# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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 1996089'
loop_
_audit_author_name
_audit_author_address
'Bin-bin Qian'
;Nankai university
China
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_audit_creation_date             2021-01-28
_audit_creation_method           
;
Olex2 1.5-dev
(compiled 2020.12.01 svn.rb'be22f01f' for OlexSys, GUI svn.r6224)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C54 H42 N12 Ni3 O18, 6[C3H7NO]'
_chemical_formula_sum            'C72 H84 N18 Ni3 O24'
_chemical_formula_weight         1761.70
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   10.13653(10)
_cell_length_b                   25.9159(2)
_cell_length_c                   15.63851(15)
_cell_angle_alpha                90
_cell_angle_beta                 101.0451(9)
_cell_angle_gamma                90
_cell_volume                     4032.10(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.546
_cell_measurement_theta_min      4.761
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.548
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22979
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.546
_diffrn_reflns_theta_min         3.347
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  riguku
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7160
_reflns_number_total             7947
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7947
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0668P)²+2.7581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1242
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1W-H1WA
 0.85 with sigma of 0.01
 O1W-H1WB
 0.85 with sigma of 0.01
 H1WA-H1WB
 1.34 with sigma of 0.02
 O2W-H2WA
 0.85 with sigma of 0.01
 O2W-H2WB
 0.85 with sigma of 0.01
 H2WA-H2WB
 1.34 with sigma of 0.02
 O3W-H3WA
 0.85 with sigma of 0.01
 O3W-H3WB
 0.85 with sigma of 0.01
 H3WA-H3WB
 1.34 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.80551(3) 0.69030(2) 0.20236(2) 0.01901(10) Uani 1 1 d . . . . .
Ni2 Ni 1.000000 0.500000 1.000000 0.02884(13) Uani 1 2 d S . P . .
O1 O 0.48289(17) 0.67341(8) 0.14431(13) 0.0536(5) Uani 1 1 d . . . . .
O1W O 0.71014(14) 0.64898(5) 0.09797(9) 0.0238(3) Uani 1 1 d D . . . .
H1WA H 0.729(2) 0.6517(10) 0.0480(9) 0.036 Uiso 1 1 d D U . . .
H1WB H 0.6292(12) 0.6563(10) 0.0949(15) 0.036 Uiso 1 1 d D U . . .
O2 O 0.63825(13) 0.70909(5) 0.24756(9) 0.0268(3) Uani 1 1 d . . . . .
O2W O 0.83173(17) 0.54559(6) 0.99205(11) 0.0378(4) Uani 1 1 d D . . . .
H2WA H 0.762(2) 0.5366(11) 1.010(2) 0.057 Uiso 1 1 d D U . . .
H2WB H 0.831(3) 0.5776(4) 0.984(2) 0.057 Uiso 1 1 d D U . . .
O3 O 0.50637(15) 0.85106(6) 0.41788(11) 0.0363(4) Uani 1 1 d . . . . .
O3W O 1.11712(17) 0.56222(6) 0.98252(11) 0.0344(3) Uani 1 1 d D . . . .
H3WA H 1.1946(15) 0.5703(10) 1.0106(18) 0.052 Uiso 1 1 d D U . . .
H3WB H 1.077(2) 0.5904(7) 0.9680(19) 0.052 Uiso 1 1 d D U . . .
O4 O 0.29853(15) 0.85468(6) 0.44492(10) 0.0309(3) Uani 1 1 d . . . . .
O5 O -0.04324(13) 0.72803(5) 0.29516(8) 0.0208(3) Uani 1 1 d . . . . .
O6 O 0.00392(13) 0.68483(5) 0.18335(9) 0.0216(3) Uani 1 1 d . . . . .
N1 N 0.95092(19) 0.48839(7) 0.86425(12) 0.0306(4) Uani 1 1 d . . . . .
N2 N 0.71834(17) 0.26161(6) 0.36323(11) 0.0242(3) Uani 1 1 d . . . . .
N3 N 0.81843(16) 0.62473(6) 0.28172(11) 0.0229(3) Uani 1 1 d . . . . .
N4 N 0.81245(17) 0.41690(6) 0.56092(11) 0.0250(3) Uani 1 1 d . . . . .
N5 N 0.84366(17) 0.50643(6) 0.53906(11) 0.0254(3) Uani 1 1 d . . . . .
N6 N 0.78763(17) 0.45057(6) 0.41738(11) 0.0269(4) Uani 1 1 d . . . . .
C1 C 0.5194(2) 0.70010(8) 0.21146(15) 0.0309(5) Uani 1 1 d . . . . .
C2 C 0.4131(2) 0.72456(8) 0.25364(14) 0.0269(4) Uani 1 1 d . . . . .
C3 C 0.44722(19) 0.76509(8) 0.31225(14) 0.0258(4) Uani 1 1 d . . . . .
H3 H 0.535991 0.776205 0.326124 0.031 Uiso 1 1 calc R U . . .
C4 C 0.35000(19) 0.78912(7) 0.35025(13) 0.0227(4) Uani 1 1 d . . . . .
C5 C 0.21772(19) 0.77143(7) 0.33051(12) 0.0210(4) Uani 1 1 d . . . . .
H5 H 0.152460 0.786769 0.356569 0.025 Uiso 1 1 calc R U . . .
C6 C 0.18287(18) 0.73106(7) 0.27218(12) 0.0208(4) Uani 1 1 d . . . . .
C7 C 0.27996(19) 0.70812(8) 0.23231(13) 0.0249(4) Uani 1 1 d . . . . .
H7 H 0.255911 0.681950 0.191621 0.030 Uiso 1 1 calc R U . . .
C8 C 0.3891(2) 0.83486(7) 0.40922(13) 0.0250(4) Uani 1 1 d . . . . .
C9 C 0.04014(18) 0.71331(7) 0.24930(12) 0.0195(4) Uani 1 1 d . . . . .
C10 C 0.9319(3) 0.52817(8) 0.80875(14) 0.0348(5) Uani 1 1 d . . . . .
H10 H 0.943403 0.561375 0.831497 0.042 Uiso 1 1 calc R U . . .
C11 C 0.8963(2) 0.52257(8) 0.71955(14) 0.0331(5) Uani 1 1 d . . . . .
H11 H 0.886369 0.551306 0.683262 0.040 Uiso 1 1 calc R U . . .
C12 C 0.8754(2) 0.47335(8) 0.68508(13) 0.0258(4) Uani 1 1 d . . . . .
C13 C 0.8923(2) 0.43163(8) 0.74218(13) 0.0273(4) Uani 1 1 d . . . . .
H13 H 0.876871 0.398134 0.721303 0.033 Uiso 1 1 calc R U . . .
C14 C 0.9323(2) 0.44078(8) 0.83043(14) 0.0301(4) Uani 1 1 d . . . . .
H14 H 0.947049 0.412674 0.868031 0.036 Uiso 1 1 calc R U . . .
C15 C 0.84035(19) 0.46502(7) 0.58968(13) 0.0241(4) Uani 1 1 d . . . . .
C16 C 0.7881(2) 0.41203(7) 0.47444(13) 0.0255(4) Uani 1 1 d . . . . .
C17 C 0.81495(19) 0.49703(7) 0.45346(13) 0.0236(4) Uani 1 1 d . . . . .
C18 C 0.7621(2) 0.35949(7) 0.43690(14) 0.0268(4) Uani 1 1 d . . . . .
C19 C 0.7484(3) 0.31712(8) 0.48789(15) 0.0344(5) Uani 1 1 d . . . . .
H19 H 0.754034 0.320647 0.547663 0.041 Uiso 1 1 calc R U . . .
C20 C 0.7262(2) 0.26930(8) 0.44848(14) 0.0316(5) Uani 1 1 d . . . . .
H20 H 0.716245 0.240985 0.483226 0.038 Uiso 1 1 calc R U . . .
C21 C 0.7343(3) 0.30259(9) 0.31457(15) 0.0423(6) Uani 1 1 d . . . . .
H21 H 0.731066 0.297883 0.255241 0.051 Uiso 1 1 calc R U . . .
C22 C 0.7556(3) 0.35172(9) 0.34870(15) 0.0454(6) Uani 1 1 d . . . . .
H22 H 0.765414 0.379400 0.312595 0.054 Uiso 1 1 calc R U . . .
C23 C 0.7833(2) 0.57743(8) 0.25031(14) 0.0274(4) Uani 1 1 d . . . . .
H23 H 0.759319 0.573006 0.190327 0.033 Uiso 1 1 calc R U . . .
C24 C 0.7815(2) 0.53492(8) 0.30396(14) 0.0288(4) Uani 1 1 d . . . . .
H24 H 0.757594 0.502563 0.280232 0.035 Uiso 1 1 calc R U . . .
C25 C 0.81587(19) 0.54140(7) 0.39372(13) 0.0247(4) Uani 1 1 d . . . . .
C26 C 0.8512(2) 0.59054(8) 0.42623(14) 0.0270(4) Uani 1 1 d . . . . .
H26 H 0.874202 0.596230 0.485951 0.032 Uiso 1 1 calc R U . . .
C27 C 0.8516(2) 0.63050(8) 0.36838(14) 0.0273(4) Uani 1 1 d . . . . .
H27 H 0.875977 0.663172 0.390505 0.033 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1W 2.0349(14) . y
Ni1 O2 2.0175(14) . y
Ni1 O5 2.1355(13) 1_655 y
Ni1 O6 2.0935(13) 1_655 y
Ni1 N2 2.1051(16) 2_655 y
Ni1 N3 2.0933(16) . y
Ni1 C9 2.4253(18) 1_655 y
Ni2 O2W 2.0590(16) 3_767 y
Ni2 O2W 2.0590(16) . y
Ni2 O3W 2.0514(16) 3_767 y
Ni2 O3W 2.0515(16) . y
Ni2 N1 2.1072(18) . y
Ni2 N1 2.1072(18) 3_767 y
O1 C1 1.253(3) . ?
O1W H1WA 0.844(10) . ?
O1W H1WB 0.835(10) . ?
O2 C1 1.250(3) . ?
O2W H2WA 0.844(10) . ?
O2W H2WB 0.839(10) . ?
O3 C8 1.243(3) . ?
O3W H3WA 0.849(10) . ?
O3W H3WB 0.848(10) . ?
O4 C8 1.271(2) . ?
O5 C9 1.268(2) . ?
O6 C9 1.264(2) . ?
N1 C10 1.338(3) . ?
N1 C14 1.341(3) . ?
N2 C20 1.335(3) . ?
N2 C21 1.334(3) . ?
N3 C23 1.343(3) . ?
N3 C27 1.341(3) . ?
N4 C15 1.338(3) . ?
N4 C16 1.333(3) . ?
N5 C15 1.338(3) . ?
N5 C17 1.337(3) . ?
N6 C16 1.339(3) . ?
N6 C17 1.336(3) . ?
C1 C2 1.507(3) . ?
C2 C3 1.393(3) . ?
C2 C7 1.393(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.392(3) . ?
C4 C5 1.394(3) . ?
C4 C8 1.508(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(3) . ?
C6 C7 1.395(3) . ?
C6 C9 1.495(2) . ?
C7 H7 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.380(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.385(3) . ?
C12 C13 1.392(3) . ?
C12 C15 1.482(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.382(3) . ?
C14 H14 0.9300 . ?
C16 C18 1.486(3) . ?
C17 C25 1.483(3) . ?
C18 C19 1.380(3) . ?
C18 C22 1.383(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.383(3) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.382(3) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C23 C24 1.387(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.390(3) . ?
C25 C26 1.392(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.376(3) . ?
C27 H27 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
O1W Ni1 O5 162.74(5) . 1_655 y
O1W Ni1 O6 99.91(5) . 1_655 y
O1W Ni1 N2 94.50(6) . 2_655 y
O1W Ni1 N3 90.84(6) . . y
O1W Ni1 C9 131.28(6) . 1_655 y
O2 Ni1 O1W 96.10(6) . . y
O2 Ni1 O5 101.15(5) . 1_655 y
O2 Ni1 O6 163.89(6) . 1_655 y
O2 Ni1 N2 86.16(6) . 2_655 y
O2 Ni1 N3 87.11(6) . . y
O2 Ni1 C9 132.51(6) . 1_655 y
O5 Ni1 C9 31.46(6) 1_655 1_655 y
O6 Ni1 O5 62.83(5) 1_655 1_655 y
O6 Ni1 N2 90.80(6) 1_655 2_655 y
O6 Ni1 C9 31.41(6) 1_655 1_655 y
N2 Ni1 O5 85.96(6) 2_655 1_655 y
N2 Ni1 C9 86.90(6) 2_655 1_655 y
N3 Ni1 O5 90.78(6) . 1_655 y
N3 Ni1 O6 94.39(6) . 1_655 y
N3 Ni1 N2 171.81(7) . 2_655 y
N3 Ni1 C9 94.23(6) . 1_655 y
O2W Ni2 O2W 180.0 . 3_767 y
O2W Ni2 N1 89.32(7) . . y
O2W Ni2 N1 90.68(7) 3_767 . y
O2W Ni2 N1 90.68(7) . 3_767 y
O2W Ni2 N1 89.32(7) 3_767 3_767 y
O3W Ni2 O2W 88.01(6) 3_767 . y
O3W Ni2 O2W 91.99(6) 3_767 3_767 y
O3W Ni2 O2W 88.01(6) . 3_767 y
O3W Ni2 O2W 91.99(6) . . y
O3W Ni2 O3W 180.00(5) 3_767 . y
O3W Ni2 N1 89.48(7) . 3_767 y
O3W Ni2 N1 90.52(7) . . y
O3W Ni2 N1 90.52(7) 3_767 3_767 y
O3W Ni2 N1 89.48(7) 3_767 . y
N1 Ni2 N1 180.0 . 3_767 y
Ni1 O1W H1WA 122.8(18) . . ?
Ni1 O1W H1WB 103.7(17) . . ?
H1WA O1W H1WB 109.1(19) . . ?
C1 O2 Ni1 126.74(13) . . ?
Ni2 O2W H2WA 124(2) . . ?
Ni2 O2W H2WB 124(2) . . ?
H2WA O2W H2WB 110(2) . . ?
Ni2 O3W H3WA 128.8(19) . . ?
Ni2 O3W H3WB 116.7(19) . . ?
H3WA O3W H3WB 106(2) . . ?
C9 O5 Ni1 86.98(11) . 1_455 ?
C9 O6 Ni1 88.93(11) . 1_455 ?
C10 N1 Ni2 121.36(14) . . ?
C10 N1 C14 117.47(18) . . ?
C14 N1 Ni2 121.12(14) . . ?
C20 N2 Ni1 126.65(13) . 2_645 ?
C21 N2 Ni1 115.85(14) . 2_645 ?
C21 N2 C20 117.40(18) . . ?
C23 N3 Ni1 122.82(14) . . ?
C27 N3 Ni1 118.94(13) . . ?
C27 N3 C23 117.96(17) . . ?
C16 N4 C15 114.55(17) . . ?
C17 N5 C15 114.91(17) . . ?
C17 N6 C16 114.65(17) . . ?
O1 C1 C2 118.52(18) . . ?
O2 C1 O1 125.88(19) . . ?
O2 C1 C2 115.59(18) . . ?
C3 C2 C1 119.76(18) . . ?
C7 C2 C1 120.52(18) . . ?
C7 C2 C3 119.69(18) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.74(18) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C5 119.20(17) . . ?
C3 C4 C8 119.23(17) . . ?
C5 C4 C8 121.53(17) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.39(17) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 120.15(17) . . ?
C5 C6 C9 120.12(17) . . ?
C7 C6 C9 119.69(17) . . ?
C2 C7 C6 119.77(18) . . ?
C2 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
O3 C8 O4 124.88(18) . . ?
O3 C8 C4 117.77(17) . . ?
O4 C8 C4 117.33(17) . . ?
O5 C9 Ni1 61.56(9) . 1_455 ?
O5 C9 C6 119.45(16) . . ?
O6 C9 Ni1 59.66(9) . 1_455 ?
O6 C9 O5 121.10(16) . . ?
O6 C9 C6 119.43(16) . . ?
C6 C9 Ni1 174.99(13) . 1_455 ?
N1 C10 H10 118.2 . . ?
N1 C10 C11 123.51(19) . . ?
C11 C10 H10 118.2 . . ?
C10 C11 H11 120.6 . . ?
C10 C11 C12 118.8(2) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 C13 118.36(19) . . ?
C11 C12 C15 121.02(18) . . ?
C13 C12 C15 120.59(18) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 118.92(18) . . ?
C14 C13 H13 120.5 . . ?
N1 C14 C13 122.93(19) . . ?
N1 C14 H14 118.5 . . ?
C13 C14 H14 118.5 . . ?
N4 C15 N5 125.22(18) . . ?
N4 C15 C12 117.97(17) . . ?
N5 C15 C12 116.78(17) . . ?
N4 C16 N6 125.57(18) . . ?
N4 C16 C18 118.15(17) . . ?
N6 C16 C18 116.27(18) . . ?
N5 C17 C25 117.60(17) . . ?
N6 C17 N5 125.08(18) . . ?
N6 C17 C25 117.30(18) . . ?
C19 C18 C16 122.04(19) . . ?
C19 C18 C22 118.03(19) . . ?
C22 C18 C16 119.89(19) . . ?
C18 C19 H19 120.6 . . ?
C18 C19 C20 118.8(2) . . ?
C20 C19 H19 120.6 . . ?
N2 C20 C19 123.51(19) . . ?
N2 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
N2 C21 H21 118.7 . . ?
N2 C21 C22 122.7(2) . . ?
C22 C21 H21 118.7 . . ?
C18 C22 H22 120.2 . . ?
C21 C22 C18 119.6(2) . . ?
C21 C22 H22 120.2 . . ?
N3 C23 H23 118.8 . . ?
N3 C23 C24 122.49(19) . . ?
C24 C23 H23 118.8 . . ?
C23 C24 H24 120.5 . . ?
C23 C24 C25 119.01(18) . . ?
C25 C24 H24 120.5 . . ?
C24 C25 C17 120.79(18) . . ?
C24 C25 C26 118.45(18) . . ?
C26 C25 C17 120.76(18) . . ?
C25 C26 H26 120.6 . . ?
C27 C26 C25 118.78(19) . . ?
C27 C26 H26 120.6 . . ?
N3 C27 C26 123.30(18) . . ?
N3 C27 H27 118.3 . . ?
C26 C27 H27 118.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C1 O1 7.2(4) . . . . ?
Ni1 O2 C1 C2 -172.21(14) . . . . ?
Ni1 O5 C9 O6 -3.99(17) 1_455 . . . ?
Ni1 O5 C9 C6 174.39(15) 1_455 . . . ?
Ni1 O6 C9 O5 4.06(17) 1_455 . . . ?
Ni1 O6 C9 C6 -174.31(15) 1_455 . . . ?
Ni1 N2 C20 C19 176.76(18) 2_645 . . . ?
Ni1 N2 C21 C22 -177.8(2) 2_645 . . . ?
Ni1 N3 C23 C24 -174.49(16) . . . . ?
Ni1 N3 C27 C26 174.13(16) . . . . ?
Ni2 N1 C10 C11 -178.25(19) . . . . ?
Ni2 N1 C14 C13 176.05(17) . . . . ?
O1 C1 C2 C3 -162.4(2) . . . . ?
O1 C1 C2 C7 15.5(4) . . . . ?
O2 C1 C2 C3 17.1(3) . . . . ?
O2 C1 C2 C7 -165.1(2) . . . . ?
N1 C10 C11 C12 1.7(4) . . . . ?
N2 C21 C22 C18 0.6(5) . . . . ?
N3 C23 C24 C25 0.7(3) . . . . ?
N4 C16 C18 C19 7.1(3) . . . . ?
N4 C16 C18 C22 -170.7(2) . . . . ?
N5 C17 C25 C24 -177.28(19) . . . . ?
N5 C17 C25 C26 2.7(3) . . . . ?
N6 C16 C18 C19 -174.3(2) . . . . ?
N6 C16 C18 C22 7.8(3) . . . . ?
N6 C17 C25 C24 3.8(3) . . . . ?
N6 C17 C25 C26 -176.17(19) . . . . ?
C1 C2 C3 C4 178.3(2) . . . . ?
C1 C2 C7 C6 179.8(2) . . . . ?
C2 C3 C4 C5 1.4(3) . . . . ?
C2 C3 C4 C8 -176.40(19) . . . . ?
C3 C2 C7 C6 -2.4(3) . . . . ?
C3 C4 C5 C6 -1.4(3) . . . . ?
C3 C4 C8 O3 3.7(3) . . . . ?
C3 C4 C8 O4 -177.74(19) . . . . ?
C4 C5 C6 C7 -0.5(3) . . . . ?
C4 C5 C6 C9 -178.19(17) . . . . ?
C5 C4 C8 O3 -174.02(19) . . . . ?
C5 C4 C8 O4 4.5(3) . . . . ?
C5 C6 C7 C2 2.4(3) . . . . ?
C5 C6 C9 O5 -13.6(3) . . . . ?
C5 C6 C9 O6 164.76(17) . . . . ?
C7 C2 C3 C4 0.5(3) . . . . ?
C7 C6 C9 O5 168.67(17) . . . . ?
C7 C6 C9 O6 -12.9(3) . . . . ?
C8 C4 C5 C6 176.37(17) . . . . ?
C9 C6 C7 C2 -179.91(18) . . . . ?
C10 N1 C14 C13 -1.4(3) . . . . ?
C10 C11 C12 C13 -0.4(3) . . . . ?
C10 C11 C12 C15 -178.4(2) . . . . ?
C11 C12 C13 C14 -1.7(3) . . . . ?
C11 C12 C15 N4 -175.4(2) . . . . ?
C11 C12 C15 N5 6.7(3) . . . . ?
C12 C13 C14 N1 2.6(3) . . . . ?
C13 C12 C15 N4 6.5(3) . . . . ?
C13 C12 C15 N5 -171.29(19) . . . . ?
C14 N1 C10 C11 -0.8(4) . . . . ?
C15 N4 C16 N6 -1.1(3) . . . . ?
C15 N4 C16 C18 177.33(17) . . . . ?
C15 N5 C17 N6 -1.7(3) . . . . ?
C15 N5 C17 C25 179.54(17) . . . . ?
C15 C12 C13 C14 176.43(19) . . . . ?
C16 N4 C15 N5 0.7(3) . . . . ?
C16 N4 C15 C12 -176.97(17) . . . . ?
C16 N6 C17 N5 1.3(3) . . . . ?
C16 N6 C17 C25 -179.93(17) . . . . ?
C16 C18 C19 C20 -179.1(2) . . . . ?
C16 C18 C22 C21 178.6(2) . . . . ?
C17 N5 C15 N4 0.6(3) . . . . ?
C17 N5 C15 C12 178.26(17) . . . . ?
C17 N6 C16 N4 0.2(3) . . . . ?
C17 N6 C16 C18 -178.24(17) . . . . ?
C17 C25 C26 C27 179.58(19) . . . . ?
C18 C19 C20 N2 0.6(4) . . . . ?
C19 C18 C22 C21 0.7(4) . . . . ?
C20 N2 C21 C22 -1.3(4) . . . . ?
C21 N2 C20 C19 0.7(4) . . . . ?
C22 C18 C19 C20 -1.3(4) . . . . ?
C23 N3 C27 C26 0.0(3) . . . . ?
C23 C24 C25 C17 179.86(19) . . . . ?
C23 C24 C25 C26 -0.1(3) . . . . ?
C24 C25 C26 C27 -0.4(3) . . . . ?
C25 C26 C27 N3 0.5(3) . . . . ?
C27 N3 C23 C24 -0.6(3) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 488 electrons were 
found in a volume of 1729Å³ in 1 void per unit cell. 
This is consistent with the presence of 6[C3H7NO] per Formula Unit 
which account for 480 electrons per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.358 -0.730 -0.917 1729.2 487.9 '12 DMF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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 1996090'
loop_
_audit_author_name
_audit_author_address
'Bin-bin Qian'
;Nankai university
China
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-03-11 downloaded from the CCDC.
;
_audit_creation_date             2021-03-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C30.92 H21 N4 Ni3 O17, 2[C3H7NO], 0.5[H2O], 0.5[CH4O]'
_chemical_formula_sum            'C37.42 H38 N6 Ni3 O20'
_chemical_formula_weight         1067.91
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   27.1230(2)
_cell_length_b                   27.1230(2)
_cell_length_c                   38.1727(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     24319.7(4)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    18598
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.8350
_cell_measurement_theta_min      4.7260
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.835
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             9873
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            24179
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.991
_diffrn_reflns_theta_max         66.991
_diffrn_reflns_theta_min         3.473
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  34.00   0.50    5.84    --    0.00 -82.00  30.00  144
  2  ω    -37.00  -5.00   0.50    5.84    --    0.00 -82.00   0.00   64
  3  ω     94.00 185.00   0.50   23.37    --  101.30  57.00   0.00  182
  4  ω     94.00 145.00   0.50   23.37    --  101.30  19.00-180.00  102
  5  ω     94.00 191.00   0.50   23.37    --  101.30  82.00  90.00  194
  6  ω    112.00 188.00   0.50   23.37    --  101.30  82.00-150.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0374272000
_diffrn_orient_matrix_UB_12      0.0471743000
_diffrn_orient_matrix_UB_13      -0.0263021000
_diffrn_orient_matrix_UB_21      0.0484749000
_diffrn_orient_matrix_UB_22      -0.0131862000
_diffrn_orient_matrix_UB_23      0.0056303000
_diffrn_orient_matrix_UB_31      -0.0235070000
_diffrn_orient_matrix_UB_32      -0.0435828000
_diffrn_orient_matrix_UB_33      -0.0300996000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4863
_reflns_number_total             5146
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.541
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5146
_refine_ls_number_restraints     230
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0561
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0836P)²+176.0993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1591
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C21-O7
 1.5 with sigma of 0.01
3. Rigid bond restraints
 O7, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
O7 \\sim C21: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
5. Others
 Fixed Sof: C21(0.46) H21A(0.5) H21B(0.5) H21C(0.5)
6.a Rotating group:
 O1W(H1WA,H1WB)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C13(H13), C14(H14), C19(H19), C20(H20)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.68063(3) 0.84032(2) 0.26381(2) 0.01526(18) Uani 1 2 d S T P . .
Ni2 Ni 0.53637(3) 0.76819(2) 0.24301(2) 0.01786(19) Uani 1 2 d S T P . .
Ni3 Ni 0.85004(2) 0.70008(4) 0.21412(2) 0.0342(2) Uani 1 2 d S T P . .
O1 O 0.77137(10) 0.67188(11) 0.19561(7) 0.0417(6) Uani 1 1 d . . . . .
O1W O 0.69960(9) 0.90432(10) 0.30214(6) 0.0370(6) Uani 1 1 d . . . . .
H1WA H 0.732318 0.914808 0.311339 0.056 Uiso 1 1 d R U . . .
H1WB H 0.676278 0.890220 0.319367 0.056 Uiso 1 1 d R U . . .
O2 O 0.66671(8) 0.77732(8) 0.23025(5) 0.0253(4) Uani 1 1 d . . . . .
O2W O 0.46861(16) 0.73430(8) 0.20803(9) 0.0530(10) Uani 1 2 d S T P . .
O3 O 0.57406(9) 0.73301(10) 0.21535(6) 0.0340(5) Uani 1 1 d . . . . .
O3W O 0.59989(11) 0.79995(6) 0.28088(7) 0.0248(6) Uani 1 2 d S T P . .
O4 O 0.55314(14) 0.70923(17) 0.31425(10) 0.1057(18) Uani 1 1 d . . . . .
O5 O 0.49131(9) 0.69292(9) 0.27088(6) 0.0331(5) Uani 1 1 d . . . . .
O6 O 0.50086(11) 0.58040(10) 0.41395(6) 0.0408(6) Uani 1 1 d . . . . .
O7 O 0.81428(12) 0.6286(2) 0.24698(15) 0.0808(15) Uani 1 2 d DS TU P . .
N1 N 0.76462(14) 0.88231(7) 0.24948(8) 0.0187(7) Uani 1 2 d S T P . .
N2 N 0.88572(9) 0.77143(19) 0.18170(12) 0.0397(10) Uani 1 2 d S T P . .
N3 N 0.94158(19) 0.97079(10) 0.14929(12) 0.0425(10) Uani 1 2 d S T P . .
N4 N 0.97084(7) 0.94168(14) 0.23899(10) 0.0243(7) Uani 1 2 d S T P . .
C1 C 0.50565(16) 0.67958(17) 0.29884(11) 0.0508(10) Uani 1 1 d . U . . .
C2 C 0.46462(15) 0.62429(16) 0.31580(10) 0.0444(9) Uani 1 1 d . U . . .
C3 C 0.41308(13) 0.58692(13) 0.29955(15) 0.0457(13) Uani 1 2 d S TU P . .
H3 H 0.403726 0.596272 0.278076 0.055 Uiso 1 2 calc R U P . .
C4 C 0.47757(14) 0.61073(15) 0.34841(10) 0.0411(8) Uani 1 1 d . U . . .
H4 H 0.511799 0.635755 0.359287 0.049 Uiso 1 1 calc R U . . .
C5 C 0.43976(11) 0.56024(11) 0.36466(13) 0.0365(10) Uani 1 2 d S TU P . .
C6 C 0.45397(11) 0.54603(11) 0.39936(13) 0.0351(10) Uani 1 2 d S TU P . .
C7 C 0.62371(12) 0.74078(12) 0.21390(8) 0.0240(6) Uani 1 1 d . U . . .
C8 C 0.63261(13) 0.70176(13) 0.18976(8) 0.0272(6) Uani 1 1 d . U . . .
C9 C 0.58970(16) 0.666667 0.166667 0.0274(9) Uani 1 2 d S TU P . .
H9 H 0.555417 0.666669 0.166666 0.033 Uiso 1 2 calc R U P . .
C10 C 0.68343(13) 0.70082(13) 0.19025(9) 0.0304(7) Uani 1 1 d . U . . .
H10 H 0.711638 0.723040 0.206340 0.036 Uiso 1 1 calc R U . . .
C11 C 0.69219(16) 0.666667 0.166667 0.0322(9) Uani 1 2 d S TU P . .
C12 C 0.74807(16) 0.666667 0.166667 0.0338(10) Uani 1 2 d S TU P . .
C13 C 0.79351(12) 0.93916(12) 0.24662(8) 0.0229(6) Uani 1 1 d . U . . .
H13 H 0.773441 0.958666 0.247351 0.027 Uiso 1 1 calc R U . . .
C14 C 0.85184(12) 0.96990(12) 0.24264(8) 0.0258(6) Uani 1 1 d . U . . .
H14 H 0.870769 1.009406 0.241142 0.031 Uiso 1 1 calc R U . . .
C15 C 0.88176(17) 0.94088(8) 0.24091(11) 0.0223(8) Uani 1 2 d S TU P . .
C16 C 0.94475(17) 0.97238(9) 0.23894(11) 0.0240(8) Uani 1 2 d S TU P . .
C17 C 0.97227(12) 0.9445(2) 0.14944(13) 0.0406(11) Uani 1 2 d S TU P . .
C18 C 0.94098(12) 0.8820(2) 0.15561(14) 0.0413(11) Uani 1 2 d S TU P . .
C19 C 0.97048(17) 0.85324(17) 0.16097(11) 0.0462(9) Uani 1 1 d . U . . .
H19 H 1.009083 0.870351 0.155792 0.055 Uiso 1 1 calc R U . . .
C20 C 0.94129(16) 0.79855(16) 0.17419(11) 0.0440(8) Uani 1 1 d . U . . .
H20 H 0.961387 0.779575 0.178087 0.053 Uiso 1 1 calc R U . . .
C21 C 0.8356(13) 0.5929(12) 0.2630(5) 0.215(12) Uani 0.46 1 d D U P . .
H21A H 0.852403 0.580898 0.245262 0.323 Uiso 0.5 1 calc R U P . .
H21B H 0.804504 0.560001 0.273778 0.323 Uiso 0.5 1 calc R U P . .
H21C H 0.863672 0.614603 0.280486 0.323 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1W 2.127(2) . ?
Ni1 O1W 2.127(2) 24_565 ?
Ni1 O2 2.014(2) 24_565 ?
Ni1 O2 2.014(2) . ?
Ni1 O3W 2.005(3) . ?
Ni1 N1 2.047(3) . ?
Ni2 O2W 2.078(3) . ?
Ni2 O3 2.011(2) 24_565 ?
Ni2 O3 2.011(2) . ?
Ni2 O3W 2.077(3) . ?
Ni2 O5 2.073(2) . ?
Ni2 O5 2.073(2) 24_565 ?
Ni3 O1 2.001(2) 23_655 ?
Ni3 O1 2.001(2) . ?
Ni3 O6 2.135(2) 18_655 ?
Ni3 O6 2.135(2) 32 ?
Ni3 O7 2.097(6) . ?
Ni3 N2 2.084(5) . ?
Ni3 C6 2.454(5) 32 ?
O1 C12 1.245(3) . ?
O1W H1WA 0.8599 . ?
O1W H1WB 0.8585 . ?
O2 C7 1.256(4) . ?
O3 C7 1.256(4) . ?
O4 C1 1.271(5) . ?
O5 C1 1.250(4) . ?
O6 C6 1.269(3) . ?
O7 C21 1.486(9) 23_655 ?
O7 C21 1.486(9) . ?
N1 C13 1.340(3) . ?
N1 C13 1.340(3) 24_565 ?
N2 C20 1.337(5) . ?
N2 C20 1.337(5) 23_655 ?
N3 C17 1.339(4) . ?
N3 C17 1.339(4) 3_675 ?
N4 C16 1.335(3) . ?
N4 C16 1.335(3) 2_765 ?
C1 C2 1.496(5) . ?
C2 C3 1.396(4) . ?
C2 C4 1.392(5) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.381(4) . ?
C5 C6 1.484(7) . ?
C7 C8 1.511(4) . ?
C8 C9 1.389(4) . ?
C8 C10 1.391(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.395(4) . ?
C11 C12 1.516(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.379(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.386(4) . ?
C15 C16 1.482(6) . ?
C17 C18 1.489(8) . ?
C18 C19 1.383(5) 23_655 ?
C18 C19 1.383(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.381(6) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1W Ni1 O1W 88.07(15) . 24_565 ?
O2 Ni1 O1W 86.95(9) . 24_565 ?
O2 Ni1 O1W 86.95(9) 24_565 . ?
O2 Ni1 O1W 174.73(9) . . ?
O2 Ni1 O1W 174.74(10) 24_565 24_565 ?
O2 Ni1 O2 97.97(12) 24_565 . ?
O2 Ni1 N1 89.23(8) . . ?
O2 Ni1 N1 89.23(8) 24_565 . ?
O3W Ni1 O1W 88.54(8) . 24_565 ?
O3W Ni1 O1W 88.54(8) . . ?
O3W Ni1 O2 93.04(8) . 24_565 ?
O3W Ni1 O2 93.04(8) . . ?
O3W Ni1 N1 176.54(12) . . ?
N1 Ni1 O1W 88.97(9) . . ?
N1 Ni1 O1W 88.97(9) . 24_565 ?
O3 Ni2 O2W 89.99(10) . . ?
O3 Ni2 O2W 89.99(10) 24_565 . ?
O3 Ni2 O3 93.52(15) 24_565 . ?
O3 Ni2 O3W 92.82(8) . . ?
O3 Ni2 O3W 92.82(8) 24_565 . ?
O3 Ni2 O5 89.52(10) 24_565 24_565 ?
O3 Ni2 O5 175.34(9) 24_565 . ?
O3 Ni2 O5 89.52(10) . . ?
O3 Ni2 O5 175.35(9) . 24_565 ?
O3W Ni2 O2W 175.90(13) . . ?
O5 Ni2 O2W 86.48(10) 24_565 . ?
O5 Ni2 O2W 86.48(10) . . ?
O5 Ni2 O3W 90.55(8) . . ?
O5 Ni2 O3W 90.55(8) 24_565 . ?
O5 Ni2 O5 87.24(14) 24_565 . ?
O1 Ni3 O1 122.13(14) . 23_655 ?
O1 Ni3 O6 87.70(9) . 18_655 ?
O1 Ni3 O6 149.68(10) . 32 ?
O1 Ni3 O6 87.69(9) 23_655 32 ?
O1 Ni3 O6 149.67(10) 23_655 18_655 ?
O1 Ni3 O7 86.90(11) . . ?
O1 Ni3 O7 86.91(11) 23_655 . ?
O1 Ni3 N2 93.24(10) . . ?
O1 Ni3 N2 93.24(10) 23_655 . ?
O1 Ni3 C6 118.55(7) 23_655 32 ?
O1 Ni3 C6 118.55(7) . 32 ?
O6 Ni3 O6 62.14(13) 18_655 32 ?
O6 Ni3 C6 31.14(6) 18_655 32 ?
O6 Ni3 C6 31.14(6) 32 32 ?
O7 Ni3 O6 89.64(16) . 32 ?
O7 Ni3 O6 89.64(16) . 18_655 ?
O7 Ni3 C6 87.4(2) . 32 ?
N2 Ni3 O6 90.10(13) . 32 ?
N2 Ni3 O6 90.10(13) . 18_655 ?
N2 Ni3 O7 179.7(2) . . ?
N2 Ni3 C6 92.28(17) . 32 ?
C12 O1 Ni3 137.7(2) . . ?
Ni1 O1W H1WA 109.8 . . ?
Ni1 O1W H1WB 109.9 . . ?
H1WA O1W H1WB 104.1 . . ?
C7 O2 Ni1 133.78(19) . . ?
C7 O3 Ni2 134.44(19) . . ?
Ni1 O3W Ni2 116.94(13) . . ?
C1 O5 Ni2 127.4(2) . . ?
C6 O6 Ni3 88.4(2) . 33_545 ?
C21 O7 Ni3 134.3(12) 23_655 . ?
C21 O7 Ni3 134.4(12) . . ?
C21 O7 C21 91(2) 23_655 . ?
C13 N1 Ni1 120.65(17) . . ?
C13 N1 Ni1 120.65(17) 24_565 . ?
C13 N1 C13 118.3(3) . 24_565 ?
C20 N2 Ni3 120.7(2) . . ?
C20 N2 Ni3 120.7(2) 23_655 . ?
C20 N2 C20 117.0(5) . 23_655 ?
C17 N3 C17 114.8(5) . 3_675 ?
C16 N4 C16 114.6(4) . 2_765 ?
O4 C1 C2 116.4(3) . . ?
O5 C1 O4 125.2(3) . . ?
O5 C1 C2 118.5(3) . . ?
C3 C2 C1 120.6(3) . . ?
C4 C2 C1 119.5(3) . . ?
C4 C2 C3 119.9(3) . . ?
C2 C3 C2 119.4(5) . 22_665 ?
C2 C3 H3 120.3 22_665 . ?
C2 C3 H3 120.3 . . ?
C2 C4 H4 119.9 . . ?
C5 C4 C2 120.2(3) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C4 120.2(4) . 22_665 ?
C4 C5 C6 119.9(2) . . ?
C4 C5 C6 119.9(2) 22_665 . ?
O6 C6 Ni3 60.5(2) 22_665 33_545 ?
O6 C6 Ni3 60.5(2) . 33_545 ?
O6 C6 O6 120.5(4) 22_665 . ?
O6 C6 C5 119.7(2) 22_665 . ?
O6 C6 C5 119.7(2) . . ?
C5 C6 Ni3 172.6(4) . 33_545 ?
O2 C7 O3 127.3(3) . . ?
O2 C7 C8 116.4(3) . . ?
O3 C7 C8 116.3(3) . . ?
C9 C8 C7 119.6(3) . . ?
C9 C8 C10 119.6(3) . . ?
C10 C8 C7 120.8(3) . . ?
C8 C9 C8 120.6(4) . 11_565 ?
C8 C9 H9 119.7 11_565 . ?
C8 C9 H9 119.7 . . ?
C8 C10 H10 119.9 . . ?
C8 C10 C11 120.2(3) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C10 119.7(4) . 11_565 ?
C10 C11 C12 120.2(2) . . ?
C10 C11 C12 120.2(2) 11_565 . ?
O1 C12 O1 126.4(4) . 11_565 ?
O1 C12 C11 116.8(2) . . ?
O1 C12 C11 116.8(2) 11_565 . ?
N1 C13 H13 118.7 . . ?
N1 C13 C14 122.6(3) . . ?
C14 C13 H13 118.7 . . ?
C13 C14 H14 120.6 . . ?
C13 C14 C15 118.8(3) . . ?
C15 C14 H14 120.6 . . ?
C14 C15 C14 118.8(4) . 24_565 ?
C14 C15 C16 120.58(18) . . ?
C14 C15 C16 120.58(18) 24_565 . ?
N4 C16 N4 125.4(4) . 3_675 ?
N4 C16 C15 117.27(19) 3_675 . ?
N4 C16 C15 117.3(2) . . ?
N3 C17 N3 125.2(5) . 2_765 ?
N3 C17 C18 117.1(3) . . ?
N3 C17 C18 117.1(3) 2_765 . ?
C19 C18 C17 120.3(3) 23_655 . ?
C19 C18 C17 120.3(3) . . ?
C19 C18 C19 118.7(5) . 23_655 ?
C18 C19 H19 120.8 . . ?
C20 C19 C18 118.5(4) . . ?
C20 C19 H19 120.8 . . ?
N2 C20 C19 123.5(4) . . ?
N2 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
O7 C21 H21A 109.5 . . ?
O7 C21 H21B 109.5 . . ?
O7 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C7 O3 -2.2(5) . . . . ?
Ni1 O2 C7 C8 177.8(2) . . . . ?
Ni1 N1 C13 C14 169.3(2) . . . . ?
Ni2 O3 C7 O2 -2.6(5) . . . . ?
Ni2 O3 C7 C8 177.4(2) . . . . ?
Ni2 O5 C1 O4 -4.7(8) . . . . ?
Ni2 O5 C1 C2 176.0(3) . . . . ?
Ni3 O1 C12 O1 25.6(2) . . . 11_565 ?
Ni3 O1 C12 C11 -154.4(2) . . . . ?
Ni3 O6 C6 O6 7.3(5) 33_545 . . 22_665 ?
Ni3 O6 C6 C5 -171.5(5) 33_545 . . . ?
Ni3 N2 C20 C19 -162.4(3) . . . . ?
O2 C7 C8 C9 -169.6(2) . . . . ?
O2 C7 C8 C10 10.0(5) . . . . ?
O3 C7 C8 C9 10.4(4) . . . . ?
O3 C7 C8 C10 -170.0(3) . . . . ?
O4 C1 C2 C3 -175.4(6) . . . . ?
O4 C1 C2 C4 6.0(7) . . . . ?
O5 C1 C2 C3 4.0(7) . . . . ?
O5 C1 C2 C4 -174.6(4) . . . . ?
N1 C13 C14 C15 1.1(5) . . . . ?
N3 C17 C18 C19 0.1(7) 2_765 . . . ?
N3 C17 C18 C19 -0.2(7) . . . 23_655 ?
N3 C17 C18 C19 -171.0(5) . . . . ?
N3 C17 C18 C19 171.0(5) 2_765 . . 23_655 ?
C1 C2 C3 C2 179.5(4) . . . 22_665 ?
C1 C2 C4 C5 179.0(4) . . . . ?
C2 C4 C5 C4 1.1(9) . . . 22_665 ?
C2 C4 C5 C6 179.8(4) . . . . ?
C3 C2 C4 C5 0.4(7) . . . . ?
C4 C2 C3 C2 -1.9(9) . . . 22_665 ?
C4 C5 C6 O6 -178.7(5) . . . 22_665 ?
C4 C5 C6 O6 0.0(8) . . . . ?
C4 C5 C6 O6 0.0(8) 22_665 . . 22_665 ?
C4 C5 C6 O6 178.7(5) 22_665 . . . ?
C7 C8 C9 C8 178.2(3) . . . 11_565 ?
C7 C8 C10 C11 -176.9(2) . . . . ?
C8 C10 C11 C10 -1.4(2) . . . 11_565 ?
C8 C10 C11 C12 178.6(2) . . . . ?
C9 C8 C10 C11 2.7(5) . . . . ?
C10 C8 C9 C8 -1.4(2) . . . 11_565 ?
C10 C11 C12 O1 35.4(2) . . . . ?
C10 C11 C12 O1 35.4(2) 11_565 . . 11_565 ?
C10 C11 C12 O1 -144.6(2) . . . 11_565 ?
C10 C11 C12 O1 -144.6(2) 11_565 . . . ?
C13 N1 C13 C14 -3.3(6) 24_565 . . . ?
C13 C14 C15 C14 1.1(6) . . . 24_565 ?
C13 C14 C15 C16 -176.0(3) . . . . ?
C14 C15 C16 N4 0.1(6) . . . 3_675 ?
C14 C15 C16 N4 177.0(4) . . . . ?
C14 C15 C16 N4 -0.1(6) 24_565 . . . ?
C14 C15 C16 N4 -177.0(4) 24_565 . . 3_675 ?
C16 N4 C16 N4 -0.2(9) 2_765 . . 3_675 ?
C16 N4 C16 C15 -176.8(2) 2_765 . . . ?
C17 N3 C17 N3 -0.9(10) 3_675 . . 2_765 ?
C17 N3 C17 C18 169.5(3) 3_675 . . . ?
C17 C18 C19 C20 165.8(4) . . . . ?
C18 C19 C20 N2 0.9(7) . . . . ?
C19 C18 C19 C20 -5.2(8) 23_655 . . . ?
C20 N2 C20 C19 3.3(7) 23_655 . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 1694 electrons were 
found in a volume of 10541.6Å³ in 1 void per unit cell. 
This is consistent with the presence of 2[C3H7NO], 0.5[H2O], 0.5[CH4O] per Formula Unit 
which account for 1692 electrons per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.374 0.431 0.358 10541.6 1694.3 '36 DMF, 9 H2O, 9 MeOH'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.833
