# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

####################################################################### 
# 
# 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_eb20162
_database_code_depnum_ccdc_archive 'CCDC 2286832'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-08-04 deposited with the CCDC.	2023-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_eb20162             
;
PROBLEM: D-H Bond Without Acceptor  O16A     --H16B     .     Please Check
RESPONSE: Disordered solvent
;
_vrf_PLAT910_eb20162             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         19 Note
RESPONSE: Not significant
;
# Added during the CSD deposition process: Friday 04 August 2023 03:29 PM
# end Validation Reply Form

_audit_creation_date             2021-02-17
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C72 H63.101 N12 Ni7 O16.449, 2(Cl O4), 6(C H4 O)'
_chemical_formula_sum            'C78 H87.09 Cl2 N12 Ni7 O30.45'
_chemical_formula_weight         2161.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Ni Cl O'
_chemical_oxdiff_usercomment     '@ 120 K KB-7A'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.1951(3)
_cell_length_b                   13.4801(4)
_cell_length_c                   15.0616(4)
_cell_angle_alpha                110.946(3)
_cell_angle_beta                 97.395(2)
_cell_angle_gamma                106.809(2)
_cell_volume                     2137.68(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    17965
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.9270
_cell_measurement_theta_min      3.7910
_shelx_estimated_absorpt_T_max   0.937
_shelx_estimated_absorpt_T_min   0.500
_exptl_absorpt_coefficient_mu    1.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86394
_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            'translucent pale blue'
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1113
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0082
0 0 1 0.0313
2 0 -1 0.0689
-2 0 1 0.0706
-1 -2 2 0.1943
0 2 -1 0.2004
1 -2 1 0.2343
-1 0 0 0.0606
1 0 0 0.0688

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by solvothermal methods'
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.04
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
0.0000 0.0000 -1.0000 0.0512 -0.0092 0.0043
-0.0000 -0.0000 1.0000 -0.0512 0.0092 -0.0043
2.0000 0.0000 -1.0000 -0.0025 -0.1229 0.0057
-2.0000 -0.0000 1.0000 0.0025 0.1229 -0.0057
-1.0000 -2.0000 2.0000 -0.0127 0.0926 -0.1110
-0.0000 2.0000 -1.0000 -0.0116 -0.0266 0.1060
1.0000 -2.0000 1.0000 -0.0152 -0.0303 -0.1054
-1.0000 -0.0000 0.0000 0.0269 0.0569 -0.0007
1.0000 0.0000 -0.0000 -0.0269 -0.0569 0.0007

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57226
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.429
_diffrn_reflns_theta_min         3.390
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00   0.00   1.00   15.00    --  -15.82 124.00-150.00   69
  2  ω    -82.00 -15.00   1.00   15.00    --  -15.82 147.00  14.00   67
  3  ω     15.00  84.00   1.00   15.00    --   17.54-147.00 -34.00   69
  4  ω      0.00  70.00   1.00   15.00    --   17.54-124.00 130.00   70
  5  ω    -85.00   3.00   1.00   15.00    --  -15.82 -37.00  30.00   88
  6  ω    -88.00 -39.00   1.00   15.00    --  -15.82-178.00  30.00   49
  7  ω    -85.00   3.00   1.00   15.00    --  -15.82 -37.00-120.00   88
  8  ω    -88.00 -35.00   1.00   15.00    --  -15.82 178.00 120.00   53
  9  ω     -9.00  39.00   1.00   15.00    --   17.54  77.00   0.00   48
 10  ω     -9.00  39.00   1.00   15.00    --   17.54  77.00-150.00   48
 11  ω      1.00  85.00   1.00   15.00    --   17.54  57.00 120.00   84
 12  ω    -52.00  37.00   1.00   15.00    --   17.54 -37.00 -30.00   89
 13  ω    -39.00  11.00   1.00   15.00    --  -15.82 -77.00-180.00   50
 14  ω    -85.00  53.00   1.00   15.00    --  -15.82   0.00  90.00  138
 15  ω    -20.00  56.00   1.00   15.00    --   17.54 -99.00-150.00   76
 16  ω    -20.00   5.00   1.00   15.00    --   17.54 -99.00   0.00   25
 17  ω      1.00  85.00   1.00   15.00    --   17.54  57.00  30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction XCalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0268698000
_diffrn_orient_matrix_UB_12      -0.0314263000
_diffrn_orient_matrix_UB_13      -0.0512287000
_diffrn_orient_matrix_UB_21      -0.0568853000
_diffrn_orient_matrix_UB_22      -0.0087286000
_diffrn_orient_matrix_UB_23      0.0091531000
_diffrn_orient_matrix_UB_31      0.0006940000
_diffrn_orient_matrix_UB_32      0.0508829000
_diffrn_orient_matrix_UB_33      -0.0042816000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8441
_reflns_number_total             10646
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_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-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         10646
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0465
_refine_ls_restrained_S_all      1.047
_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)+(0.0426P)²+3.3001P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1078
_refine_special_details          
;
Three of the hmp ligands were modelled as partly oxidised.  This explains the partial H and O values in the formula. The methanol molecules were modelled as disordered with appropriate restraints used.


#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

420_ALERT_2_B D-H Without Acceptor       O16A     --H16B     .     Please Check

Disordered solvent

910_ALERT_3_B Missing # of FCF Reflection(s) Below Theta(Min).         19 Note

Not serious

#===============================================================================
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
077_ALERT_4_C Unitcell Contains Non-integer Number of Atoms ..     Please Check
220_ALERT_2_C NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        3.8 Ratio
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        Cl1 Check
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.7 Note
260_ALERT_2_C Large Average Ueq of Residue Including       O14      0.101 Check
260_ALERT_2_C Large Average Ueq of Residue Including      O15B      0.125 Check

All of these are a consequence of disorder, discussed above.

788_ALERT_4_C Change 101       into 10        in MoietyFormula     Please Do
906_ALERT_3_C Large K Value in the Analysis of Variance ......      5.609 Check
976_ALERT_2_C Check Calcd Resid. Dens.  0.67A   From O14            -0.78 eA-3
976_ALERT_2_C Check Calcd Resid. Dens.  0.77A   From O14            -0.69 eA-3
977_ALERT_2_C Check Negative Difference Density on H14A             -0.36 eA-3

Noted

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{C24, C24A}
{C30, C30A}
{C36, C36A}
{C38, C38A}
3. Restrained distances
 O16-C39 \\sim O16-O16A
 with sigma of 0.02
 C38-O15 \\sim C38-O15B
 with sigma of 0.02
 O16A-C39A \\sim O16-C39
 with sigma of 0.02
 Cl1-O11 \\sim Cl1-O11A
 with sigma of 0.02
 Cl1-O13 \\sim Cl1-O13A
 with sigma of 0.02
 Cl1-O12 \\sim Cl1-O12A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C24A)
Uanis(C30) = Uanis(C30A)
Uanis(C36) = Uanis(C36A)
Uanis(C38) = Uanis(C38A)
5. Others
 Sof(C24A)=Sof(H24A)=Sof(H24B)=1-FVAR(1)
 Sof(O5)=Sof(C24)=FVAR(1)
 Sof(C30A)=Sof(H30A)=Sof(H30B)=1-FVAR(2)
 Sof(O7)=Sof(C30)=FVAR(2)
 Sof(C36A)=Sof(H36A)=Sof(H36B)=1-FVAR(3)
 Sof(O9)=Sof(C36)=FVAR(3)
 Sof(O16A)=Sof(H16B)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(4)
 Sof(O16)=Sof(H16A)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(4)
 Sof(O15B)=Sof(H15B)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(5)
 Sof(O15)=Sof(H15A)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(5)
 Sof(O11A)=Sof(O12A)=Sof(O13A)=1-FVAR(6)
 Sof(O11)=Sof(O12)=Sof(O13)=FVAR(6)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24A(H24A,H24B), C30A(H30A,H30B),
  C36A(H36A,H36B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34)
6.c Tetrahedral OH refined with riding coordinates:
 O14(H14A), O15(H15A), O15B(H15B), O16A(H16B)
6.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F), C39(H39A,H39B,
 H39C), C39A(H39D,H39E,H39F)
6.e Idealised tetrahedral OH refined as rotating group:
 O16(H16A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.50517(3) 0.75145(3) 0.56860(3) 0.01476(9) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 0.500000 0.01250(11) Uani 1 2 d S . P . .
Ni3 Ni 0.34326(3) 0.31528(3) 0.29412(3) 0.01639(9) Uani 1 1 d . . . . .
Ni4 Ni 0.32917(3) 0.55967(3) 0.37108(3) 0.01682(9) Uani 1 1 d . . . . .
O1 O 0.62192(16) 0.66700(15) 0.56085(14) 0.0142(4) Uani 1 1 d . . . . .
O2 O 0.45647(16) 0.48111(15) 0.35589(14) 0.0147(4) Uani 1 1 d . . . . .
O3 O 0.37993(16) 0.58335(16) 0.51462(14) 0.0154(4) Uani 1 1 d . . . . .
O4 O 0.45281(18) 0.71641(16) 0.42483(15) 0.0214(4) Uani 1 1 d . . . . .
O5 O 0.4979(3) 0.8735(3) 0.3945(3) 0.0311(14) Uani 0.625(9) 1 d . . P A 1
O6 O 0.22110(17) 0.39114(17) 0.31448(15) 0.0209(4) Uani 1 1 d . . . . .
O7 O 0.0283(3) 0.3589(3) 0.2637(2) 0.0425(13) Uani 0.824(10) 1 d . . P B 1
O8 O 0.46474(18) 0.23585(17) 0.29150(15) 0.0203(4) Uani 1 1 d . . . . .
O9 O 0.5062(4) 0.1624(4) 0.1467(3) 0.0546(17) Uani 0.776(11) 1 d . . P C 1
N1 N 0.6595(2) 0.88302(19) 0.59423(18) 0.0194(5) Uani 1 1 d . . . . .
N2 N 0.3694(2) 0.3346(2) 0.16901(18) 0.0210(5) Uani 1 1 d . . . . .
N3 N 0.1961(2) 0.6101(2) 0.42343(19) 0.0214(5) Uani 1 1 d . . . . .
N4 N 0.3156(2) 0.5922(2) 0.24598(19) 0.0230(5) Uani 1 1 d . . . . .
N5 N 0.1870(2) 0.1748(2) 0.22707(18) 0.0226(5) Uani 1 1 d . . . . .
N6 N 0.5951(2) 0.15366(19) 0.37496(18) 0.0190(5) Uani 1 1 d . . . . .
C1 C 0.6793(3) 0.9951(2) 0.6307(2) 0.0257(7) Uani 1 1 d . . . . .
H1 H 0.616628 1.020310 0.647514 0.031 Uiso 1 1 calc R U . . .
C2 C 0.7882(3) 1.0748(3) 0.6443(3) 0.0336(8) Uani 1 1 d . . . . .
H2 H 0.800377 1.153752 0.670887 0.040 Uiso 1 1 calc R U . . .
C3 C 0.8788(3) 1.0387(3) 0.6190(3) 0.0331(8) Uani 1 1 d . . . . .
H3 H 0.954218 1.092236 0.627629 0.040 Uiso 1 1 calc R U . . .
C4 C 0.8586(3) 0.9235(3) 0.5808(2) 0.0257(7) Uani 1 1 d . . . . .
H4 H 0.919690 0.896573 0.562269 0.031 Uiso 1 1 calc R U . . .
C5 C 0.7472(3) 0.8474(2) 0.5698(2) 0.0190(6) Uani 1 1 d . . . . .
C6 C 0.7171(2) 0.7195(2) 0.5284(2) 0.0187(6) Uani 1 1 d . . . . .
H6A H 0.695010 0.687428 0.455544 0.022 Uiso 1 1 calc R U . . .
H6B H 0.787551 0.703172 0.549813 0.022 Uiso 1 1 calc R U . . .
C7 C 0.3111(3) 0.2624(3) 0.0750(2) 0.0273(7) Uani 1 1 d . . . . .
H7 H 0.241756 0.199335 0.062729 0.033 Uiso 1 1 calc R U . . .
C8 C 0.3474(3) 0.2760(3) -0.0036(2) 0.0307(7) Uani 1 1 d . . . . .
H8 H 0.304035 0.223610 -0.069020 0.037 Uiso 1 1 calc R U . . .
C9 C 0.4485(3) 0.3675(3) 0.0143(2) 0.0285(7) Uani 1 1 d . . . . .
H9 H 0.475838 0.378774 -0.038938 0.034 Uiso 1 1 calc R U . . .
C10 C 0.5094(3) 0.4423(3) 0.1102(2) 0.0226(6) Uani 1 1 d . . . . .
H10 H 0.578980 0.505653 0.123929 0.027 Uiso 1 1 calc R U . . .
C11 C 0.4672(3) 0.4235(2) 0.1865(2) 0.0184(6) Uani 1 1 d . . . . .
C12 C 0.5299(2) 0.5008(2) 0.2938(2) 0.0171(6) Uani 1 1 d . . . . .
H12A H 0.603388 0.487130 0.312039 0.020 Uiso 1 1 calc R U . . .
H12B H 0.552562 0.581306 0.303339 0.020 Uiso 1 1 calc R U . . .
C13 C 0.1162(3) 0.6405(3) 0.3800(3) 0.0284(7) Uani 1 1 d . . . . .
H13 H 0.117934 0.640133 0.317051 0.034 Uiso 1 1 calc R U . . .
C14 C 0.0317(3) 0.6722(3) 0.4236(3) 0.0366(9) Uani 1 1 d . . . . .
H14 H -0.023879 0.693279 0.391227 0.044 Uiso 1 1 calc R U . . .
C15 C 0.0297(3) 0.6727(3) 0.5149(3) 0.0355(8) Uani 1 1 d . . . . .
H15 H -0.026555 0.695739 0.546913 0.043 Uiso 1 1 calc R U . . .
C16 C 0.1099(3) 0.6396(3) 0.5598(3) 0.0289(7) Uani 1 1 d . . . . .
H16 H 0.108783 0.638250 0.622329 0.035 Uiso 1 1 calc R U . . .
C17 C 0.1919(2) 0.6084(2) 0.5113(2) 0.0214(6) Uani 1 1 d . . . . .
C18 C 0.2814(2) 0.5686(2) 0.5545(2) 0.0179(6) Uani 1 1 d . . . . .
H18A H 0.308053 0.612525 0.626820 0.022 Uiso 1 1 calc R U . . .
H18B H 0.243250 0.487132 0.540293 0.022 Uiso 1 1 calc R U . . .
C19 C 0.2478(3) 0.5223(3) 0.1536(3) 0.0323(8) Uani 1 1 d . . . . .
H19 H 0.197906 0.447256 0.140430 0.039 Uiso 1 1 calc R U . . .
C20 C 0.2489(4) 0.5571(3) 0.0774(3) 0.0410(9) Uani 1 1 d . . . . .
H20 H 0.200578 0.506559 0.012944 0.049 Uiso 1 1 calc R U . . .
C21 C 0.3210(4) 0.6661(3) 0.0965(3) 0.0399(9) Uani 1 1 d . . . . .
H21 H 0.322554 0.691621 0.045314 0.048 Uiso 1 1 calc R U . . .
C22 C 0.3906(3) 0.7376(3) 0.1903(2) 0.0309(7) Uani 1 1 d . . . . .
H22 H 0.440833 0.812981 0.204785 0.037 Uiso 1 1 calc R U . . .
C23 C 0.3862(3) 0.6977(3) 0.2635(2) 0.0227(6) Uani 1 1 d . . . . .
C24 C 0.4604(3) 0.7728(3) 0.3679(2) 0.0245(7) Uani 0.625(9) 1 d . . P A 1
C24A C 0.4604(3) 0.7728(3) 0.3679(2) 0.0245(7) Uani 0.375(9) 1 d . . P A 2
H24A H 0.544324 0.804250 0.367460 0.029 Uiso 0.375(9) 1 calc R U P A 2
H24B H 0.433772 0.837481 0.395876 0.029 Uiso 0.375(9) 1 calc R U P A 2
C25 C 0.1742(3) 0.0652(3) 0.1830(2) 0.0313(8) Uani 1 1 d . . . . .
H25 H 0.242515 0.044969 0.186483 0.038 Uiso 1 1 calc R U . . .
C26 C 0.0632(4) -0.0203(3) 0.1321(3) 0.0415(9) Uani 1 1 d . . . . .
H26 H 0.055959 -0.097693 0.101235 0.050 Uiso 1 1 calc R U . . .
C27 C -0.0352(3) 0.0094(3) 0.1273(3) 0.0462(10) Uani 1 1 d . . . . .
H27 H -0.111730 -0.047519 0.093486 0.055 Uiso 1 1 calc R U . . .
C28 C -0.0224(3) 0.1220(3) 0.1717(3) 0.0383(9) Uani 1 1 d . . . . .
H28 H -0.089581 0.144044 0.168841 0.046 Uiso 1 1 calc R U . . .
C29 C 0.0904(3) 0.2030(3) 0.2208(2) 0.0254(7) Uani 1 1 d . . . . .
C30 C 0.1111(3) 0.3284(3) 0.2684(2) 0.0258(7) Uani 0.824(10) 1 d . . P B 1
C30A C 0.1111(3) 0.3284(3) 0.2684(2) 0.0258(7) Uani 0.176(10) 1 d . . P B 2
H30A H 0.085312 0.352593 0.217033 0.031 Uiso 0.176(10) 1 calc R U P B 2
H30B H 0.061540 0.340898 0.315473 0.031 Uiso 0.176(10) 1 calc R U P B 2
C31 C 0.6572(3) 0.1094(2) 0.4206(2) 0.0236(6) Uani 1 1 d . . . . .
H31 H 0.659102 0.123778 0.487400 0.028 Uiso 1 1 calc R U . . .
C32 C 0.7181(3) 0.0437(3) 0.3731(3) 0.0283(7) Uani 1 1 d . . . . .
H32 H 0.760223 0.012542 0.406596 0.034 Uiso 1 1 calc R U . . .
C33 C 0.7171(3) 0.0240(3) 0.2774(3) 0.0335(8) Uani 1 1 d . . . . .
H33 H 0.759519 -0.019885 0.243989 0.040 Uiso 1 1 calc R U . . .
C34 C 0.6533(3) 0.0689(3) 0.2291(3) 0.0328(8) Uani 1 1 d . . . . .
H34 H 0.651442 0.056467 0.162679 0.039 Uiso 1 1 calc R U . . .
C35 C 0.5925(3) 0.1324(3) 0.2810(2) 0.0236(6) Uani 1 1 d . . . . .
C36 C 0.5161(3) 0.1804(3) 0.2324(2) 0.0276(7) Uani 0.776(11) 1 d . . P C 1
C36A C 0.5161(3) 0.1804(3) 0.2324(2) 0.0276(7) Uani 0.224(11) 1 d . . P C 2
H36A H 0.566470 0.231915 0.208404 0.033 Uiso 0.224(11) 1 calc R U P C 2
H36B H 0.454616 0.116832 0.174611 0.033 Uiso 0.224(11) 1 calc R U P C 2
Cl1 Cl 0.78392(7) 0.75074(7) 0.25780(6) 0.02844(17) Uani 1 1 d D . . . .
O10 O 0.6621(2) 0.7379(2) 0.23269(19) 0.0359(6) Uani 1 1 d . . . . .
O11 O 0.7922(16) 0.6465(9) 0.192(2) 0.080(6) Uani 0.54(4) 1 d D . P D 1
O11A O 0.7932(18) 0.6434(11) 0.240(3) 0.092(7) Uani 0.46(4) 1 d D . P D 2
O12 O 0.8512(14) 0.8345(14) 0.2295(14) 0.050(4) Uani 0.54(4) 1 d D . P D 1
O12A O 0.8572(17) 0.812(2) 0.2161(14) 0.055(5) Uani 0.46(4) 1 d D . P D 2
O13 O 0.8337(11) 0.773(2) 0.3552(10) 0.071(4) Uani 0.54(4) 1 d D . P D 1
O13A O 0.8234(14) 0.818(2) 0.3631(7) 0.055(4) Uani 0.46(4) 1 d D . P D 2
O14 O 0.3034(4) -0.0040(4) -0.0009(3) 0.1039(14) Uani 1 1 d . . . . .
H14A H 0.349581 0.057361 0.045441 0.156 Uiso 1 1 calc R U . . .
C37 C 0.3180(7) -0.1001(5) 0.0165(4) 0.099(2) Uani 1 1 d . . . . .
H37A H 0.249855 -0.169779 -0.025425 0.148 Uiso 1 1 calc R U . . .
H37B H 0.322856 -0.085368 0.085802 0.148 Uiso 1 1 calc R U . . .
H37C H 0.390888 -0.109559 0.000907 0.148 Uiso 1 1 calc R U . . .
O15 O 0.8888(5) 0.4114(5) 0.1425(4) 0.082(2) Uani 0.698(10) 1 d . . P E 1
H15A H 0.948082 0.413104 0.179110 0.123 Uiso 0.698(10) 1 calc R U P E 1
C38 C 0.7967(4) 0.4013(5) 0.1854(4) 0.0619(13) Uani 0.698(10) 1 d . . P E 1
H38A H 0.825009 0.455001 0.254951 0.093 Uiso 0.698(10) 1 calc R U P E 1
H38B H 0.763854 0.323404 0.180224 0.093 Uiso 0.698(10) 1 calc R U P E 1
H38C H 0.734935 0.418416 0.151855 0.093 Uiso 0.698(10) 1 calc R U P E 1
O15B O 0.8096(14) 0.3018(12) 0.165(2) 0.190(14) Uani 0.302(10) 1 d . . P E 2
H15B H 0.745793 0.248997 0.127766 0.285 Uiso 0.302(10) 1 calc R U P E 2
C38A C 0.7967(4) 0.4013(5) 0.1854(4) 0.0619(13) Uani 0.302(10) 1 d . . P E 2
H38D H 0.750216 0.413399 0.234104 0.093 Uiso 0.302(10) 1 calc R U P E 2
H38E H 0.755346 0.401738 0.125320 0.093 Uiso 0.302(10) 1 calc R U P E 2
H38F H 0.874888 0.462488 0.212224 0.093 Uiso 0.302(10) 1 calc R U P E 2
O16 O -0.0699(5) -0.2965(5) 0.0442(4) 0.0420(16) Uani 0.475(6) 1 d D . P F 1
H16A H -0.057084 -0.296723 0.100232 0.063 Uiso 0.475(6) 1 calc R U P F 1
C39 C 0.0292(13) -0.3003(9) 0.0063(9) 0.091(5) Uani 0.475(6) 1 d D . P F 1
H39A H 0.037334 -0.258150 -0.035237 0.137 Uiso 0.475(6) 1 calc R U P F 1
H39B H 0.018452 -0.379706 -0.033066 0.137 Uiso 0.475(6) 1 calc R U P F 1
H39C H 0.100843 -0.265538 0.060795 0.137 Uiso 0.475(6) 1 calc R U P F 1
O16A O 0.0285(6) -0.3226(5) 0.0844(6) 0.073(2) Uani 0.525(6) 1 d D . P F 2
H16B H 0.046692 -0.370499 0.041468 0.109 Uiso 0.525(6) 1 calc R U P F 2
C39A C 0.0006(8) -0.3621(8) 0.1561(7) 0.057(2) Uani 0.525(6) 1 d D . P F 2
H39D H -0.041791 -0.444796 0.124594 0.085 Uiso 0.525(6) 1 calc R U P F 2
H39E H -0.049695 -0.325063 0.189895 0.085 Uiso 0.525(6) 1 calc R U P F 2
H39F H 0.073863 -0.344065 0.204042 0.085 Uiso 0.525(6) 1 calc R U P F 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 O1 2.0548(18) . ?
Ni1 O3 2.1189(19) . ?
Ni1 O4 2.014(2) . ?
Ni1 O8 2.027(2) 2_666 ?
Ni1 N1 2.056(2) . ?
Ni1 N6 2.061(2) 2_666 ?
Ni2 O1 2.0872(18) 2_666 ?
Ni2 O1 2.0872(18) . ?
Ni2 O2 2.0707(18) 2_666 ?
Ni2 O2 2.0707(18) . ?
Ni2 O3 2.0768(18) . ?
Ni2 O3 2.0768(18) 2_666 ?
Ni3 O1 2.0828(19) 2_666 ?
Ni3 O2 2.0412(18) . ?
Ni3 O6 2.033(2) . ?
Ni3 O8 2.060(2) . ?
Ni3 N2 2.044(2) . ?
Ni3 N5 2.070(2) . ?
Ni4 O2 2.1102(19) . ?
Ni4 O3 2.0511(19) . ?
Ni4 O4 2.003(2) . ?
Ni4 O6 2.054(2) . ?
Ni4 N3 2.074(3) . ?
Ni4 N4 2.079(2) . ?
O1 C6 1.416(3) . ?
O2 C12 1.415(3) . ?
O3 C18 1.406(3) . ?
O4 C24 1.329(3) . ?
O4 C24A 1.329(3) . ?
O5 C24 1.191(4) . ?
O6 C30 1.297(4) . ?
O6 C30A 1.297(4) . ?
O7 C30 1.198(4) . ?
O8 C36 1.297(4) . ?
O8 C36A 1.297(4) . ?
O9 C36 1.207(5) . ?
N1 C1 1.344(4) . ?
N1 C5 1.335(4) . ?
N2 C7 1.347(4) . ?
N2 C11 1.339(4) . ?
N3 C13 1.343(4) . ?
N3 C17 1.340(4) . ?
N4 C19 1.351(4) . ?
N4 C23 1.341(4) . ?
N5 C25 1.336(4) . ?
N5 C29 1.340(4) . ?
N6 C31 1.350(4) . ?
N6 C35 1.334(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.381(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.375(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.393(4) . ?
C5 C6 1.518(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.369(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.380(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.391(4) . ?
C11 C12 1.517(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13 0.9500 . ?
C13 C14 1.379(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.376(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.386(4) . ?
C17 C18 1.518(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19 0.9500 . ?
C19 C20 1.386(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.379(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.374(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.390(4) . ?
C23 C24 1.511(4) . ?
C23 C24A 1.511(4) . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
C25 H25 0.9500 . ?
C25 C26 1.395(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.372(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.373(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.387(4) . ?
C29 C30 1.509(5) . ?
C29 C30A 1.509(5) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
C31 H31 0.9500 . ?
C31 C32 1.383(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.368(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.392(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.390(4) . ?
C35 C36 1.528(4) . ?
C35 C36A 1.528(4) . ?
C36A H36A 0.9900 . ?
C36A H36B 0.9900 . ?
Cl1 O10 1.428(2) . ?
Cl1 O11 1.440(8) . ?
Cl1 O11A 1.416(10) . ?
Cl1 O12 1.424(8) . ?
Cl1 O12A 1.405(11) . ?
Cl1 O13 1.402(9) . ?
Cl1 O13A 1.446(9) . ?
O14 H14A 0.8400 . ?
O14 C37 1.464(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
O15 H15A 0.8400 . ?
O15 C38 1.364(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O15B H15B 0.8400 . ?
O15B C38A 1.326(14) . ?
C38A H38D 0.9800 . ?
C38A H38E 0.9800 . ?
C38A H38F 0.9800 . ?
O16 H16A 0.8400 . ?
O16 C39 1.408(12) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
O16A H16B 0.8400 . ?
O16A C39A 1.403(10) . ?
C39A H39D 0.9800 . ?
C39A H39E 0.9800 . ?
C39A H39F 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
O1 Ni1 O3 81.67(7) . . ?
O1 Ni1 N1 80.57(8) . . ?
O1 Ni1 N6 160.82(9) . 2_666 ?
O4 Ni1 O1 99.01(8) . . ?
O4 Ni1 O3 79.27(8) . . ?
O4 Ni1 O8 170.86(8) . 2_666 ?
O4 Ni1 N1 94.10(9) . . ?
O4 Ni1 N6 100.16(9) . 2_666 ?
O8 Ni1 O1 81.50(8) 2_666 . ?
O8 Ni1 O3 91.82(8) 2_666 . ?
O8 Ni1 N1 94.98(9) 2_666 . ?
O8 Ni1 N6 79.49(9) 2_666 2_666 ?
N1 Ni1 O3 159.81(9) . . ?
N1 Ni1 N6 98.59(10) . 2_666 ?
N6 Ni1 O3 101.34(8) 2_666 . ?
O1 Ni2 O1 180.0 2_666 . ?
O2 Ni2 O1 82.17(7) 2_666 . ?
O2 Ni2 O1 97.83(7) 2_666 2_666 ?
O2 Ni2 O1 82.17(7) . 2_666 ?
O2 Ni2 O1 97.82(7) . . ?
O2 Ni2 O2 180.0 . 2_666 ?
O2 Ni2 O3 97.69(7) . 2_666 ?
O2 Ni2 O3 82.31(7) . . ?
O2 Ni2 O3 82.31(7) 2_666 2_666 ?
O2 Ni2 O3 97.69(7) 2_666 . ?
O3 Ni2 O1 81.92(7) . . ?
O3 Ni2 O1 98.08(7) . 2_666 ?
O3 Ni2 O1 98.08(7) 2_666 . ?
O3 Ni2 O1 81.92(7) 2_666 2_666 ?
O3 Ni2 O3 180.0 . 2_666 ?
O2 Ni3 O1 82.99(7) . 2_666 ?
O2 Ni3 O8 99.55(8) . . ?
O2 Ni3 N2 80.67(9) . . ?
O2 Ni3 N5 159.99(9) . . ?
O6 Ni3 O1 92.22(8) . 2_666 ?
O6 Ni3 O2 81.57(8) . . ?
O6 Ni3 O8 171.95(8) . . ?
O6 Ni3 N2 96.66(9) . . ?
O6 Ni3 N5 79.06(9) . . ?
O8 Ni3 O1 80.05(7) . 2_666 ?
O8 Ni3 N5 100.33(9) . . ?
N2 Ni3 O1 160.03(9) . 2_666 ?
N2 Ni3 O8 91.38(9) . . ?
N2 Ni3 N5 96.55(10) . . ?
N5 Ni3 O1 102.70(8) . 2_666 ?
O3 Ni4 O2 81.96(7) . . ?
O3 Ni4 O6 97.75(8) . . ?
O3 Ni4 N3 80.27(9) . . ?
O3 Ni4 N4 160.80(9) . . ?
O4 Ni4 O2 92.80(8) . . ?
O4 Ni4 O3 81.16(8) . . ?
O4 Ni4 O6 172.25(8) . . ?
O4 Ni4 N3 96.26(9) . . ?
O4 Ni4 N4 79.76(9) . . ?
O6 Ni4 O2 79.44(7) . . ?
O6 Ni4 N3 91.10(9) . . ?
O6 Ni4 N4 101.45(9) . . ?
N3 Ni4 O2 158.53(9) . . ?
N3 Ni4 N4 99.68(10) . . ?
N4 Ni4 O2 101.07(9) . . ?
Ni1 O1 Ni2 98.97(8) . . ?
Ni1 O1 Ni3 98.38(8) . 2_666 ?
Ni3 O1 Ni2 96.44(7) 2_666 . ?
C6 O1 Ni1 108.69(15) . . ?
C6 O1 Ni2 130.73(16) . . ?
C6 O1 Ni3 117.99(16) . 2_666 ?
Ni2 O2 Ni4 96.98(8) . . ?
Ni3 O2 Ni2 98.27(8) . . ?
Ni3 O2 Ni4 98.38(8) . . ?
C12 O2 Ni2 130.42(16) . . ?
C12 O2 Ni3 110.11(15) . . ?
C12 O2 Ni4 117.09(16) . . ?
Ni2 O3 Ni1 97.27(7) . . ?
Ni4 O3 Ni1 97.21(8) . . ?
Ni4 O3 Ni2 98.66(8) . . ?
C18 O3 Ni1 116.79(16) . . ?
C18 O3 Ni2 130.53(16) . . ?
C18 O3 Ni4 110.46(16) . . ?
Ni4 O4 Ni1 102.28(9) . . ?
C24 O4 Ni1 138.00(19) . . ?
C24 O4 Ni4 117.95(19) . . ?
C24A O4 Ni1 138.00(19) . . ?
C24A O4 Ni4 117.95(19) . . ?
Ni3 O6 Ni4 100.50(8) . . ?
C30 O6 Ni3 117.55(19) . . ?
C30 O6 Ni4 138.4(2) . . ?
C30A O6 Ni3 117.55(19) . . ?
C30A O6 Ni4 138.4(2) . . ?
Ni1 O8 Ni3 100.01(9) 2_666 . ?
C36 O8 Ni1 118.06(19) . 2_666 ?
C36 O8 Ni3 141.7(2) . . ?
C36A O8 Ni3 141.7(2) . . ?
C1 N1 Ni1 128.0(2) . . ?
C5 N1 Ni1 112.88(18) . . ?
C5 N1 C1 119.1(3) . . ?
C7 N2 Ni3 127.9(2) . . ?
C11 N2 Ni3 112.71(19) . . ?
C11 N2 C7 118.7(3) . . ?
C13 N3 Ni4 128.5(2) . . ?
C17 N3 Ni4 112.84(18) . . ?
C17 N3 C13 118.6(3) . . ?
C19 N4 Ni4 128.8(2) . . ?
C23 N4 Ni4 112.7(2) . . ?
C23 N4 C19 118.5(3) . . ?
C25 N5 Ni3 127.9(2) . . ?
C25 N5 C29 118.8(3) . . ?
C29 N5 Ni3 113.0(2) . . ?
C31 N6 Ni1 127.8(2) . 2_666 ?
C35 N6 Ni1 113.68(19) . 2_666 ?
C35 N6 C31 118.5(3) . . ?
N1 C1 H1 119.0 . . ?
N1 C1 C2 121.9(3) . . ?
C2 C1 H1 119.0 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.1(3) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 121.7(3) . . ?
N1 C5 C6 115.8(2) . . ?
C4 C5 C6 122.6(3) . . ?
O1 C6 C5 110.8(2) . . ?
O1 C6 H6A 109.5 . . ?
O1 C6 H6B 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
N2 C7 H7 118.6 . . ?
N2 C7 C8 122.7(3) . . ?
C8 C7 H7 118.6 . . ?
C7 C8 H8 120.7 . . ?
C7 C8 C9 118.7(3) . . ?
C9 C8 H8 120.7 . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.3(3) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 120.5 . . ?
C9 C10 C11 119.0(3) . . ?
C11 C10 H10 120.5 . . ?
N2 C11 C10 121.6(3) . . ?
N2 C11 C12 116.2(2) . . ?
C10 C11 C12 122.2(3) . . ?
O2 C12 C11 111.2(2) . . ?
O2 C12 H12A 109.4 . . ?
O2 C12 H12B 109.4 . . ?
C11 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N3 C13 H13 118.8 . . ?
N3 C13 C14 122.4(3) . . ?
C14 C13 H13 118.8 . . ?
C13 C14 H14 120.7 . . ?
C15 C14 C13 118.5(3) . . ?
C15 C14 H14 120.7 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.9(3) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 120.8 . . ?
C15 C16 C17 118.3(3) . . ?
C17 C16 H16 120.8 . . ?
N3 C17 C16 122.2(3) . . ?
N3 C17 C18 116.0(3) . . ?
C16 C17 C18 121.7(3) . . ?
O3 C18 C17 110.9(2) . . ?
O3 C18 H18A 109.5 . . ?
O3 C18 H18B 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.0 . . ?
N4 C19 H19 119.1 . . ?
N4 C19 C20 121.8(3) . . ?
C20 C19 H19 119.1 . . ?
C19 C20 H20 120.4 . . ?
C21 C20 C19 119.1(3) . . ?
C21 C20 H20 120.4 . . ?
C20 C21 H21 120.3 . . ?
C22 C21 C20 119.4(3) . . ?
C22 C21 H21 120.3 . . ?
C21 C22 H22 120.6 . . ?
C21 C22 C23 118.9(3) . . ?
C23 C22 H22 120.6 . . ?
N4 C23 C22 122.3(3) . . ?
N4 C23 C24 116.6(3) . . ?
N4 C23 C24A 116.6(3) . . ?
C22 C23 C24 121.1(3) . . ?
C22 C23 C24A 121.1(3) . . ?
O4 C24 C23 112.1(2) . . ?
O5 C24 O4 126.8(3) . . ?
O5 C24 C23 119.3(3) . . ?
O4 C24A C23 112.1(2) . . ?
O4 C24A H24A 109.2 . . ?
O4 C24A H24B 109.2 . . ?
C23 C24A H24A 109.2 . . ?
C23 C24A H24B 109.2 . . ?
H24A C24A H24B 107.9 . . ?
N5 C25 H25 119.1 . . ?
N5 C25 C26 121.8(4) . . ?
C26 C25 H25 119.1 . . ?
C25 C26 H26 120.6 . . ?
C27 C26 C25 118.9(3) . . ?
C27 C26 H26 120.6 . . ?
C26 C27 H27 120.3 . . ?
C26 C27 C28 119.5(3) . . ?
C28 C27 H27 120.3 . . ?
C27 C28 H28 120.6 . . ?
C27 C28 C29 118.8(4) . . ?
C29 C28 H28 120.6 . . ?
N5 C29 C28 122.2(3) . . ?
N5 C29 C30 116.3(3) . . ?
N5 C29 C30A 116.3(3) . . ?
C28 C29 C30 121.5(3) . . ?
C28 C29 C30A 121.5(3) . . ?
O6 C30 C29 113.0(3) . . ?
O7 C30 O6 127.5(3) . . ?
O7 C30 C29 119.4(3) . . ?
O6 C30A C29 113.0(3) . . ?
O6 C30A H30A 109.0 . . ?
O6 C30A H30B 109.0 . . ?
C29 C30A H30A 109.0 . . ?
C29 C30A H30B 109.0 . . ?
H30A C30A H30B 107.8 . . ?
N6 C31 H31 119.0 . . ?
N6 C31 C32 122.1(3) . . ?
C32 C31 H31 119.0 . . ?
C31 C32 H32 120.4 . . ?
C33 C32 C31 119.2(3) . . ?
C33 C32 H32 120.4 . . ?
C32 C33 H33 120.2 . . ?
C32 C33 C34 119.5(3) . . ?
C34 C33 H33 120.2 . . ?
C33 C34 H34 120.9 . . ?
C35 C34 C33 118.1(3) . . ?
C35 C34 H34 120.9 . . ?
N6 C35 C34 122.6(3) . . ?
N6 C35 C36 115.9(3) . . ?
N6 C35 C36A 115.9(3) . . ?
C34 C35 C36 121.5(3) . . ?
C34 C35 C36A 121.5(3) . . ?
O8 C36 C35 112.9(3) . . ?
O9 C36 O8 127.0(3) . . ?
O9 C36 C35 120.1(3) . . ?
O8 C36A C35 112.9(3) . . ?
O8 C36A H36A 109.0 . . ?
O8 C36A H36B 109.0 . . ?
C35 C36A H36A 109.0 . . ?
C35 C36A H36B 109.0 . . ?
H36A C36A H36B 107.8 . . ?
O10 Cl1 O11 106.0(9) . . ?
O10 Cl1 O13A 104.3(8) . . ?
O11A Cl1 O10 110.0(8) . . ?
O11A Cl1 O13A 107.3(8) . . ?
O12 Cl1 O10 108.4(7) . . ?
O12 Cl1 O11 103.8(9) . . ?
O12A Cl1 O10 114.6(9) . . ?
O12A Cl1 O11A 113.5(13) . . ?
O12A Cl1 O13A 106.4(10) . . ?
O13 Cl1 O10 117.1(6) . . ?
O13 Cl1 O11 109.1(7) . . ?
O13 Cl1 O12 111.5(10) . . ?
C37 O14 H14A 109.5 . . ?
O14 C37 H37A 109.5 . . ?
O14 C37 H37B 109.5 . . ?
O14 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C38 O15 H15A 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 . . ?
C38A O15B H15B 109.5 . . ?
O15B C38A H38D 109.5 . . ?
O15B C38A H38E 109.5 . . ?
O15B C38A H38F 109.5 . . ?
H38D C38A H38E 109.5 . . ?
H38D C38A H38F 109.5 . . ?
H38E C38A H38F 109.5 . . ?
C39 O16 H16A 109.5 . . ?
O16 C39 H39A 109.5 . . ?
O16 C39 H39B 109.5 . . ?
O16 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C39A O16A H16B 109.5 . . ?
O16A C39A H39D 109.5 . . ?
O16A C39A H39E 109.5 . . ?
O16A C39A H39F 109.5 . . ?
H39D C39A H39E 109.5 . . ?
H39D C39A H39F 109.5 . . ?
H39E C39A H39F 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
O14 H14A O9 0.84 2.03 2.811(6) 154.4 . yes
O15 H15A O7 0.84 1.97 2.747(6) 153.9 1_655 yes
O16 H16A O11 0.84 2.55 3.14(2) 128.2 1_445 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 C6 C5 35.9(3) . . . . ?
Ni1 O3 C18 C17 76.5(2) . . . . ?
Ni1 O4 C24 O5 -7.4(6) . . . . ?
Ni1 O4 C24 C23 -172.0(2) . . . . ?
Ni1 O4 C24A C23 -172.0(2) . . . . ?
Ni1 O8 C36 O9 178.3(4) 2_666 . . . ?
Ni1 O8 C36 C35 0.3(3) 2_666 . . . ?
Ni1 O8 C36A C35 0.3(3) 2_666 . . . ?
Ni1 N1 C1 C2 179.9(2) . . . . ?
Ni1 N1 C5 C4 179.4(2) . . . . ?
Ni1 N1 C5 C6 0.1(3) . . . . ?
Ni1 N6 C31 C32 177.8(2) 2_666 . . . ?
Ni1 N6 C35 C34 -179.4(3) 2_666 . . . ?
Ni1 N6 C35 C36 -0.5(3) 2_666 . . . ?
Ni1 N6 C35 C36A -0.5(3) 2_666 . . . ?
Ni2 O1 C6 C5 156.42(17) . . . . ?
Ni2 O2 C12 C11 150.84(18) . . . . ?
Ni2 O3 C18 C17 -155.35(18) . . . . ?
Ni3 O1 C6 C5 -74.9(2) 2_666 . . . ?
Ni3 O2 C12 C11 30.0(3) . . . . ?
Ni3 O6 C30 O7 -172.7(3) . . . . ?
Ni3 O6 C30 C29 10.3(3) . . . . ?
Ni3 O6 C30A C29 10.3(3) . . . . ?
Ni3 O8 C36 O9 4.3(6) . . . . ?
Ni3 O8 C36 C35 -173.7(2) . . . . ?
Ni3 O8 C36A C35 -173.7(2) . . . . ?
Ni3 N2 C7 C8 -170.1(3) . . . . ?
Ni3 N2 C11 C10 171.3(2) . . . . ?
Ni3 N2 C11 C12 -7.7(3) . . . . ?
Ni3 N5 C25 C26 -173.5(2) . . . . ?
Ni3 N5 C29 C28 174.9(3) . . . . ?
Ni3 N5 C29 C30 -3.9(3) . . . . ?
Ni3 N5 C29 C30A -3.9(3) . . . . ?
Ni4 O2 C12 C11 -81.2(2) . . . . ?
Ni4 O3 C18 C17 -33.3(3) . . . . ?
Ni4 O4 C24 O5 154.3(3) . . . . ?
Ni4 O4 C24 C23 -10.3(3) . . . . ?
Ni4 O4 C24A C23 -10.3(3) . . . . ?
Ni4 O6 C30 O7 -19.0(6) . . . . ?
Ni4 O6 C30 C29 164.0(2) . . . . ?
Ni4 O6 C30A C29 164.0(2) . . . . ?
Ni4 N3 C13 C14 179.9(2) . . . . ?
Ni4 N3 C17 C16 179.7(2) . . . . ?
Ni4 N3 C17 C18 -1.1(3) . . . . ?
Ni4 N4 C19 C20 -180.0(3) . . . . ?
Ni4 N4 C23 C22 -179.6(2) . . . . ?
Ni4 N4 C23 C24 -0.4(3) . . . . ?
Ni4 N4 C23 C24A -0.4(3) . . . . ?
N1 C1 C2 C3 0.7(5) . . . . ?
N1 C5 C6 O1 -24.6(3) . . . . ?
N2 C7 C8 C9 0.2(5) . . . . ?
N2 C11 C12 O2 -15.1(3) . . . . ?
N3 C13 C14 C15 0.1(5) . . . . ?
N3 C17 C18 O3 23.2(3) . . . . ?
N4 C19 C20 C21 -0.2(6) . . . . ?
N4 C23 C24 O4 6.8(4) . . . . ?
N4 C23 C24 O5 -159.0(3) . . . . ?
N4 C23 C24A O4 6.8(4) . . . . ?
N5 C25 C26 C27 0.0(5) . . . . ?
N5 C29 C30 O6 -4.0(4) . . . . ?
N5 C29 C30 O7 178.7(3) . . . . ?
N5 C29 C30A O6 -4.0(4) . . . . ?
N6 C31 C32 C33 0.9(5) . . . . ?
N6 C35 C36 O8 0.2(4) . . . . ?
N6 C35 C36 O9 -178.0(4) . . . . ?
N6 C35 C36A O8 0.2(4) . . . . ?
C1 N1 C5 C4 -0.2(4) . . . . ?
C1 N1 C5 C6 -179.5(3) . . . . ?
C1 C2 C3 C4 -0.2(5) . . . . ?
C2 C3 C4 C5 -0.5(5) . . . . ?
C3 C4 C5 N1 0.7(5) . . . . ?
C3 C4 C5 C6 180.0(3) . . . . ?
C4 C5 C6 O1 156.1(3) . . . . ?
C5 N1 C1 C2 -0.5(5) . . . . ?
C7 N2 C11 C10 -0.1(4) . . . . ?
C7 N2 C11 C12 -179.2(3) . . . . ?
C7 C8 C9 C10 -0.2(5) . . . . ?
C8 C9 C10 C11 0.0(5) . . . . ?
C9 C10 C11 N2 0.2(4) . . . . ?
C9 C10 C11 C12 179.1(3) . . . . ?
C10 C11 C12 O2 165.9(2) . . . . ?
C11 N2 C7 C8 -0.1(5) . . . . ?
C13 N3 C17 C16 -1.6(4) . . . . ?
C13 N3 C17 C18 177.6(3) . . . . ?
C13 C14 C15 C16 -1.3(5) . . . . ?
C14 C15 C16 C17 1.1(5) . . . . ?
C15 C16 C17 N3 0.4(5) . . . . ?
C15 C16 C17 C18 -178.7(3) . . . . ?
C16 C17 C18 O3 -157.6(3) . . . . ?
C17 N3 C13 C14 1.4(4) . . . . ?
C19 N4 C23 C22 0.8(4) . . . . ?
C19 N4 C23 C24 180.0(3) . . . . ?
C19 N4 C23 C24A 180.0(3) . . . . ?
C19 C20 C21 C22 0.4(6) . . . . ?
C20 C21 C22 C23 0.0(5) . . . . ?
C21 C22 C23 N4 -0.6(5) . . . . ?
C21 C22 C23 C24 -179.7(3) . . . . ?
C21 C22 C23 C24A -179.7(3) . . . . ?
C22 C23 C24 O4 -174.0(3) . . . . ?
C22 C23 C24 O5 20.2(5) . . . . ?
C22 C23 C24A O4 -174.0(3) . . . . ?
C23 N4 C19 C20 -0.4(5) . . . . ?
C25 N5 C29 C28 1.2(5) . . . . ?
C25 N5 C29 C30 -177.6(3) . . . . ?
C25 N5 C29 C30A -177.6(3) . . . . ?
C25 C26 C27 C28 0.6(6) . . . . ?
C26 C27 C28 C29 -0.3(6) . . . . ?
C27 C28 C29 N5 -0.7(5) . . . . ?
C27 C28 C29 C30 178.1(3) . . . . ?
C27 C28 C29 C30A 178.1(3) . . . . ?
C28 C29 C30 O6 177.2(3) . . . . ?
C28 C29 C30 O7 -0.1(5) . . . . ?
C28 C29 C30A O6 177.2(3) . . . . ?
C29 N5 C25 C26 -0.9(5) . . . . ?
C31 N6 C35 C34 -1.6(4) . . . . ?
C31 N6 C35 C36 177.3(3) . . . . ?
C31 N6 C35 C36A 177.3(3) . . . . ?
C31 C32 C33 C34 -1.0(5) . . . . ?
C32 C33 C34 C35 -0.1(5) . . . . ?
C33 C34 C35 N6 1.4(5) . . . . ?
C33 C34 C35 C36 -177.3(3) . . . . ?
C33 C34 C35 C36A -177.3(3) . . . . ?
C34 C35 C36 O8 179.0(3) . . . . ?
C34 C35 C36 O9 0.9(5) . . . . ?
C34 C35 C36A O8 179.0(3) . . . . ?
C35 N6 C31 C32 0.3(4) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id KB-7A
_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 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.815
