# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_ea-416_acetone_auto
_database_code_depnum_ccdc_archive 'CCDC 2169986'
loop_
_audit_author_name
_audit_author_address
'Gary S Nichol'
;University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2022-05-02 deposited with the CCDC.	2022-07-05 downloaded from the CCDC.
;
_audit_creation_date             2022-05-02
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        EA-416_Acetone
_chemical_formula_moiety         'C75 H116 Cl14 N24 Ni14 O30, 4(C3 H6 O)'
_chemical_formula_sum            'C87 H140 Cl14 N24 Ni14 O34'
_chemical_formula_weight         3384.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C87 H140 Cl14 N24 Ni14 O34'
_chemical_oxdiff_usercomment     '@ 120 K ABG-0549'
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'
Cl Cl 0.1484 0.1585 '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'

_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      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'

_cell_length_a                   37.1760(2)
_cell_length_b                   37.1760(2)
_cell_length_c                   11.96640(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16538.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    94703
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      30.3920
_cell_measurement_theta_min      3.6250
_shelx_estimated_absorpt_T_max   0.853
_shelx_estimated_absorpt_T_min   0.303
_exptl_absorpt_coefficient_mu    1.841
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic light blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             6928
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0411
-1 0 0 0.0484
0 -1 2 0.4483
0 1 -2 0.3727
-2 1 -2 0.3574
0 1 0 0.0460
0 -1 0 0.0723

_exptl_crystal_preparation       
'NiCl2 and ligand in methanol has been refluxed for a day and the clear solution was layered with acetone.'
_exptl_crystal_recrystallization_method 
'The material was recrystallised from Acetone by solvent layering'
_exptl_crystal_size_max          0.851
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.089
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0005 0.0006 0.0000 0.0054 -0.0160 0.0090
-1.0005 -0.0006 -0.0000 -0.0054 0.0160 -0.0090
-0.0073 -1.0004 2.0004 -0.0256 0.0512 0.1056
0.0073 1.0004 -2.0004 0.0256 -0.0512 -0.1056
-1.9936 0.9992 -2.0004 0.0149 -0.0193 -0.1236
-0.0004 0.9998 -0.0002 0.0183 0.0052 -0.0016
0.0004 -0.9998 0.0002 -0.0183 -0.0052 0.0016

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            152030
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         3.195
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      5.00  68.00   0.30   30.00    --   14.65-124.00 -23.00  210
  2  ω     20.00  83.00   0.30   30.00    --   14.65-148.00 171.00  210
  3  ω    -43.00  19.10   0.30   30.00    --  -13.08  77.00-150.00  207
  4  ω    -21.00   7.20   0.30   30.00    --  -13.08  77.00-120.00   94
  5  ω    -42.00  10.20   0.30   30.00    --  -13.08 -77.00 -30.00  174
  6  ω    -44.00 -17.90   0.30   30.00    --   14.65 -38.00 120.00   87
  7  ω     58.00  85.00   0.30   30.00    --   14.65 178.00-150.00   90
  8  ω     38.00  87.20   0.30   30.00    --   14.65-178.00 120.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0053456000
_diffrn_orient_matrix_UB_12      0.0182744000
_diffrn_orient_matrix_UB_13      -0.0036556000
_diffrn_orient_matrix_UB_21      -0.0159544000
_diffrn_orient_matrix_UB_22      0.0052478000
_diffrn_orient_matrix_UB_23      0.0281700000
_diffrn_orient_matrix_UB_31      0.0090084000
_diffrn_orient_matrix_UB_32      -0.0015669000
_diffrn_orient_matrix_UB_33      0.0520273000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15915
_reflns_number_total             17519
_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 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         17519
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0570
_refine_ls_restrained_S_all      1.172
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0423P)²+72.7487P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1300
_refine_special_details          
'One acetone molecule was modelled as disordered.  A methanol ligand was modelled as disordered with an aqua ligand.  Geometric restraints were used.  Solvent masking was used to handle residual density corresponding with a further two molecules of acetone per formula unit.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Shared sites
{O15, O15A}
3. Restrained distances
 O15-H15
 0.87 with sigma of 0.01
 Ni5-H15
 2.623747 with sigma of 0.02
 C42-C44 \\sim C42A-C44
 with sigma of 0.02
 O17-C44 \\sim O17A-C44
 with sigma of 0.04
 O17-C43 \\sim O17A-C43
 with sigma of 0.04
 C42-C43 \\sim C42A-C43
 with sigma of 0.02
 O17-C42 \\sim O17A-C42A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O15) = Uanis(O15A)
5. Rigid body (RIGU) restrains
 O17A, C42A, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O17A)=Sof(C42A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=1-FVAR(1)
 Sof(O17)=Sof(C42)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 FVAR(1)
 Fixed Sof: O15(0.5) H15(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) O15A(0.5)
 H15A(0.5) H15B(0.5)
7.a Rotating group:
 O15A(H15A,H15B)
7.b Me refined with riding coordinates:
 C43(H43A,H43B,H43C), C43(H43D,H43E,H43F), C44(H44A,H44B,H44C), C44(H44D,H44E,
 H44F)
7.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), N8(H8), N10(H10), N12(H12), C2(H2A), C7(H7),
 C12(H12A), C17(H17), C22(H22), C27(H27), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37)
7.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C15(H15C,H15D,H15E), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
7.e Idealised tetrahedral OH refined as rotating group:
 O15(H15)
;
_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 0.05619(2) 0.64211(2) 0.26534(4) 0.01481(11) Uani 1 1 d . . . . .
Ni2 Ni 0.12564(2) 0.61027(2) 0.40115(4) 0.01459(11) Uani 1 1 d . . . . .
Ni3 Ni 0.15008(2) 0.53403(2) 0.29490(4) 0.01544(12) Uani 1 1 d . . . . .
Ni4 Ni 0.16235(2) 0.47344(2) 0.48442(5) 0.01520(12) Uani 1 1 d . . . . .
Ni5 Ni 0.12575(2) 0.39770(2) 0.41934(5) 0.01695(12) Uani 1 1 d D . . . .
Ni6 Ni 0.08517(2) 0.36072(2) 0.62809(5) 0.01654(12) Uani 1 1 d . . . . .
Ni7 Ni 0.00599(2) 0.33214(2) 0.55992(4) 0.01490(12) Uani 1 1 d . . . . .
Cl1 Cl 0.01898(3) 0.69469(3) 0.26632(9) 0.0188(2) Uani 1 1 d . . . . .
Cl2 Cl 0.11253(3) 0.67053(3) 0.33363(9) 0.0180(2) Uani 1 1 d . . . . .
Cl3 Cl 0.16972(3) 0.59555(3) 0.25792(9) 0.0199(2) Uani 1 1 d . . . . .
Cl4 Cl 0.20332(3) 0.51595(3) 0.40003(9) 0.0195(2) Uani 1 1 d . . . . .
Cl5 Cl 0.18511(3) 0.42098(3) 0.37978(9) 0.0200(2) Uani 1 1 d . . . . .
Cl6 Cl 0.14565(3) 0.35409(3) 0.55405(10) 0.0233(2) Uani 1 1 d . . . . .
Cl7 Cl 0.06341(3) 0.30372(3) 0.56251(9) 0.0187(2) Uani 1 1 d . . . . .
O1 O 0.01252(8) 0.61105(8) 0.2218(3) 0.0195(6) Uani 1 1 d . . . . .
O2 O -0.03113(7) 0.63093(7) 0.3366(2) 0.0159(6) Uani 1 1 d . . . . .
O3 O 0.04064(7) 0.63811(7) 0.4306(2) 0.0153(6) Uani 1 1 d . . . . .
O4 O 0.08776(7) 0.61460(8) 0.5229(2) 0.0179(6) Uani 1 1 d . . . . .
O5 O 0.08584(7) 0.59649(7) 0.2871(2) 0.0158(6) Uani 1 1 d . . . . .
O6 O 0.10174(8) 0.54229(8) 0.2194(3) 0.0200(6) Uani 1 1 d . . . . .
O7 O 0.13078(7) 0.55656(7) 0.4405(2) 0.0156(6) Uani 1 1 d . . . . .
O8 O 0.13602(8) 0.51306(8) 0.5698(2) 0.0186(6) Uani 1 1 d . . . . .
O9 O 0.13076(7) 0.48446(7) 0.3482(2) 0.0156(6) Uani 1 1 d . . . . .
O10 O 0.10265(8) 0.43287(8) 0.3096(3) 0.0206(6) Uani 1 1 d . . . . .
O11 O 0.12487(7) 0.43684(7) 0.5405(2) 0.0171(6) Uani 1 1 d . . . . .
O12 O 0.09586(8) 0.41173(8) 0.6854(3) 0.0205(6) Uani 1 1 d . . . . .
O13 O 0.07586(7) 0.38120(8) 0.4698(3) 0.0185(6) Uani 1 1 d . . . . .
O14 O 0.02045(8) 0.36205(8) 0.4241(2) 0.0188(6) Uani 1 1 d . . . . .
O15 O 0.12645(10) 0.36213(9) 0.2891(3) 0.0347(8) Uani 0.5 1 d D . P A 1
H15 H 0.136122 0.367252 0.227738 0.052 Uiso 0.5 1 calc DR U P A 1
C38 C 0.1183(4) 0.3249(3) 0.2919(11) 0.056(4) Uani 0.5 1 d . . P A 1
H38A H 0.096506 0.320294 0.248117 0.085 Uiso 0.5 1 calc R U P A 1
H38B H 0.114370 0.317329 0.369444 0.085 Uiso 0.5 1 calc R U P A 1
H38C H 0.138410 0.311232 0.260135 0.085 Uiso 0.5 1 calc R U P A 1
O15A O 0.12645(10) 0.36213(9) 0.2891(3) 0.0347(8) Uani 0.5 1 d . . P A 2
H15A H 0.123549 0.374450 0.229058 0.052 Uiso 0.5 1 d R U P A 2
H15B H 0.107007 0.350237 0.300411 0.052 Uiso 0.5 1 d R U P A 2
N1 N 0.07418(9) 0.64646(10) 0.1026(3) 0.0210(8) Uani 1 1 d . . . . .
N2 N 0.11021(10) 0.64462(10) 0.0838(3) 0.0217(8) Uani 1 1 d . . . . .
H2 H 0.126112 0.640518 0.136776 0.026 Uiso 1 1 calc R U . . .
N3 N 0.16579(9) 0.62306(10) 0.5125(3) 0.0213(8) Uani 1 1 d . . . . .
N4 N 0.19770(10) 0.60447(11) 0.5068(4) 0.0261(9) Uani 1 1 d . . . . .
H4 H 0.202279 0.587470 0.457611 0.031 Uiso 1 1 calc R U . . .
N5 N 0.16857(10) 0.51084(10) 0.1522(3) 0.0218(8) Uani 1 1 d . . . . .
N6 N 0.18557(10) 0.47847(10) 0.1625(3) 0.0243(8) Uani 1 1 d . . . . .
H6 H 0.190985 0.468449 0.226985 0.029 Uiso 1 1 calc R U . . .
N7 N 0.19365(9) 0.46100(9) 0.6176(3) 0.0177(7) Uani 1 1 d . . . . .
N8 N 0.20251(9) 0.42608(10) 0.6376(3) 0.0212(8) Uani 1 1 d . . . . .
H8 H 0.194015 0.407856 0.598757 0.025 Uiso 1 1 calc R U . . .
N9 N 0.09319(10) 0.34024(10) 0.7864(3) 0.0220(8) Uani 1 1 d . . . . .
N10 N 0.06760(10) 0.31830(9) 0.8321(3) 0.0196(7) Uani 1 1 d . . . . .
H10 H 0.046904 0.313419 0.799782 0.024 Uiso 1 1 calc R U . . .
N11 N -0.02056(10) 0.29481(9) 0.4660(3) 0.0209(8) Uani 1 1 d . . . . .
N12 N -0.05252(10) 0.28245(10) 0.5046(4) 0.0272(9) Uani 1 1 d . . . . .
H12 H -0.062104 0.289154 0.568515 0.033 Uiso 1 1 calc R U . . .
C1 C 0.11899(13) 0.64968(13) -0.0233(4) 0.0274(10) Uani 1 1 d . . . . .
C2 C 0.08714(15) 0.6548(2) -0.0779(5) 0.0490(17) Uani 1 1 d . . . . .
H2A H 0.083988 0.659126 -0.155517 0.059 Uiso 1 1 calc R U . . .
C3 C 0.06023(14) 0.65245(18) 0.0025(4) 0.0397(14) Uani 1 1 d . . . . .
C4 C 0.15712(13) 0.65045(16) -0.0611(4) 0.0357(12) Uani 1 1 d . . . . .
H4A H 0.160465 0.633019 -0.121680 0.053 Uiso 1 1 calc R U . . .
H4B H 0.172912 0.644218 0.001524 0.053 Uiso 1 1 calc R U . . .
H4C H 0.163077 0.674608 -0.088132 0.053 Uiso 1 1 calc R U . . .
C5 C 0.02029(17) 0.6564(3) -0.0120(6) 0.093(4) Uani 1 1 d . . . . .
H5A H 0.015127 0.678517 -0.053397 0.140 Uiso 1 1 calc R U . . .
H5B H 0.008737 0.657437 0.061503 0.140 Uiso 1 1 calc R U . . .
H5C H 0.010942 0.635674 -0.053679 0.140 Uiso 1 1 calc R U . . .
C6 C 0.22111(12) 0.61547(13) 0.5856(4) 0.0290(11) Uani 1 1 d . . . . .
C7 C 0.20433(13) 0.64146(15) 0.6448(4) 0.0340(12) Uani 1 1 d . . . . .
H7 H 0.214003 0.654332 0.706451 0.041 Uiso 1 1 calc R U . . .
C8 C 0.16988(13) 0.64594(13) 0.5983(4) 0.0275(10) Uani 1 1 d . . . . .
C9 C 0.25797(14) 0.59964(18) 0.5928(6) 0.0477(15) Uani 1 1 d . . . . .
H9A H 0.257606 0.575078 0.563065 0.072 Uiso 1 1 calc R U . . .
H9B H 0.265752 0.599138 0.671035 0.072 Uiso 1 1 calc R U . . .
H9C H 0.274739 0.614310 0.549034 0.072 Uiso 1 1 calc R U . . .
C10 C 0.14084(14) 0.67140(15) 0.6314(5) 0.0372(12) Uani 1 1 d . . . . .
H10A H 0.129013 0.680789 0.564226 0.056 Uiso 1 1 calc R U . . .
H10B H 0.151252 0.691376 0.673908 0.056 Uiso 1 1 calc R U . . .
H10C H 0.123138 0.658800 0.677741 0.056 Uiso 1 1 calc R U . . .
C11 C 0.16606(15) 0.51689(14) 0.0425(4) 0.0336(12) Uani 1 1 d . . . . .
C12 C 0.18088(16) 0.48800(15) -0.0152(5) 0.0403(13) Uani 1 1 d . . . . .
H12A H 0.182306 0.485500 -0.094059 0.048 Uiso 1 1 calc R U . . .
C13 C 0.19308(13) 0.46369(13) 0.0628(4) 0.0297(11) Uani 1 1 d . . . . .
C14 C 0.14853(19) 0.54972(15) -0.0041(5) 0.0441(15) Uani 1 1 d . . . . .
H14A H 0.159694 0.555873 -0.075812 0.066 Uiso 1 1 calc R U . . .
H14B H 0.151547 0.569779 0.048198 0.066 Uiso 1 1 calc R U . . .
H14C H 0.122835 0.545086 -0.015397 0.066 Uiso 1 1 calc R U . . .
C15 C 0.21094(15) 0.42792(14) 0.0542(5) 0.0388(13) Uani 1 1 d . . . . .
H15C H 0.236785 0.431285 0.041878 0.058 Uiso 1 1 calc R U . . .
H15D H 0.200626 0.414478 -0.008517 0.058 Uiso 1 1 calc R U . . .
H15E H 0.207166 0.414469 0.123665 0.058 Uiso 1 1 calc R U . . .
C16 C 0.22570(11) 0.42249(12) 0.7233(4) 0.0210(9) Uani 1 1 d . . . . .
C17 C 0.23192(11) 0.45652(12) 0.7631(4) 0.0207(9) Uani 1 1 d . . . . .
H17 H 0.247036 0.462975 0.823862 0.025 Uiso 1 1 calc R U . . .
C18 C 0.21145(11) 0.48001(12) 0.6960(4) 0.0204(9) Uani 1 1 d . . . . .
C19 C 0.24040(12) 0.38655(12) 0.7564(4) 0.0266(10) Uani 1 1 d . . . . .
H19A H 0.233756 0.381393 0.833968 0.040 Uiso 1 1 calc R U . . .
H19B H 0.266666 0.386787 0.749403 0.040 Uiso 1 1 calc R U . . .
H19C H 0.230406 0.367941 0.707357 0.040 Uiso 1 1 calc R U . . .
C20 C 0.20869(13) 0.52001(12) 0.7046(4) 0.0268(10) Uani 1 1 d . . . . .
H20A H 0.212477 0.530752 0.630782 0.040 Uiso 1 1 calc R U . . .
H20B H 0.227017 0.528948 0.756533 0.040 Uiso 1 1 calc R U . . .
H20C H 0.184751 0.526572 0.732257 0.040 Uiso 1 1 calc R U . . .
C21 C 0.12001(13) 0.34023(14) 0.8609(4) 0.0300(11) Uani 1 1 d . . . . .
C22 C 0.11110(15) 0.31862(15) 0.9527(5) 0.0376(12) Uani 1 1 d . . . . .
H22 H 0.125491 0.314272 1.016848 0.045 Uiso 1 1 calc R U . . .
C23 C 0.07760(13) 0.30503(12) 0.9317(4) 0.0255(10) Uani 1 1 d . . . . .
C24 C 0.15372(15) 0.36080(19) 0.8428(5) 0.0487(16) Uani 1 1 d . . . . .
H24A H 0.148082 0.386443 0.835618 0.073 Uiso 1 1 calc R U . . .
H24B H 0.165473 0.352362 0.774336 0.073 Uiso 1 1 calc R U . . .
H24C H 0.169877 0.357167 0.906530 0.073 Uiso 1 1 calc R U . . .
C25 C 0.05383(15) 0.28068(13) 0.9994(4) 0.0322(11) Uani 1 1 d . . . . .
H25A H 0.044177 0.293975 1.063446 0.048 Uiso 1 1 calc R U . . .
H25B H 0.067875 0.260101 1.026162 0.048 Uiso 1 1 calc R U . . .
H25C H 0.033940 0.272082 0.952777 0.048 Uiso 1 1 calc R U . . .
C26 C -0.01609(12) 0.27854(12) 0.3664(4) 0.0229(9) Uani 1 1 d . . . . .
C27 C -0.04555(14) 0.25600(13) 0.3444(4) 0.0312(11) Uani 1 1 d . . . . .
H27 H -0.049200 0.241625 0.279711 0.037 Uiso 1 1 calc R U . . .
C28 C -0.06792(13) 0.25889(13) 0.4345(5) 0.0310(11) Uani 1 1 d . . . . .
C29 C 0.01635(13) 0.28528(13) 0.2954(4) 0.0289(10) Uani 1 1 d . . . . .
H29A H 0.012448 0.306840 0.249838 0.043 Uiso 1 1 calc R U . . .
H29B H 0.020452 0.264557 0.246384 0.043 Uiso 1 1 calc R U . . .
H29C H 0.037398 0.288857 0.343412 0.043 Uiso 1 1 calc R U . . .
C30 C -0.10280(16) 0.24101(16) 0.4625(6) 0.0484(16) Uani 1 1 d . . . . .
H30A H -0.115068 0.233974 0.393392 0.073 Uiso 1 1 calc R U . . .
H30B H -0.118029 0.257752 0.504493 0.073 Uiso 1 1 calc R U . . .
H30C H -0.098170 0.219576 0.507971 0.073 Uiso 1 1 calc R U . . .
C31 C -0.01893(11) 0.61157(11) 0.2575(4) 0.0196(9) Uani 1 1 d . . . . .
H31 H -0.035558 0.595878 0.222071 0.024 Uiso 1 1 calc R U . . .
C32 C 0.05704(11) 0.62717(11) 0.5178(4) 0.0177(8) Uani 1 1 d . . . . .
H32 H 0.044247 0.628870 0.586334 0.021 Uiso 1 1 calc R U . . .
C33 C 0.08197(11) 0.56909(11) 0.2241(4) 0.0189(9) Uani 1 1 d . . . . .
H33 H 0.061755 0.569235 0.175520 0.023 Uiso 1 1 calc R U . . .
C34 C 0.12787(11) 0.54377(11) 0.5388(4) 0.0178(8) Uani 1 1 d . . . . .
H34 H 0.118438 0.559460 0.594158 0.021 Uiso 1 1 calc R U . . .
C35 C 0.10939(11) 0.46478(11) 0.2924(4) 0.0184(8) Uani 1 1 d . . . . .
H35 H 0.097397 0.475812 0.231300 0.022 Uiso 1 1 calc R U . . .
C36 C 0.11229(11) 0.43645(12) 0.6390(4) 0.0207(9) Uani 1 1 d . . . . .
H36 H 0.115931 0.457605 0.682039 0.025 Uiso 1 1 calc R U . . .
C37 C 0.04906(12) 0.37784(11) 0.4047(4) 0.0201(9) Uani 1 1 d . . . . .
H37 H 0.051238 0.388663 0.333123 0.024 Uiso 1 1 calc R U . . .
O16 O 0.12776(16) 0.39819(18) 0.0916(5) 0.0822(17) Uani 1 1 d . . . . .
C39 C 0.0979(2) 0.4080(3) 0.0475(7) 0.071(2) Uani 1 1 d . . . . .
C40 C 0.0970(3) 0.4379(3) -0.0302(8) 0.103(4) Uani 1 1 d . . . . .
H40A H 0.117553 0.453804 -0.016013 0.154 Uiso 1 1 calc R U . . .
H40B H 0.074593 0.451416 -0.020225 0.154 Uiso 1 1 calc R U . . .
H40C H 0.098299 0.428798 -0.106966 0.154 Uiso 1 1 calc R U . . .
C41 C 0.0644(2) 0.3894(3) 0.0751(7) 0.075(2) Uani 1 1 d . . . . .
H41A H 0.055690 0.376400 0.009232 0.112 Uiso 1 1 calc R U . . .
H41B H 0.046362 0.406982 0.098778 0.112 Uiso 1 1 calc R U . . .
H41C H 0.068839 0.372271 0.135927 0.112 Uiso 1 1 calc R U . . .
O17 O 0.2695(2) 0.7030(3) 0.2920(11) 0.134(5) Uani 0.793(10) 1 d D . P B 1
O17A O 0.2018(9) 0.7576(6) 0.320(3) 0.128(12) Uani 0.207(10) 1 d D . P B 2
C42 C 0.2374(3) 0.7016(2) 0.2935(10) 0.071(3) Uani 0.793(10) 1 d D . P B 1
C42A C 0.2065(13) 0.7264(7) 0.3001(19) 0.103(12) Uani 0.207(10) 1 d D . P B 2
C43 C 0.2118(4) 0.7032(4) 0.1954(11) 0.131(4) Uani 1 1 d D . . . .
H43A H 0.186964 0.701469 0.222508 0.197 Uiso 0.793(10) 1 calc R U P B 1
H43B H 0.215016 0.726054 0.155757 0.197 Uiso 0.793(10) 1 calc R U P B 1
H43C H 0.216777 0.683196 0.144509 0.197 Uiso 0.793(10) 1 calc R U P B 1
H43D H 0.214873 0.678020 0.217445 0.197 Uiso 0.207(10) 1 calc R U P B 2
H43E H 0.190635 0.705444 0.147039 0.197 Uiso 0.207(10) 1 calc R U P B 2
H43F H 0.233195 0.711379 0.154954 0.197 Uiso 0.207(10) 1 calc R U P B 2
C44 C 0.2166(3) 0.7049(4) 0.4021(10) 0.140(5) Uani 1 1 d D . . . .
H44A H 0.190747 0.703164 0.386728 0.209 Uiso 0.793(10) 1 calc R U P B 1
H44B H 0.223730 0.685481 0.452816 0.209 Uiso 0.793(10) 1 calc R U P B 1
H44C H 0.221845 0.728179 0.436850 0.209 Uiso 0.793(10) 1 calc R U P B 1
H44D H 0.220106 0.679668 0.381029 0.209 Uiso 0.207(10) 1 calc R U P B 2
H44E H 0.238910 0.714441 0.433966 0.209 Uiso 0.207(10) 1 calc R U P B 2
H44F H 0.197273 0.706586 0.457579 0.209 Uiso 0.207(10) 1 calc R U P B 2


_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 Cl1 2.3946(11) . ?
Ni1 Cl2 2.4841(11) . ?
Ni1 O1 2.059(3) . ?
Ni1 O3 2.066(3) . ?
Ni1 O5 2.039(3) . ?
Ni1 N1 2.066(4) . ?
Ni2 Cl2 2.4305(11) . ?
Ni2 Cl3 2.4335(11) . ?
Ni2 O4 2.033(3) . ?
Ni2 O5 2.077(3) . ?
Ni2 O7 2.060(3) . ?
Ni2 N3 2.056(4) . ?
Ni3 Cl3 2.4412(11) . ?
Ni3 Cl4 2.4396(11) . ?
Ni3 O6 2.034(3) . ?
Ni3 O7 2.062(3) . ?
Ni3 O9 2.078(3) . ?
Ni3 N5 2.033(4) . ?
Ni4 Cl4 2.4162(11) . ?
Ni4 Cl5 2.4673(11) . ?
Ni4 O8 2.043(3) . ?
Ni4 O9 2.051(3) . ?
Ni4 O11 2.060(3) . ?
Ni4 N7 2.027(4) . ?
Ni5 Cl5 2.4173(11) . ?
Ni5 Cl6 2.4029(12) . ?
Ni5 O10 2.043(3) . ?
Ni5 O11 2.054(3) . ?
Ni5 O13 2.044(3) . ?
Ni5 O15 2.044(3) . ?
Ni5 O15A 2.044(3) . ?
Ni6 Cl6 2.4292(11) . ?
Ni6 Cl7 2.4002(11) . ?
Ni6 O2 2.076(3) 5_566 ?
Ni6 O12 2.055(3) . ?
Ni6 O13 2.071(3) . ?
Ni6 N9 2.064(4) . ?
Ni7 Cl1 2.4859(11) 5_566 ?
Ni7 Cl7 2.3823(11) . ?
Ni7 O2 2.072(3) 5_566 ?
Ni7 O3 2.059(3) 5_566 ?
Ni7 O14 2.041(3) . ?
Ni7 N11 2.041(4) . ?
O1 C31 1.246(5) . ?
O2 C31 1.272(5) . ?
O3 C32 1.275(5) . ?
O4 C32 1.235(5) . ?
O5 C33 1.275(5) . ?
O6 C33 1.239(5) . ?
O7 C34 1.273(5) . ?
O8 C34 1.238(5) . ?
O9 C35 1.269(5) . ?
O10 C35 1.230(5) . ?
O11 C36 1.268(5) . ?
O12 C36 1.236(5) . ?
O13 C37 1.271(5) . ?
O14 C37 1.237(5) . ?
O15 H15 0.8400 . ?
O15 C38 1.418(11) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O15A H15A 0.8593 . ?
O15A H15B 0.8578 . ?
N1 N2 1.360(5) . ?
N1 C3 1.324(6) . ?
N2 H2 0.8800 . ?
N2 C1 1.336(6) . ?
N3 N4 1.375(5) . ?
N3 C8 1.342(6) . ?
N4 H4 0.8800 . ?
N4 C6 1.347(6) . ?
N5 N6 1.365(5) . ?
N5 C11 1.335(6) . ?
N6 H6 0.8800 . ?
N6 C13 1.343(6) . ?
N7 N8 1.360(5) . ?
N7 C18 1.348(6) . ?
N8 H8 0.8800 . ?
N8 C16 1.346(6) . ?
N9 N10 1.367(5) . ?
N9 C21 1.337(6) . ?
N10 H10 0.8800 . ?
N10 C23 1.343(6) . ?
N11 N12 1.355(5) . ?
N11 C26 1.347(6) . ?
N12 H12 0.8800 . ?
N12 C28 1.341(6) . ?
C1 C2 1.366(7) . ?
C1 C4 1.488(7) . ?
C2 H2A 0.9500 . ?
C2 C3 1.390(7) . ?
C3 C5 1.502(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.351(8) . ?
C6 C9 1.494(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.406(7) . ?
C8 C10 1.490(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.391(7) . ?
C11 C14 1.492(7) . ?
C12 H12A 0.9500 . ?
C12 C13 1.376(8) . ?
C13 C15 1.490(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15C 0.9800 . ?
C15 H15D 0.9800 . ?
C15 H15E 0.9800 . ?
C16 C17 1.372(6) . ?
C16 C19 1.497(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.409(6) . ?
C18 C20 1.494(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.401(7) . ?
C21 C24 1.484(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.367(7) . ?
C23 C25 1.502(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.404(6) . ?
C26 C29 1.496(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.367(7) . ?
C28 C30 1.495(7) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
O16 C39 1.282(10) . ?
C39 C40 1.451(12) . ?
C39 C41 1.460(11) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
O17 C42 1.197(12) . ?
O17A C42A 1.20(2) . ?
C42 C43 1.511(16) . ?
C42 C44 1.517(15) . ?
C42A C43 1.53(2) . ?
C42A C44 1.51(2) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 H43D 0.9800 . ?
C43 H43E 0.9800 . ?
C43 H43F 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C44 H44D 0.9800 . ?
C44 H44E 0.9800 . ?
C44 H44F 0.9800 . ?

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
Cl1 Ni1 Cl2 97.95(4) . . ?
O1 Ni1 Cl1 90.20(9) . . ?
O1 Ni1 Cl2 170.56(9) . . ?
O1 Ni1 O3 88.95(12) . . ?
O1 Ni1 N1 93.46(14) . . ?
O3 Ni1 Cl1 83.82(8) . . ?
O3 Ni1 Cl2 87.22(8) . . ?
O5 Ni1 Cl1 172.06(9) . . ?
O5 Ni1 Cl2 81.72(8) . . ?
O5 Ni1 O1 89.54(11) . . ?
O5 Ni1 O3 88.24(11) . . ?
O5 Ni1 N1 90.60(13) . . ?
N1 Ni1 Cl1 97.33(10) . . ?
N1 Ni1 Cl2 90.22(11) . . ?
N1 Ni1 O3 177.32(13) . . ?
Cl2 Ni2 Cl3 96.21(4) . . ?
O4 Ni2 Cl2 91.52(9) . . ?
O4 Ni2 Cl3 171.52(9) . . ?
O4 Ni2 O5 89.82(11) . . ?
O4 Ni2 O7 88.69(11) . . ?
O4 Ni2 N3 91.16(13) . . ?
O5 Ni2 Cl2 82.30(8) . . ?
O5 Ni2 Cl3 87.79(8) . . ?
O7 Ni2 Cl2 170.98(9) . . ?
O7 Ni2 Cl3 83.13(8) . . ?
O7 Ni2 O5 88.68(11) . . ?
N3 Ni2 Cl2 98.51(11) . . ?
N3 Ni2 Cl3 91.12(11) . . ?
N3 Ni2 O5 178.71(13) . . ?
N3 Ni2 O7 90.51(13) . . ?
Cl4 Ni3 Cl3 96.25(4) . . ?
O6 Ni3 Cl3 92.42(9) . . ?
O6 Ni3 Cl4 170.79(9) . . ?
O6 Ni3 O7 90.36(11) . . ?
O6 Ni3 O9 87.98(11) . . ?
O7 Ni3 Cl3 82.91(8) . . ?
O7 Ni3 Cl4 87.63(8) . . ?
O7 Ni3 O9 88.91(11) . . ?
O9 Ni3 Cl3 171.81(9) . . ?
O9 Ni3 Cl4 82.99(8) . . ?
N5 Ni3 Cl3 98.27(11) . . ?
N5 Ni3 Cl4 92.41(11) . . ?
N5 Ni3 O6 89.42(14) . . ?
N5 Ni3 O7 178.81(13) . . ?
N5 Ni3 O9 89.91(13) . . ?
Cl4 Ni4 Cl5 95.09(4) . . ?
O8 Ni4 Cl4 92.26(9) . . ?
O8 Ni4 Cl5 171.22(9) . . ?
O8 Ni4 O9 88.81(12) . . ?
O8 Ni4 O11 89.38(11) . . ?
O9 Ni4 Cl4 84.14(8) . . ?
O9 Ni4 Cl5 87.18(8) . . ?
O9 Ni4 O11 90.20(11) . . ?
O11 Ni4 Cl4 174.07(9) . . ?
O11 Ni4 Cl5 82.83(8) . . ?
N7 Ni4 Cl4 96.66(10) . . ?
N7 Ni4 Cl5 91.26(11) . . ?
N7 Ni4 O8 92.64(13) . . ?
N7 Ni4 O9 178.31(13) . . ?
N7 Ni4 O11 88.95(13) . . ?
Cl6 Ni5 Cl5 95.27(4) . . ?
O10 Ni5 Cl5 91.64(9) . . ?
O10 Ni5 Cl6 173.07(9) . . ?
O10 Ni5 O11 89.63(12) . . ?
O10 Ni5 O13 90.02(12) . . ?
O10 Ni5 O15 85.95(14) . . ?
O10 Ni5 O15A 85.95(14) . . ?
O11 Ni5 Cl5 84.21(8) . . ?
O11 Ni5 Cl6 90.54(9) . . ?
O13 Ni5 Cl5 173.40(9) . . ?
O13 Ni5 Cl6 83.05(9) . . ?
O13 Ni5 O11 89.41(11) . . ?
O15 Ni5 Cl5 94.06(10) . . ?
O15 Ni5 Cl6 94.07(11) . . ?
O15 Ni5 O11 175.21(13) . . ?
O15 Ni5 O13 92.43(13) . . ?
O15A Ni5 Cl5 94.06(10) . . ?
O15A Ni5 Cl6 94.07(11) . . ?
O15A Ni5 O11 175.21(13) . . ?
O15A Ni5 O13 92.43(13) . . ?
Cl7 Ni6 Cl6 95.92(4) . . ?
O2 Ni6 Cl6 170.05(9) 5_566 . ?
O2 Ni6 Cl7 82.67(8) 5_566 . ?
O12 Ni6 Cl6 92.09(9) . . ?
O12 Ni6 Cl7 171.44(9) . . ?
O12 Ni6 O2 88.92(11) . 5_566 ?
O12 Ni6 O13 89.90(12) . . ?
O12 Ni6 N9 90.35(14) . . ?
O13 Ni6 Cl6 81.86(8) . . ?
O13 Ni6 Cl7 88.24(9) . . ?
O13 Ni6 O2 88.25(11) . 5_566 ?
N9 Ni6 Cl6 99.43(11) . . ?
N9 Ni6 Cl7 91.32(11) . . ?
N9 Ni6 O2 90.46(13) . 5_566 ?
N9 Ni6 O13 178.68(13) . . ?
Cl7 Ni7 Cl1 98.38(4) . 5_566 ?
O2 Ni7 Cl1 86.24(8) 5_566 5_566 ?
O2 Ni7 Cl7 83.21(8) 5_566 . ?
O3 Ni7 Cl1 81.67(8) 5_566 5_566 ?
O3 Ni7 Cl7 172.68(9) 5_566 . ?
O3 Ni7 O2 89.49(11) 5_566 5_566 ?
O14 Ni7 Cl1 169.36(9) . 5_566 ?
O14 Ni7 Cl7 90.92(9) . . ?
O14 Ni7 O2 89.76(12) . 5_566 ?
O14 Ni7 O3 88.44(11) . 5_566 ?
N11 Ni7 Cl1 90.42(11) . 5_566 ?
N11 Ni7 Cl7 97.98(11) . . ?
N11 Ni7 O2 176.59(13) . 5_566 ?
N11 Ni7 O3 89.34(13) . 5_566 ?
N11 Ni7 O14 93.41(13) . . ?
Ni1 Cl1 Ni7 83.82(3) . 5_566 ?
Ni2 Cl2 Ni1 83.48(3) . . ?
Ni2 Cl3 Ni3 83.21(3) . . ?
Ni4 Cl4 Ni3 83.36(3) . . ?
Ni5 Cl5 Ni4 82.56(3) . . ?
Ni5 Cl6 Ni6 83.75(4) . . ?
Ni7 Cl7 Ni6 85.11(4) . . ?
C31 O1 Ni1 130.1(3) . . ?
Ni7 O2 Ni6 102.47(12) 5_566 5_566 ?
C31 O2 Ni6 125.5(3) . 5_566 ?
C31 O2 Ni7 131.2(3) . 5_566 ?
Ni7 O3 Ni1 104.44(12) 5_566 . ?
C32 O3 Ni1 132.3(3) . . ?
C32 O3 Ni7 121.9(3) . 5_566 ?
C32 O4 Ni2 129.4(3) . . ?
Ni1 O5 Ni2 105.29(12) . . ?
C33 O5 Ni1 121.9(3) . . ?
C33 O5 Ni2 131.7(3) . . ?
C33 O6 Ni3 128.7(3) . . ?
Ni2 O7 Ni3 103.48(12) . . ?
C34 O7 Ni2 124.4(3) . . ?
C34 O7 Ni3 131.2(3) . . ?
C34 O8 Ni4 129.2(3) . . ?
Ni4 O9 Ni3 102.89(12) . . ?
C35 O9 Ni3 124.5(3) . . ?
C35 O9 Ni4 131.4(3) . . ?
C35 O10 Ni5 129.7(3) . . ?
Ni5 O11 Ni4 103.14(13) . . ?
C36 O11 Ni4 124.0(3) . . ?
C36 O11 Ni5 130.8(3) . . ?
C36 O12 Ni6 129.2(3) . . ?
Ni5 O13 Ni6 103.22(13) . . ?
C37 O13 Ni5 124.1(3) . . ?
C37 O13 Ni6 130.9(3) . . ?
C37 O14 Ni7 129.4(3) . . ?
Ni5 O15 H15 121.7 . . ?
C38 O15 Ni5 127.7(6) . . ?
C38 O15 H15 109.5 . . ?
O15 C38 H38A 109.5 . . ?
O15 C38 H38B 109.5 . . ?
O15 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Ni5 O15A H15A 106.9 . . ?
Ni5 O15A H15B 101.7 . . ?
H15A O15A H15B 107.5 . . ?
N2 N1 Ni1 118.1(3) . . ?
C3 N1 Ni1 137.7(3) . . ?
C3 N1 N2 104.2(4) . . ?
N1 N2 H2 123.5 . . ?
C1 N2 N1 113.1(4) . . ?
C1 N2 H2 123.5 . . ?
N4 N3 Ni2 118.6(3) . . ?
C8 N3 Ni2 136.4(3) . . ?
C8 N3 N4 105.0(4) . . ?
N3 N4 H4 124.1 . . ?
C6 N4 N3 111.7(4) . . ?
C6 N4 H4 124.1 . . ?
N6 N5 Ni3 117.0(3) . . ?
C11 N5 Ni3 137.0(3) . . ?
C11 N5 N6 105.6(4) . . ?
N5 N6 H6 123.9 . . ?
C13 N6 N5 112.1(4) . . ?
C13 N6 H6 123.9 . . ?
N8 N7 Ni4 119.6(3) . . ?
C18 N7 Ni4 135.2(3) . . ?
C18 N7 N8 105.0(3) . . ?
N7 N8 H8 123.7 . . ?
C16 N8 N7 112.5(4) . . ?
C16 N8 H8 123.7 . . ?
N10 N9 Ni6 119.1(3) . . ?
C21 N9 Ni6 136.0(3) . . ?
C21 N9 N10 104.6(4) . . ?
N9 N10 H10 123.8 . . ?
C23 N10 N9 112.4(4) . . ?
C23 N10 H10 123.8 . . ?
N12 N11 Ni7 117.8(3) . . ?
C26 N11 Ni7 137.2(3) . . ?
C26 N11 N12 104.9(4) . . ?
N11 N12 H12 123.7 . . ?
C28 N12 N11 112.5(4) . . ?
C28 N12 H12 123.7 . . ?
N2 C1 C2 105.5(4) . . ?
N2 C1 C4 121.8(4) . . ?
C2 C1 C4 132.6(5) . . ?
C1 C2 H2A 126.7 . . ?
C1 C2 C3 106.5(5) . . ?
C3 C2 H2A 126.7 . . ?
N1 C3 C2 110.8(4) . . ?
N1 C3 C5 120.5(5) . . ?
C2 C3 C5 128.7(5) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 C7 106.6(4) . . ?
N4 C6 C9 120.9(5) . . ?
C7 C6 C9 132.5(5) . . ?
C6 C7 H7 126.3 . . ?
C6 C7 C8 107.3(4) . . ?
C8 C7 H7 126.3 . . ?
N3 C8 C7 109.3(4) . . ?
N3 C8 C10 121.6(4) . . ?
C7 C8 C10 129.0(5) . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 C12 109.3(5) . . ?
N5 C11 C14 122.4(5) . . ?
C12 C11 C14 128.3(5) . . ?
C11 C12 H12A 126.2 . . ?
C13 C12 C11 107.5(5) . . ?
C13 C12 H12A 126.2 . . ?
N6 C13 C12 105.4(4) . . ?
N6 C13 C15 121.2(5) . . ?
C12 C13 C15 133.4(5) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15C 109.5 . . ?
C13 C15 H15D 109.5 . . ?
C13 C15 H15E 109.5 . . ?
H15C C15 H15D 109.5 . . ?
H15C C15 H15E 109.5 . . ?
H15D C15 H15E 109.5 . . ?
N8 C16 C17 106.3(4) . . ?
N8 C16 C19 121.6(4) . . ?
C17 C16 C19 132.1(4) . . ?
C16 C17 H17 126.8 . . ?
C16 C17 C18 106.4(4) . . ?
C18 C17 H17 126.8 . . ?
N7 C18 C17 109.7(4) . . ?
N7 C18 C20 122.4(4) . . ?
C17 C18 C20 127.9(4) . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N9 C21 C22 110.2(4) . . ?
N9 C21 C24 122.2(5) . . ?
C22 C21 C24 127.6(5) . . ?
C21 C22 H22 126.8 . . ?
C23 C22 C21 106.5(5) . . ?
C23 C22 H22 126.8 . . ?
N10 C23 C22 106.2(4) . . ?
N10 C23 C25 122.5(4) . . ?
C22 C23 C25 131.3(5) . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N11 C26 C27 109.8(4) . . ?
N11 C26 C29 121.8(4) . . ?
C27 C26 C29 128.5(4) . . ?
C26 C27 H27 126.9 . . ?
C28 C27 C26 106.2(4) . . ?
C28 C27 H27 126.9 . . ?
N12 C28 C27 106.5(4) . . ?
N12 C28 C30 121.4(5) . . ?
C27 C28 C30 132.0(5) . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O1 C31 O2 126.8(4) . . ?
O1 C31 H31 116.6 . . ?
O2 C31 H31 116.6 . . ?
O3 C32 H32 116.5 . . ?
O4 C32 O3 127.1(4) . . ?
O4 C32 H32 116.5 . . ?
O5 C33 H33 116.5 . . ?
O6 C33 O5 127.0(4) . . ?
O6 C33 H33 116.5 . . ?
O7 C34 H34 116.5 . . ?
O8 C34 O7 126.9(4) . . ?
O8 C34 H34 116.5 . . ?
O9 C35 H35 116.7 . . ?
O10 C35 O9 126.6(4) . . ?
O10 C35 H35 116.7 . . ?
O11 C36 H36 116.2 . . ?
O12 C36 O11 127.5(4) . . ?
O12 C36 H36 116.2 . . ?
O13 C37 H37 116.3 . . ?
O14 C37 O13 127.3(4) . . ?
O14 C37 H37 116.3 . . ?
O16 C39 C40 120.1(8) . . ?
O16 C39 C41 120.6(8) . . ?
C40 C39 C41 119.3(9) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O17 C42 C43 128.0(12) . . ?
O17 C42 C44 121.2(13) . . ?
C43 C42 C44 110.0(9) . . ?
O17A C42A C43 136(3) . . ?
O17A C42A C44 113(2) . . ?
C44 C42A C43 109.4(15) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
C42A C43 H43D 109.5 . . ?
C42A C43 H43E 109.5 . . ?
C42A C43 H43F 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
H43D C43 H43E 109.5 . . ?
H43D C43 H43F 109.5 . . ?
H43E C43 H43F 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
C42A C44 H44D 109.5 . . ?
C42A C44 H44E 109.5 . . ?
C42A C44 H44F 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
H44D C44 H44E 109.5 . . ?
H44D C44 H44F 109.5 . . ?
H44E C44 H44F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O15 H15 O16 0.84 2.02 2.718(7) 140.3 . yes
O15A H15A O16 0.86 1.87 2.718(7) 167.3 . yes

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 O1 C31 O2 -4.3(7) . . . . ?
Ni1 O3 C32 O4 -2.5(6) . . . . ?
Ni1 O5 C33 O6 168.9(3) . . . . ?
Ni1 N1 N2 C1 -176.6(3) . . . . ?
Ni1 N1 C3 C2 175.8(4) . . . . ?
Ni1 N1 C3 C5 -3.2(11) . . . . ?
Ni2 O4 C32 O3 6.0(6) . . . . ?
Ni2 O5 C33 O6 2.9(7) . . . . ?
Ni2 O7 C34 O8 -168.0(3) . . . . ?
Ni2 N3 N4 C6 -179.2(3) . . . . ?
Ni2 N3 C8 C7 178.6(4) . . . . ?
Ni2 N3 C8 C10 -2.1(8) . . . . ?
Ni3 O6 C33 O5 -7.7(7) . . . . ?
Ni3 O7 C34 O8 -1.1(6) . . . . ?
Ni3 O9 C35 O10 165.1(3) . . . . ?
Ni3 N5 N6 C13 173.0(3) . . . . ?
Ni3 N5 C11 C12 -171.6(4) . . . . ?
Ni3 N5 C11 C14 6.6(8) . . . . ?
Ni4 O8 C34 O7 8.2(6) . . . . ?
Ni4 O9 C35 O10 0.1(7) . . . . ?
Ni4 O11 C36 O12 -163.9(3) . . . . ?
Ni4 N7 N8 C16 174.9(3) . . . . ?
Ni4 N7 C18 C17 -174.4(3) . . . . ?
Ni4 N7 C18 C20 5.2(7) . . . . ?
Ni5 O10 C35 O9 -7.1(7) . . . . ?
Ni5 O11 C36 O12 -2.8(7) . . . . ?
Ni5 O13 C37 O14 165.7(3) . . . . ?
Ni6 O2 C31 O1 166.1(3) 5_566 . . . ?
Ni6 O12 C36 O11 4.6(7) . . . . ?
Ni6 O13 C37 O14 3.5(7) . . . . ?
Ni6 N9 N10 C23 175.6(3) . . . . ?
Ni6 N9 C21 C22 -174.4(4) . . . . ?
Ni6 N9 C21 C24 5.4(8) . . . . ?
Ni7 O2 C31 O1 -1.4(7) 5_566 . . . ?
Ni7 O3 C32 O4 -167.0(3) 5_566 . . . ?
Ni7 O14 C37 O13 -5.3(7) . . . . ?
Ni7 N11 N12 C28 178.2(3) . . . . ?
Ni7 N11 C26 C27 -176.7(4) . . . . ?
Ni7 N11 C26 C29 3.2(7) . . . . ?
N1 N2 C1 C2 -0.5(6) . . . . ?
N1 N2 C1 C4 177.1(4) . . . . ?
N2 N1 C3 C2 -0.8(7) . . . . ?
N2 N1 C3 C5 -179.8(7) . . . . ?
N2 C1 C2 C3 0.0(7) . . . . ?
N3 N4 C6 C7 0.5(6) . . . . ?
N3 N4 C6 C9 -178.2(5) . . . . ?
N4 N3 C8 C7 0.2(5) . . . . ?
N4 N3 C8 C10 179.5(5) . . . . ?
N4 C6 C7 C8 -0.3(6) . . . . ?
N5 N6 C13 C12 1.0(6) . . . . ?
N5 N6 C13 C15 -178.7(4) . . . . ?
N5 C11 C12 C13 -0.5(7) . . . . ?
N6 N5 C11 C12 1.1(6) . . . . ?
N6 N5 C11 C14 179.2(5) . . . . ?
N7 N8 C16 C17 1.2(5) . . . . ?
N7 N8 C16 C19 -177.1(4) . . . . ?
N8 N7 C18 C17 1.1(5) . . . . ?
N8 N7 C18 C20 -179.2(4) . . . . ?
N8 C16 C17 C18 -0.4(5) . . . . ?
N9 N10 C23 C22 -0.2(5) . . . . ?
N9 N10 C23 C25 179.0(4) . . . . ?
N9 C21 C22 C23 0.3(6) . . . . ?
N10 N9 C21 C22 -0.4(6) . . . . ?
N10 N9 C21 C24 179.4(5) . . . . ?
N11 N12 C28 C27 -1.2(6) . . . . ?
N11 N12 C28 C30 178.0(5) . . . . ?
N11 C26 C27 C28 -0.5(6) . . . . ?
N12 N11 C26 C27 -0.2(5) . . . . ?
N12 N11 C26 C29 179.6(4) . . . . ?
C1 C2 C3 N1 0.5(8) . . . . ?
C1 C2 C3 C5 179.4(8) . . . . ?
C3 N1 N2 C1 0.8(6) . . . . ?
C4 C1 C2 C3 -177.2(6) . . . . ?
C6 C7 C8 N3 0.1(6) . . . . ?
C6 C7 C8 C10 -179.2(5) . . . . ?
C8 N3 N4 C6 -0.5(5) . . . . ?
C9 C6 C7 C8 178.2(6) . . . . ?
C11 N5 N6 C13 -1.4(5) . . . . ?
C11 C12 C13 N6 -0.3(6) . . . . ?
C11 C12 C13 C15 179.4(6) . . . . ?
C14 C11 C12 C13 -178.5(6) . . . . ?
C16 C17 C18 N7 -0.5(5) . . . . ?
C16 C17 C18 C20 179.9(4) . . . . ?
C18 N7 N8 C16 -1.5(5) . . . . ?
C19 C16 C17 C18 177.7(5) . . . . ?
C21 N9 N10 C23 0.3(5) . . . . ?
C21 C22 C23 N10 -0.1(6) . . . . ?
C21 C22 C23 C25 -179.2(5) . . . . ?
C24 C21 C22 C23 -179.5(6) . . . . ?
C26 N11 N12 C28 0.9(5) . . . . ?
C26 C27 C28 N12 1.0(6) . . . . ?
C26 C27 C28 C30 -178.1(6) . . . . ?
C29 C26 C27 C28 179.6(5) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 268 electrons were 
found in a volume of 4122Å³ in 3 voids per unit cell. 
This is consistent with the presence of 
2[C3H6O] per Formula Unit 
which account for 256 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 0.000 0.000 -0.409 560.6 66.8 '2 C3H6O'
2 0.000 0.500 -0.208 560.6 66.8 '2 C3H6O'
3 0.115 0.736 0.827 26.5 0.0 ?
4 0.250 0.250 -0.951 834.7 0.0 ?
5 0.236 0.885 0.327 26.5 0.0 ?
6 0.264 0.615 0.327 26.5 0.0 ?
7 0.500 0.000 -0.763 560.6 65.3 '2 C3H6O'
8 0.385 0.764 0.827 26.5 0.0 ?
9 0.500 0.500 -0.725 560.6 65.3 '2 C3H6O'
10 0.615 0.236 0.173 26.5 0.0 ?
11 0.750 0.750 -0.436 834.7 0.0 ?
12 0.736 0.385 0.673 26.5 0.0 ?
13 0.764 0.115 0.673 26.5 0.0 ?
14 0.885 0.264 0.173 26.5 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.770
_vrf_PLAT420_ea-416_acetone_auto 
;
PROBLEM: D-H Bond Without Acceptor  O15A     --H15B     .     Please Check 
RESPONSE: Consequence of disorder
;
_vrf_PLAT_420_EA-416_Acetone_auto 
;
PROBLEM: D-H Bond Without Acceptor O15A --H15B . Please Check:
RESPONSE: Consequence of disorder
;
_vrf_PLAT_910_EA-416_Acetone_auto 
;
PROBLEM: Missing # of FCF Reflection[s] Below Theta[Min]. 29 Note:
RESPONSE: Not significant
;
