.7 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C11 N7 120.6(7) . . ?
O2 C11 N5 121.2(5) . . ?
N7 C11 N5 118.1(5) . . ?
C1 C2 C3 115.5(6) . . ?
C1 C2 H2 122.3 . . ?
C3 C2 H2 122.3 . . ?
C17 C16 N11 104.9(4) . . ?
C17 C16 H16 127.5 . . ?
N11 C16 H16 127.5 . . ?
C16 C17 N10 111.8(4) . . ?
C16 C17 H17 124.1 . . ?
N10 C17 H17 124.1 . . ?
N8 C12 N9 110.7(5) . . ?
N8 C12 H12 124.7 . . ?
N9 C12 H12 124.7 . . ?
C14 C13 N9 108.5(5) . . ?
C14 C13 H13 125.8 . . ?
N9 C13 H13 125.7 . . ?
N1 C5 C4 118.4(6) . . ?
N1 C5 C8 115.9(4) . . ?
C4 C5 C8 125.8(5) . . ?
C3 C4 C5 120.2(6) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C8 C9 H9D 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9D C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9D C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 N1 C1 121.5(4) . . ?
C5 N1 Ni1 119.7(3) . . ?
C1 N1 Ni1 118.8(2) . . ?
C6 N2 N3 121.8(3) . . ?
C6 N2 Ni1 119.1(2) . . ?
N3 N2 Ni1 118.97(18) . . ?
N2 N3 C10 114.5(2) . . ?
N2 N3 H3A 111(7) . . ?
C10 N3 H3A 121(7) . . ?
C8 N4 N5 119.9(4) . . ?
C8 N4 Ni1 117.8(4) . . ?
N5 N4 Ni1 122.2(4) . . ?
N4 N5 C11 116.2(4) . . ?
N4 N5 H5A 108(3) . . ?
C11 N5 H5A 131(3) . . ?
C15 N10 C17 104.1(3) . . ?
C15 N10 Ni1 126.5(2) . . ?
C17 N10 Ni1 129.1(3) . . ?
C12 N8 C14 105.5(4) . . ?
C12 N8 Ni1 127.3(3) . . ?
C14 N8 Ni1 127.1(3) . . ?
C15 N11 C16 107.2(4) . . ?
C15 N11 H11A 122(4) . . ?
C16 N11 H11A 129(4) . . ?
C13 N9 C12 106.6(5) . . ?
C13 N9 H9A 136(5) . . ?
C12 N9 H9A 106(5) . . ?
C10 N6 H6B 119(2) . . ?
C10 N6 H6A 87(5) . . ?
H6B N6 H6A 134(4) . . ?
C11 N7 H7E 106(3) . . ?
C11 N7 H7D 120(4) . . ?
H7E N7 H7D 127(4) . . ?
N10 Ni1 N8 171.24(12) . . ?
N10 Ni1 N1 93.59(11) . . ?
N8 Ni1 N1 94.34(12) . . ?
N10 Ni1 N2 92.51(10) . . ?
N8 Ni1 N2 93.22(11) . . ?
N1 Ni1 N2 74.27(11) . . ?
N10 Ni1 N4 88.96(11) . . ?
N8 Ni1 N4 89.78(12) . . ?
N1 Ni1 N4 73.12(15) . . ?
N2 Ni1 N4 147.39(14) . . ?
N10 Ni1 O1 87.03(10) . . ?
N8 Ni1 O1 88.54(11) . . ?
N1 Ni1 O1 145.50(11) . . ?
N2 Ni1 O1 71.24(8) . . ?
N4 Ni1 O1 141.34(13) . . ?
C10 O1 Ni1 114.40(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C6 N2 -2.0(4) . . . . ?
C2 C1 C6 N2 177.6(3) . . . . ?
N1 C1 C6 C7 175.9(3) . . . . ?
C2 C1 C6 C7 -4.5(6) . . . . ?
N1 C1 C2 C3 0.4(6) . . . . ?
C6 C1 C2 C3 -179.2(4) . . . . ?
C4 C3 C2 C1 -2.9(9) . . . . ?
N11 C16 C17 N10 0.3(5) . . . . ?
N8 C14 C13 N9 -2.3(6) . . . . ?
N4 C8 C5 N1 3.5(5) . . . . ?
C9 C8 C5 N1 -174.4(4) . . . . ?
N4 C8 C5 C4 -176.2(4) . . . . ?
C9 C8 C5 C4 5.9(7) . . . . ?
C2 C3 C4 C5 3.3(10) . . . . ?
N1 C5 C4 C3 -1.1(8) . . . . ?
C8 C5 C4 C3 178.6(6) . . . . ?
C4 C5 N1 C1 -1.3(5) . . . . ?
C8 C5 N1 C1 178.9(3) . . . . ?
C4 C5 N1 Ni1 177.7(3) . . . . ?
C8 C5 N1 Ni1 -2.0(4) . . . . ?
C2 C1 N1 C5 1.6(5) . . . . ?
C6 C1 N1 C5 -178.8(3) . . . . ?
C2 C1 N1 Ni1 -177.4(3) . . . . ?
C6 C1 N1 Ni1 2.2(4) . . . . ?
C1 C6 N2 N3 178.4(3) . . . . ?
C7 C6 N2 N3 0.5(5) . . . . ?
C1 C6 N2 Ni1 1.0(4) . . . . ?
C7 C6 N2 Ni1 -176.9(3) . . . . ?
C6 N2 N3 C10 -178.3(3) . . . . ?
Ni1 N2 N3 C10 -0.9(3) . . . . ?
O1 C10 N3 N2 -1.5(4) . . . . ?
N6 C10 N3 N2 178.2(3) . . . . ?
C5 C8 N4 N5 177.5(4) . . . . ?
C9 C8 N4 N5 -4.6(7) . . . . ?
C5 C8 N4 Ni1 -3.4(5) . . . . ?
C9 C8 N4 Ni1 174.5(4) . . . . ?
C8 N4 N5 C11 -177.9(4) . . . . ?
Ni1 N4 N5 C11 3.1(6) . . . . ?
O2 C11 N5 N4 -8.4(7) . . . . ?
N7 C11 N5 N4 173.7(4) . . . . ?
N11 C15 N10 C17 0.1(4) . . . . ?
N11 C15 N10 Ni1 -174.0(2) . . . . ?
C16 C17 N10 C15 -0.3(5) . . . . ?
C16 C17 N10 Ni1 173.6(3) . . . . ?
N9 C12 N8 C14 0.4(5) . . . . ?
N9 C12 N8 Ni1 178.4(3) . . . . ?
C13 C14 N8 C12 1.2(5) . . . . ?
C13 C14 N8 Ni1 -176.8(3) . . . . ?
N10 C15 N11 C16 0.1(5) . . . . ?
C17 C16 N11 C15 -0.3(5) . . . . ?
C14 C13 N9 C12 2.5(6) . . . . ?
N8 C12 N9 C13 -1.8(6) . . . . ?
N6 C10 O1 Ni1 -176.7(2) . . . . ?
N3 C10 O1 Ni1 2.9(3) . . . . ?

_refine_diff_density_max         0.309
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.071

