# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 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_cp125
_database_code_depnum_ccdc_archive 'CCDC 2348000'
loop_
_audit_author_name
_audit_author_address
'Joshua Buss'
;University of Michigan
United States of America
;
_audit_update_record             
;
2024-06-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_audit_creation_date             2024-06-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H39 F6 N6 Ni2 O7 S2, C H2 Cl2, C F3 O3 S'
_chemical_formula_sum            'C40 H41 Cl2 F9 N6 Ni2 O10 S3'
_chemical_formula_weight         1221.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         C38H39CuF6N6NiO7S2
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 '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                   11.11800(10)
_cell_length_b                   20.66740(10)
_cell_length_c                   21.7121(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.0290(10)
_cell_angle_gamma                90
_cell_volume                     4940.10(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    49765
_cell_measurement_temperature    85
_cell_measurement_theta_max      69.1270
_cell_measurement_theta_min      2.0720
_shelx_estimated_absorpt_T_max   0.669
_shelx_estimated_absorpt_T_min   0.520
_exptl_absorpt_coefficient_mu    3.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73909
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.429
_diffrn_reflns_theta_min         2.966
_diffrn_ambient_temperature      85
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   1.00    1.00    --  -20.00   0.00-180.00  180
  2  ω    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  3  ω    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  4  ω    -25.00  43.00   1.00    1.00    --  -20.00  36.00 120.00   68
  5  ω    -45.00   0.00   1.00    1.00    --  -20.00  72.00-180.00   45
  6  ω   -173.00-128.00   1.00    2.00    --  -92.00 -36.00 120.00   45
  7  ω   -133.00 -88.00   1.00    2.00    --  -92.00 -36.00 -60.00   45
  8  ω   -104.00 -59.00   1.00    2.00    --  -92.00  36.00  60.00   45
  9  ω   -122.00 -77.00   1.00    2.00    --  -92.00 -72.00  60.00   45
 10  ω   -174.00 -78.00   1.00    2.00    --  -92.00 -72.00-120.00   96
 11  ω    -93.00 -35.00   1.00    2.00    --  -92.00  36.00-120.00   58
 12  ω   -176.00 -77.00   1.00    2.00    --  -92.00 -72.00 -60.00   99
 13  ω   -147.00 -75.00   1.00    2.00    --  -92.00 -72.00-180.00   72
 14  ω   -176.00 -77.00   1.00    2.00    --  -92.00 -72.00 120.00   99
 15  ω   -177.00-116.00   1.00    2.00    --  -92.00 -36.00  60.00   61
 16  ω    -87.00  -9.00   1.00    2.00    --  -92.00  36.00 -60.00   78
 17  ω   -102.00 -14.00   1.00    2.00    --  -92.00  36.00   0.00   88
 18  ω   -102.00 -21.00   1.00    2.00    --  -92.00  72.00 120.00   81
 19  ω   -175.00-104.00   1.00    2.00    --  -92.00 -36.00   0.00   71
 20  ω   -104.00 -52.00   1.00    2.00    --  -92.00  72.00  60.00   52
 21  ω   -109.00 -14.00   1.00    2.00    --  -92.00  72.00-120.00   95
 22  ω   -105.00 -24.00   1.00    2.00    --  -92.00  36.00-120.00   81
 23  ω   -105.00  -2.00   1.00    2.00    --  -92.00  36.00-180.00  103
 24  ω   -106.00  -2.00   1.00    2.00    --  -92.00  72.00 -60.00  104
 25  ω   -106.00  -2.00   1.00    2.00    --  -92.00  72.00 -60.00  104
 26  ω   -107.00 -29.00   1.00    2.00    --  -92.00  72.00   0.00   78
 27  ω   -117.00 -72.00   1.00    2.00    --  -92.00  72.00 180.00   45
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0556175000
_diffrn_orient_matrix_UB_12      -0.0427697000
_diffrn_orient_matrix_UB_13      0.0548302000
_diffrn_orient_matrix_UB_21      0.0027440000
_diffrn_orient_matrix_UB_22      0.0585485000
_diffrn_orient_matrix_UB_23      0.0440367000
_diffrn_orient_matrix_UB_31      -0.1283962000
_diffrn_orient_matrix_UB_32      -0.0172347000
_diffrn_orient_matrix_UB_33      0.0137811000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9031
_reflns_number_total             9159
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.30
_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 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00202(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         9159
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.111
_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)+(0.0512P)²+6.7725P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1116
_refine_special_details          ?
_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
2. Restrained distances
 Cl1-C40B \\sim Cl1-C40A
 with sigma of 0.02
 Cl2A-C40B \\sim Cl2B-C40A
 with sigma of 0.02
 Cl1-Cl2A \\sim Cl1-Cl2B
 with sigma of 0.02
 Cl1-C40A \\sim Cl1-C40B \\sim Cl2A-C40A \\sim Cl2B-C40B
 with sigma of 0.02
 Cl1-C40B \\sim Cl2A-C40A
 with sigma of 0.02
 Cl1-C40A \\sim Cl2B-C40B
 with sigma of 0.02
 Cl2B-C40B \\sim Cl1-C40B
 with sigma of 0.02
 Cl1-C40A \\sim Cl2A-C40A
 with sigma of 0.02
3. Rigid bond restraints
 C40B, Cl1, Cl2B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C40A \\sim Cl1 \\sim C40B \\sim Cl2A \\sim H40A \\sim H40B \\sim Cl2B \\sim
H40C \\sim H40D: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
5. Rigid body (RIGU) restrains
 C40B, Cl1, Cl2B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=
 Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(Cl2B)=Sof(C40B)=Sof(H40C)=Sof(H40D)=1-FVAR(2)
 Sof(Cl2A)=Sof(C40A)=Sof(H40A)=Sof(H40B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C25(H25A,
 H25B), C31(H31A,H31B), C40A(H40A,H40B), C40B(H40C,H40D)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21),
 C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
  C35(H35), C36(H36)
7.c Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C8B(H8BA,H8BB,
 H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F)
;
_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 0.40133(3) 0.51049(2) 0.28196(2) 0.01947(12) Uani 1 1 d . . . . .
Ni2 Ni 0.18851(3) 0.64390(2) 0.28899(2) 0.01950(12) Uani 1 1 d . . . . .
S1 S 0.18006(6) 0.49705(3) 0.36178(3) 0.02985(15) Uani 1 1 d . . . . .
S2 S 0.46296(6) 0.65918(4) 0.36149(3) 0.03424(17) Uani 1 1 d . . . . .
F1 F 0.1894(3) 0.41490(10) 0.45267(10) 0.0714(7) Uani 1 1 d . . . . .
F2 F 0.0948(2) 0.50196(12) 0.46694(11) 0.0753(7) Uani 1 1 d . . . . .
F3 F 0.2874(2) 0.50146(15) 0.47618(10) 0.0819(8) Uani 1 1 d . . . . .
F4 F 0.61674(19) 0.65779(14) 0.46326(10) 0.0719(7) Uani 1 1 d . . . . .
F5 F 0.4451(3) 0.61363(14) 0.47115(10) 0.0827(8) Uani 1 1 d . . . . .
F6 F 0.4581(2) 0.71533(13) 0.46884(11) 0.0761(7) Uani 1 1 d . . . . .
O1 O 0.28005(15) 0.57715(8) 0.24752(8) 0.0265(4) Uani 1 1 d . . . . .
O2 O 0.29628(17) 0.47555(9) 0.34685(8) 0.0311(4) Uani 1 1 d . . . . .
O3 O 0.0794(2) 0.46166(12) 0.33200(12) 0.0528(6) Uani 1 1 d . . . . .
O4 O 0.1663(2) 0.56666(10) 0.36066(10) 0.0439(5) Uani 1 1 d . . . . .
O5 O 0.4860(3) 0.59222(14) 0.34849(12) 0.0727(9) Uani 1 1 d . . . . .
O6 O 0.5418(2) 0.70533(19) 0.34039(15) 0.0853(11) Uani 1 1 d . . . . .
O7 O 0.33621(16) 0.67659(9) 0.35002(9) 0.0321(4) Uani 1 1 d . . . . .
N1 N 0.51748(18) 0.53275(10) 0.21882(10) 0.0267(4) Uani 1 1 d . . . . .
N2 N 0.33518(19) 0.44037(11) 0.21368(10) 0.0284(5) Uani 1 1 d . . . . .
N3 N 0.55153(19) 0.46503(10) 0.32423(9) 0.0270(4) Uani 1 1 d . . . . .
N4 N 0.03058(19) 0.62503(10) 0.22989(10) 0.0259(4) Uani 1 1 d . . . . .
N5 N 0.06714(19) 0.68799(10) 0.33717(10) 0.0264(4) Uani 1 1 d . . . . .
N6 N 0.20940(19) 0.71845(11) 0.22330(10) 0.0297(5) Uani 1 1 d . . . . .
C1 C 0.2600(2) 0.58051(12) 0.18390(11) 0.0253(5) Uani 1 1 d . . . . .
C2 C 0.3571(2) 0.59002(12) 0.15063(12) 0.0260(5) Uani 1 1 d . . . . .
C3 C 0.3361(2) 0.59334(12) 0.08578(12) 0.0262(5) Uani 1 1 d . . . . .
H3 H 0.402999 0.599257 0.063524 0.031 Uiso 1 1 calc R U . . .
C4 C 0.2193(2) 0.58819(12) 0.05277(11) 0.0257(5) Uani 1 1 d . . . . .
C5 C 0.1235(2) 0.57982(12) 0.08734(12) 0.0260(5) Uani 1 1 d . . . . .
H5 H 0.042932 0.577167 0.066070 0.031 Uiso 1 1 calc R U . . .
C6 C 0.1422(2) 0.57524(12) 0.15195(12) 0.0254(5) Uani 1 1 d . . . . .
C7 C 0.1959(2) 0.59441(14) -0.01823(12) 0.0310(6) Uani 1 1 d . . . . .
C11 C 0.4827(2) 0.59505(12) 0.18589(12) 0.0283(5) Uani 1 1 d . . . . .
H11A H 0.541122 0.605064 0.156752 0.034 Uiso 1 1 calc R U . . .
H11B H 0.485611 0.630661 0.216558 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5143(2) 0.47875(13) 0.17340(12) 0.0282(5) Uani 1 1 d . . . . .
H12A H 0.579070 0.447342 0.188356 0.034 Uiso 1 1 calc R U . . .
H12B H 0.531566 0.496097 0.133044 0.034 Uiso 1 1 calc R U . . .
C13 C 0.3935(2) 0.44402(12) 0.16362(12) 0.0264(5) Uani 1 1 d . . . . .
C14 C 0.3491(2) 0.41556(13) 0.10757(13) 0.0315(6) Uani 1 1 d . . . . .
H14 H 0.391817 0.419251 0.072778 0.038 Uiso 1 1 calc R U . . .
C15 C 0.2406(3) 0.38138(14) 0.10304(14) 0.0357(6) Uani 1 1 d . . . . .
H15 H 0.207538 0.361591 0.064919 0.043 Uiso 1 1 calc R U . . .
C16 C 0.1813(3) 0.37657(14) 0.15485(14) 0.0348(6) Uani 1 1 d . . . . .
H16 H 0.107869 0.352681 0.153098 0.042 Uiso 1 1 calc R U . . .
C17 C 0.2305(2) 0.40705(13) 0.20900(13) 0.0312(6) Uani 1 1 d . . . . .
H17 H 0.189021 0.404400 0.244303 0.037 Uiso 1 1 calc R U . . .
C18 C 0.6401(2) 0.53722(13) 0.25542(13) 0.0303(5) Uani 1 1 d . . . . .
H18A H 0.651674 0.580788 0.274281 0.036 Uiso 1 1 calc R U . . .
H18B H 0.702503 0.530875 0.227617 0.036 Uiso 1 1 calc R U . . .
C19 C 0.6552(2) 0.48668(12) 0.30586(12) 0.0270(5) Uani 1 1 d . . . . .
C20 C 0.7679(2) 0.46533(13) 0.33367(13) 0.0312(6) Uani 1 1 d . . . . .
H20 H 0.839929 0.481133 0.320020 0.037 Uiso 1 1 calc R U . . .
C21 C 0.7744(3) 0.42093(14) 0.38134(13) 0.0342(6) Uani 1 1 d . . . . .
H21 H 0.850912 0.406064 0.401217 0.041 Uiso 1 1 calc R U . . .
C22 C 0.6678(3) 0.39821(14) 0.39995(13) 0.0353(6) Uani 1 1 d . . . . .
H22 H 0.670074 0.367334 0.432505 0.042 Uiso 1 1 calc R U . . .
C23 C 0.5586(2) 0.42124(14) 0.37035(12) 0.0320(6) Uani 1 1 d . . . . .
H23 H 0.485545 0.405587 0.383007 0.038 Uiso 1 1 calc R U . . .
C24 C 0.0395(2) 0.56689(12) 0.18935(12) 0.0269(5) Uani 1 1 d . . . . .
H24A H 0.053321 0.527662 0.215552 0.032 Uiso 1 1 calc R U . . .
H24B H -0.037661 0.561231 0.161035 0.032 Uiso 1 1 calc R U . . .
C25 C -0.0632(2) 0.61549(13) 0.27091(12) 0.0305(6) Uani 1 1 d . . . . .
H25A H -0.058483 0.570722 0.287299 0.037 Uiso 1 1 calc R U . . .
H25B H -0.144743 0.621760 0.246800 0.037 Uiso 1 1 calc R U . . .
C26 C -0.0451(2) 0.66278(12) 0.32422(12) 0.0281(5) Uani 1 1 d . . . . .
C27 C -0.1365(3) 0.67809(14) 0.35932(13) 0.0342(6) Uani 1 1 d . . . . .
H27 H -0.215020 0.659396 0.349966 0.041 Uiso 1 1 calc R U . . .
C28 C -0.1108(3) 0.72114(15) 0.40820(13) 0.0380(6) Uani 1 1 d . . . . .
H28 H -0.171307 0.731571 0.433480 0.046 Uiso 1 1 calc R U . . .
C29 C 0.0034(3) 0.74896(14) 0.42013(13) 0.0360(6) Uani 1 1 d . . . . .
H29 H 0.021395 0.780099 0.452279 0.043 Uiso 1 1 calc R U . . .
C30 C 0.0901(2) 0.73039(13) 0.38423(12) 0.0311(6) Uani 1 1 d . . . . .
H30 H 0.169347 0.748261 0.393096 0.037 Uiso 1 1 calc R U . . .
C31 C 0.0024(2) 0.68388(13) 0.19070(12) 0.0283(5) Uani 1 1 d . . . . .
H31A H -0.048601 0.713424 0.211941 0.034 Uiso 1 1 calc R U . . .
H31B H -0.045165 0.670964 0.150612 0.034 Uiso 1 1 calc R U . . .
C32 C 0.1143(2) 0.71950(12) 0.17806(12) 0.0276(5) Uani 1 1 d . . . . .
C33 C 0.1157(3) 0.75365(14) 0.12361(14) 0.0359(6) Uani 1 1 d . . . . .
H33 H 0.047866 0.752641 0.091753 0.043 Uiso 1 1 calc R U . . .
C34 C 0.2183(3) 0.78953(15) 0.11630(16) 0.0433(7) Uani 1 1 d . . . . .
H34 H 0.221561 0.813777 0.079401 0.052 Uiso 1 1 calc R U . . .
C35 C 0.3157(3) 0.78948(14) 0.16350(15) 0.0391(7) Uani 1 1 d . . . . .
H35 H 0.386267 0.814331 0.159845 0.047 Uiso 1 1 calc R U . . .
C36 C 0.3089(2) 0.75290(13) 0.21578(13) 0.0326(6) Uani 1 1 d . . . . .
H36 H 0.376704 0.751944 0.247664 0.039 Uiso 1 1 calc R U . . .
C37 C 0.1897(3) 0.47827(16) 0.44421(15) 0.0438(7) Uani 1 1 d . . . . .
C38 C 0.4972(3) 0.66221(17) 0.44567(15) 0.0465(7) Uani 1 1 d . . . . .
C8A C 0.1147(4) 0.54091(18) -0.04747(16) 0.0391(9) Uani 0.824(5) 1 d . . P A 1
H8AA H 0.035060 0.543995 -0.033252 0.059 Uiso 0.824(5) 1 calc R U P A 1
H8AB H 0.151445 0.498896 -0.035291 0.059 Uiso 0.824(5) 1 calc R U P A 1
H8AC H 0.105004 0.545119 -0.092855 0.059 Uiso 0.824(5) 1 calc R U P A 1
C9A C 0.1284(3) 0.66066(17) -0.03378(16) 0.0352(8) Uani 0.824(5) 1 d . . P A 1
H9AA H 0.112974 0.666517 -0.078985 0.053 Uiso 0.824(5) 1 calc R U P A 1
H9AB H 0.179130 0.696230 -0.015029 0.053 Uiso 0.824(5) 1 calc R U P A 1
H9AC H 0.050996 0.660452 -0.016997 0.053 Uiso 0.824(5) 1 calc R U P A 1
C10A C 0.3124(3) 0.5961(2) -0.04816(16) 0.0391(9) Uani 0.824(5) 1 d . . P A 1
H10A H 0.291680 0.599945 -0.093381 0.059 Uiso 0.824(5) 1 calc R U P A 1
H10B H 0.358326 0.556055 -0.038163 0.059 Uiso 0.824(5) 1 calc R U P A 1
H10C H 0.361871 0.633226 -0.032125 0.059 Uiso 0.824(5) 1 calc R U P A 1
C8B C 0.0620(14) 0.5895(7) -0.0447(7) 0.030(4) Uani 0.176(5) 1 d . . P A 2
H8BA H 0.018860 0.627612 -0.032306 0.045 Uiso 0.176(5) 1 calc R U P A 2
H8BB H 0.027396 0.550383 -0.028559 0.045 Uiso 0.176(5) 1 calc R U P A 2
H8BC H 0.053689 0.587182 -0.090145 0.045 Uiso 0.176(5) 1 calc R U P A 2
C9B C 0.2602(18) 0.6447(10) -0.0390(8) 0.045(5) Uani 0.176(5) 1 d . . P A 2
H9BA H 0.242092 0.647609 -0.084364 0.067 Uiso 0.176(5) 1 calc R U P A 2
H9BB H 0.347366 0.637119 -0.026998 0.067 Uiso 0.176(5) 1 calc R U P A 2
H9BC H 0.237122 0.685221 -0.020341 0.067 Uiso 0.176(5) 1 calc R U P A 2
C10B C 0.2499(16) 0.5225(9) -0.0404(7) 0.039(4) Uani 0.176(5) 1 d . . P A 2
H10D H 0.203912 0.487066 -0.024783 0.059 Uiso 0.176(5) 1 calc R U P A 2
H10E H 0.335946 0.518368 -0.023277 0.059 Uiso 0.176(5) 1 calc R U P A 2
H10F H 0.241125 0.520454 -0.085891 0.059 Uiso 0.176(5) 1 calc R U P A 2
Cl1 Cl 0.85135(6) 0.82530(3) 0.27090(3) 0.03751(17) Uani 1 1 d D U . . .
Cl2A Cl 0.59585(14) 0.86177(11) 0.26208(18) 0.0482(7) Uani 0.793(13) 1 d D U P
B 1
C40A C 0.7039(4) 0.8002(2) 0.2827(3) 0.0373(11) Uani 0.793(13) 1 d D U P B 1
H40A H 0.680737 0.761213 0.257342 0.045 Uiso 0.793(13) 1 calc R U P B 1
H40B H 0.704335 0.788672 0.326972 0.045 Uiso 0.793(13) 1 calc R U P B 1
Cl2B Cl 0.6205(13) 0.8858(11) 0.2861(7) 0.077(4) Uani 0.207(13) 1 d D U P B 2
C40B C 0.6903(13) 0.8145(14) 0.2646(13) 0.063(5) Uani 0.207(13) 1 d D U P B 2
H40C H 0.657487 0.803062 0.221177 0.076 Uiso 0.207(13) 1 calc R U P B 2
H40D H 0.671998 0.778501 0.291856 0.076 Uiso 0.207(13) 1 calc R U P B 2
S3 S 0.72000(6) 0.65155(3) 0.07404(3) 0.03320(16) Uani 1 1 d . . . . .
F7 F 0.75625(19) 0.75748(9) 0.14097(9) 0.0545(5) Uani 1 1 d . . . . .
F8 F 0.6528(2) 0.77222(10) 0.05147(11) 0.0726(7) Uani 1 1 d . . . . .
F9 F 0.56934(19) 0.72714(10) 0.12347(12) 0.0648(6) Uani 1 1 d . . . . .
O8 O 0.61604(18) 0.63039(11) 0.03170(9) 0.0417(5) Uani 1 1 d . . . . .
O9 O 0.74190(17) 0.61660(10) 0.13194(9) 0.0353(4) Uani 1 1 d . . . . .
O10 O 0.8277(2) 0.66568(14) 0.04678(10) 0.0524(6) Uani 1 1 d . . . . .
C39 C 0.6719(3) 0.73075(15) 0.09856(15) 0.0447(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.9983(18) . ?
Ni1 O2 2.0808(18) . ?
Ni1 O5 2.334(3) . ?
Ni1 N1 2.062(2) . ?
Ni1 N2 2.130(2) . ?
Ni1 N3 2.021(2) . ?
Ni2 O1 2.0014(18) . ?
Ni2 O4 2.267(2) . ?
Ni2 O7 2.0738(19) . ?
Ni2 N4 2.062(2) . ?
Ni2 N5 2.035(2) . ?
Ni2 N6 2.134(2) . ?
S1 O2 1.4454(19) . ?
S1 O3 1.416(2) . ?
S1 O4 1.447(2) . ?
S1 C37 1.820(3) . ?
S2 O5 1.443(3) . ?
S2 O6 1.415(3) . ?
S2 O7 1.4420(19) . ?
S2 C38 1.815(3) . ?
F1 C37 1.323(4) . ?
F2 C37 1.320(4) . ?
F3 C37 1.296(4) . ?
F4 C38 1.334(4) . ?
F5 C38 1.319(4) . ?
F6 C38 1.307(4) . ?
O1 C1 1.370(3) . ?
N1 C11 1.497(3) . ?
N1 C12 1.486(3) . ?
N1 C18 1.482(3) . ?
N2 C13 1.343(3) . ?
N2 C17 1.343(3) . ?
N3 C19 1.347(3) . ?
N3 C23 1.344(3) . ?
N4 C24 1.501(3) . ?
N4 C25 1.476(3) . ?
N4 C31 1.492(3) . ?
N5 C26 1.345(3) . ?
N5 C30 1.343(3) . ?
N6 C32 1.339(3) . ?
N6 C36 1.344(3) . ?
C1 C2 1.394(4) . ?
C1 C6 1.398(4) . ?
C2 C3 1.396(4) . ?
C2 C11 1.499(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.396(4) . ?
C4 C5 1.398(4) . ?
C4 C7 1.532(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(4) . ?
C6 C24 1.501(3) . ?
C7 C8A 1.510(4) . ?
C7 C9A 1.575(4) . ?
C7 C10A 1.528(4) . ?
C7 C8B 1.522(16) . ?
C7 C9B 1.372(18) . ?
C7 C10B 1.698(17) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.511(4) . ?
C13 C14 1.379(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.390(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.378(4) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.506(4) . ?
C19 C20 1.385(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.378(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.377(4) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.507(4) . ?
C26 C27 1.390(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.384(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.385(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.376(4) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.504(4) . ?
C32 C33 1.379(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.388(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.383(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.375(4) . ?
C36 H36 0.9500 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C8B H8BA 0.9800 . ?
C8B H8BB 0.9800 . ?
C8B H8BC 0.9800 . ?
C9B H9BA 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
Cl1 C40A 1.772(4) . ?
Cl1 C40B 1.790(14) . ?
Cl2A C40A 1.764(4) . ?
C40A H40A 0.9900 . ?
C40A H40B 0.9900 . ?
Cl2B C40B 1.759(15) . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
S3 O8 1.441(2) . ?
S3 O9 1.441(2) . ?
S3 O10 1.438(2) . ?
S3 C39 1.825(3) . ?
F7 C39 1.339(3) . ?
F8 C39 1.328(4) . ?
F9 C39 1.330(4) . ?

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 O2 94.55(7) . . ?
O1 Ni1 O5 85.73(8) . . ?
O1 Ni1 N1 92.87(8) . . ?
O1 Ni1 N2 93.40(8) . . ?
O1 Ni1 N3 164.12(8) . . ?
O2 Ni1 O5 92.76(10) . . ?
O2 Ni1 N2 93.62(8) . . ?
N1 Ni1 O2 171.99(8) . . ?
N1 Ni1 O5 90.80(10) . . ?
N1 Ni1 N2 82.90(8) . . ?
N2 Ni1 O5 173.60(10) . . ?
N3 Ni1 O2 92.15(8) . . ?
N3 Ni1 O5 79.57(8) . . ?
N3 Ni1 N1 81.44(8) . . ?
N3 Ni1 N2 100.54(8) . . ?
O1 Ni2 O4 86.24(7) . . ?
O1 Ni2 O7 96.03(7) . . ?
O1 Ni2 N4 91.83(8) . . ?
O1 Ni2 N5 162.83(8) . . ?
O1 Ni2 N6 95.01(8) . . ?
O7 Ni2 O4 86.75(8) . . ?
O7 Ni2 N6 92.37(8) . . ?
N4 Ni2 O4 97.42(8) . . ?
N4 Ni2 O7 171.34(8) . . ?
N4 Ni2 N6 83.30(8) . . ?
N5 Ni2 O4 79.56(8) . . ?
N5 Ni2 O7 92.78(8) . . ?
N5 Ni2 N4 80.58(8) . . ?
N5 Ni2 N6 99.33(8) . . ?
N6 Ni2 O4 178.55(8) . . ?
O2 S1 O4 113.43(12) . . ?
O2 S1 C37 102.91(13) . . ?
O3 S1 O2 114.42(13) . . ?
O3 S1 O4 115.54(15) . . ?
O3 S1 C37 105.86(16) . . ?
O4 S1 C37 102.72(14) . . ?
O5 S2 C38 102.25(15) . . ?
O6 S2 O5 116.6(2) . . ?
O6 S2 O7 114.26(15) . . ?
O6 S2 C38 104.51(18) . . ?
O7 S2 O5 113.69(15) . . ?
O7 S2 C38 103.16(14) . . ?
Ni1 O1 Ni2 131.74(9) . . ?
C1 O1 Ni1 114.74(15) . . ?
C1 O1 Ni2 113.41(15) . . ?
S1 O2 Ni1 130.48(11) . . ?
S1 O4 Ni2 133.67(13) . . ?
S2 O5 Ni1 138.42(15) . . ?
S2 O7 Ni2 134.15(12) . . ?
C11 N1 Ni1 111.42(15) . . ?
C12 N1 Ni1 108.34(15) . . ?
C12 N1 C11 110.4(2) . . ?
C18 N1 Ni1 105.79(15) . . ?
C18 N1 C11 111.07(19) . . ?
C18 N1 C12 109.7(2) . . ?
C13 N2 Ni1 111.48(17) . . ?
C13 N2 C17 118.6(2) . . ?
C17 N2 Ni1 127.79(18) . . ?
C19 N3 Ni1 113.43(17) . . ?
C23 N3 Ni1 127.60(18) . . ?
C23 N3 C19 118.7(2) . . ?
C24 N4 Ni2 113.33(15) . . ?
C25 N4 Ni2 105.17(15) . . ?
C25 N4 C24 110.91(19) . . ?
C25 N4 C31 110.1(2) . . ?
C31 N4 Ni2 107.06(15) . . ?
C31 N4 C24 110.12(19) . . ?
C26 N5 Ni2 112.43(17) . . ?
C30 N5 Ni2 127.89(18) . . ?
C30 N5 C26 118.9(2) . . ?
C32 N6 Ni2 110.71(17) . . ?
C32 N6 C36 118.7(2) . . ?
C36 N6 Ni2 129.17(19) . . ?
O1 C1 C2 120.1(2) . . ?
O1 C1 C6 120.4(2) . . ?
C2 C1 C6 119.6(2) . . ?
C1 C2 C3 119.8(2) . . ?
C1 C2 C11 118.6(2) . . ?
C3 C2 C11 121.6(2) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.8(2) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C5 117.2(2) . . ?
C3 C4 C7 121.7(2) . . ?
C5 C4 C7 121.0(2) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 C4 122.1(2) . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C24 118.1(2) . . ?
C5 C6 C1 119.5(2) . . ?
C5 C6 C24 122.3(2) . . ?
C4 C7 C9A 107.3(2) . . ?
C4 C7 C10B 101.2(6) . . ?
C8A C7 C4 111.7(2) . . ?
C8A C7 C9A 107.9(3) . . ?
C8A C7 C10A 109.3(3) . . ?
C10A C7 C4 113.2(2) . . ?
C10A C7 C9A 107.2(3) . . ?
C8B C7 C4 113.2(6) . . ?
C8B C7 C10B 101.5(8) . . ?
C9B C7 C4 111.7(8) . . ?
C9B C7 C8B 117.0(10) . . ?
C9B C7 C10B 110.4(11) . . ?
N1 C11 C2 110.1(2) . . ?
N1 C11 H11A 109.6 . . ?
N1 C11 H11B 109.6 . . ?
C2 C11 H11A 109.6 . . ?
C2 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N1 C12 H12A 109.0 . . ?
N1 C12 H12B 109.0 . . ?
N1 C12 C13 112.8(2) . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
N2 C13 C12 115.7(2) . . ?
N2 C13 C14 122.4(2) . . ?
C14 C13 C12 121.9(2) . . ?
C13 C14 H14 120.7 . . ?
C13 C14 C15 118.7(3) . . ?
C15 C14 H14 120.7 . . ?
C14 C15 H15 120.5 . . ?
C16 C15 C14 119.1(3) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 120.6 . . ?
C17 C16 C15 118.8(3) . . ?
C17 C16 H16 120.6 . . ?
N2 C17 C16 122.4(2) . . ?
N2 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
N1 C18 H18A 109.6 . . ?
N1 C18 H18B 109.6 . . ?
N1 C18 C19 110.3(2) . . ?
H18A C18 H18B 108.1 . . ?
C19 C18 H18A 109.6 . . ?
C19 C18 H18B 109.6 . . ?
N3 C19 C18 115.6(2) . . ?
N3 C19 C20 121.6(2) . . ?
C20 C19 C18 122.7(2) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 C19 119.3(3) . . ?
C21 C20 H20 120.4 . . ?
C20 C21 H21 120.4 . . ?
C20 C21 C22 119.2(3) . . ?
C22 C21 H21 120.4 . . ?
C21 C22 H22 120.6 . . ?
C23 C22 C21 118.7(3) . . ?
C23 C22 H22 120.6 . . ?
N3 C23 C22 122.5(3) . . ?
N3 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
N4 C24 H24A 109.7 . . ?
N4 C24 H24B 109.7 . . ?
C6 C24 N4 110.05(19) . . ?
C6 C24 H24A 109.7 . . ?
C6 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
N4 C25 H25A 109.6 . . ?
N4 C25 H25B 109.6 . . ?
N4 C25 C26 110.3(2) . . ?
H25A C25 H25B 108.1 . . ?
C26 C25 H25A 109.6 . . ?
C26 C25 H25B 109.6 . . ?
N5 C26 C25 115.6(2) . . ?
N5 C26 C27 121.7(2) . . ?
C27 C26 C25 122.7(2) . . ?
C26 C27 H27 120.7 . . ?
C28 C27 C26 118.6(3) . . ?
C28 C27 H27 120.7 . . ?
C27 C28 H28 120.1 . . ?
C27 C28 C29 119.7(3) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 H29 120.8 . . ?
C30 C29 C28 118.4(3) . . ?
C30 C29 H29 120.8 . . ?
N5 C30 C29 122.6(3) . . ?
N5 C30 H30 118.7 . . ?
C29 C30 H30 118.7 . . ?
N4 C31 H31A 109.0 . . ?
N4 C31 H31B 109.0 . . ?
N4 C31 C32 113.0(2) . . ?
H31A C31 H31B 107.8 . . ?
C32 C31 H31A 109.0 . . ?
C32 C31 H31B 109.0 . . ?
N6 C32 C31 116.5(2) . . ?
N6 C32 C33 122.3(2) . . ?
C33 C32 C31 121.1(2) . . ?
C32 C33 H33 120.7 . . ?
C32 C33 C34 118.6(3) . . ?
C34 C33 H33 120.7 . . ?
C33 C34 H34 120.5 . . ?
C35 C34 C33 119.1(3) . . ?
C35 C34 H34 120.5 . . ?
C34 C35 H35 120.5 . . ?
C36 C35 C34 119.0(3) . . ?
C36 C35 H35 120.5 . . ?
N6 C36 C35 122.2(3) . . ?
N6 C36 H36 118.9 . . ?
C35 C36 H36 118.9 . . ?
F1 C37 S1 110.3(2) . . ?
F2 C37 S1 110.4(2) . . ?
F2 C37 F1 107.3(3) . . ?
F3 C37 S1 112.2(2) . . ?
F3 C37 F1 108.0(3) . . ?
F3 C37 F2 108.4(3) . . ?
F4 C38 S2 110.3(2) . . ?
F5 C38 S2 110.7(2) . . ?
F5 C38 F4 107.8(3) . . ?
F6 C38 S2 112.5(2) . . ?
F6 C38 F4 108.6(3) . . ?
F6 C38 F5 106.8(3) . . ?
C7 C8A H8AA 109.5 . . ?
C7 C8A H8AB 109.5 . . ?
C7 C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C7 C9A H9AA 109.5 . . ?
C7 C9A H9AB 109.5 . . ?
C7 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C7 C10A H10A 109.5 . . ?
C7 C10A H10B 109.5 . . ?
C7 C10A H10C 109.5 . . ?
H10A C10A H10B 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C7 C8B H8BA 109.5 . . ?
C7 C8B H8BB 109.5 . . ?
C7 C8B H8BC 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
C7 C9B H9BA 109.5 . . ?
C7 C9B H9BB 109.5 . . ?
C7 C9B H9BC 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
C7 C10B H10D 109.5 . . ?
C7 C10B H10E 109.5 . . ?
C7 C10B H10F 109.5 . . ?
H10D C10B H10E 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
Cl1 C40A H40A 109.4 . . ?
Cl1 C40A H40B 109.4 . . ?
Cl2A C40A Cl1 111.3(2) . . ?
Cl2A C40A H40A 109.4 . . ?
Cl2A C40A H40B 109.4 . . ?
H40A C40A H40B 108.0 . . ?
Cl1 C40B H40C 109.6 . . ?
Cl1 C40B H40D 109.6 . . ?
Cl2B C40B Cl1 110.4(11) . . ?
Cl2B C40B H40C 109.6 . . ?
Cl2B C40B H40D 109.6 . . ?
H40C C40B H40D 108.1 . . ?
O8 S3 O9 115.31(12) . . ?
O8 S3 C39 102.50(14) . . ?
O9 S3 C39 102.47(13) . . ?
O10 S3 O8 116.04(13) . . ?
O10 S3 O9 114.34(13) . . ?
O10 S3 C39 103.47(16) . . ?
F7 C39 S3 111.4(2) . . ?
F8 C39 S3 112.1(2) . . ?
F8 C39 F7 106.5(2) . . ?
F8 C39 F9 107.2(3) . . ?
F9 C39 S3 111.8(2) . . ?
F9 C39 F7 107.6(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 O1 C1 C2 -55.1(3) . . . . ?
Ni1 O1 C1 C6 125.6(2) . . . . ?
Ni1 N1 C11 C2 -60.8(2) . . . . ?
Ni1 N1 C12 C13 29.5(2) . . . . ?
Ni1 N1 C18 C19 37.5(2) . . . . ?
Ni1 N2 C13 C12 18.9(3) . . . . ?
Ni1 N2 C13 C14 -163.8(2) . . . . ?
Ni1 N2 C17 C16 161.9(2) . . . . ?
Ni1 N3 C19 C18 -3.3(3) . . . . ?
Ni1 N3 C19 C20 174.2(2) . . . . ?
Ni1 N3 C23 C22 -173.3(2) . . . . ?
Ni2 O1 C1 C2 121.6(2) . . . . ?
Ni2 O1 C1 C6 -57.6(3) . . . . ?
Ni2 N4 C24 C6 -57.2(2) . . . . ?
Ni2 N4 C25 C26 39.1(2) . . . . ?
Ni2 N4 C31 C32 31.8(2) . . . . ?
Ni2 N5 C26 C25 -9.0(3) . . . . ?
Ni2 N5 C26 C27 169.0(2) . . . . ?
Ni2 N5 C30 C29 -168.9(2) . . . . ?
Ni2 N6 C32 C31 16.2(3) . . . . ?
Ni2 N6 C32 C33 -166.6(2) . . . . ?
Ni2 N6 C36 C35 165.8(2) . . . . ?
O1 C1 C2 C3 179.9(2) . . . . ?
O1 C1 C2 C11 1.2(3) . . . . ?
O1 C1 C6 C5 179.0(2) . . . . ?
O1 C1 C6 C24 0.9(3) . . . . ?
O2 S1 O4 Ni2 53.1(2) . . . . ?
O2 S1 C37 F1 -68.8(3) . . . . ?
O2 S1 C37 F2 172.8(2) . . . . ?
O2 S1 C37 F3 51.7(3) . . . . ?
O3 S1 O2 Ni1 97.00(19) . . . . ?
O3 S1 O4 Ni2 -81.9(2) . . . . ?
O3 S1 C37 F1 51.6(3) . . . . ?
O3 S1 C37 F2 -66.8(3) . . . . ?
O3 S1 C37 F3 172.1(2) . . . . ?
O4 S1 O2 Ni1 -38.5(2) . . . . ?
O4 S1 C37 F1 173.2(2) . . . . ?
O4 S1 C37 F2 54.8(3) . . . . ?
O4 S1 C37 F3 -66.3(3) . . . . ?
O5 S2 O7 Ni2 -29.7(2) . . . . ?
O5 S2 C38 F4 72.2(3) . . . . ?
O5 S2 C38 F5 -47.1(3) . . . . ?
O5 S2 C38 F6 -166.4(3) . . . . ?
O6 S2 O5 Ni1 -106.3(3) . . . . ?
O6 S2 O7 Ni2 107.6(2) . . . . ?
O6 S2 C38 F4 -49.8(3) . . . . ?
O6 S2 C38 F5 -169.1(3) . . . . ?
O6 S2 C38 F6 71.6(3) . . . . ?
O7 S2 O5 Ni1 29.9(3) . . . . ?
O7 S2 C38 F4 -169.6(2) . . . . ?
O7 S2 C38 F5 71.2(3) . . . . ?
O7 S2 C38 F6 -48.2(3) . . . . ?
N1 C12 C13 N2 -33.4(3) . . . . ?
N1 C12 C13 C14 149.3(2) . . . . ?
N1 C18 C19 N3 -23.9(3) . . . . ?
N1 C18 C19 C20 158.6(2) . . . . ?
N2 C13 C14 C15 -0.6(4) . . . . ?
N3 C19 C20 C21 -0.1(4) . . . . ?
N4 C25 C26 N5 -21.2(3) . . . . ?
N4 C25 C26 C27 160.8(3) . . . . ?
N4 C31 C32 N6 -33.5(3) . . . . ?
N4 C31 C32 C33 149.3(2) . . . . ?
N5 C26 C27 C28 0.9(4) . . . . ?
N6 C32 C33 C34 -1.7(4) . . . . ?
C1 C2 C3 C4 0.8(4) . . . . ?
C1 C2 C11 N1 63.6(3) . . . . ?
C1 C6 C24 N4 62.6(3) . . . . ?
C2 C1 C6 C5 -0.3(4) . . . . ?
C2 C1 C6 C24 -178.3(2) . . . . ?
C2 C3 C4 C5 0.3(4) . . . . ?
C2 C3 C4 C7 177.6(2) . . . . ?
C3 C2 C11 N1 -115.1(3) . . . . ?
C3 C4 C5 C6 -1.4(4) . . . . ?
C3 C4 C7 C8A 132.7(3) . . . . ?
C3 C4 C7 C9A -109.3(3) . . . . ?
C3 C4 C7 C10A 8.8(4) . . . . ?
C3 C4 C7 C8B -178.1(6) . . . . ?
C3 C4 C7 C9B -43.5(10) . . . . ?
C3 C4 C7 C10B 74.0(7) . . . . ?
C4 C5 C6 C1 1.4(4) . . . . ?
C4 C5 C6 C24 179.4(2) . . . . ?
C5 C4 C7 C8A -50.1(3) . . . . ?
C5 C4 C7 C9A 68.0(3) . . . . ?
C5 C4 C7 C10A -173.9(3) . . . . ?
C5 C4 C7 C8B -0.9(7) . . . . ?
C5 C4 C7 C9B 133.7(10) . . . . ?
C5 C4 C7 C10B -108.7(7) . . . . ?
C5 C6 C24 N4 -115.4(3) . . . . ?
C6 C1 C2 C3 -0.8(4) . . . . ?
C6 C1 C2 C11 -179.6(2) . . . . ?
C7 C4 C5 C6 -178.8(2) . . . . ?
C11 N1 C12 C13 -92.7(2) . . . . ?
C11 N1 C18 C19 158.5(2) . . . . ?
C11 C2 C3 C4 179.5(2) . . . . ?
C12 N1 C11 C2 59.6(3) . . . . ?
C12 N1 C18 C19 -79.2(3) . . . . ?
C12 C13 C14 C15 176.5(2) . . . . ?
C13 N2 C17 C16 0.1(4) . . . . ?
C13 C14 C15 C16 -0.5(4) . . . . ?
C14 C15 C16 C17 1.4(4) . . . . ?
C15 C16 C17 N2 -1.2(4) . . . . ?
C17 N2 C13 C12 -176.4(2) . . . . ?
C17 N2 C13 C14 0.9(4) . . . . ?
C18 N1 C11 C2 -178.4(2) . . . . ?
C18 N1 C12 C13 144.6(2) . . . . ?
C18 C19 C20 C21 177.3(3) . . . . ?
C19 N3 C23 C22 0.7(4) . . . . ?
C19 C20 C21 C22 0.6(4) . . . . ?
C20 C21 C22 C23 -0.5(4) . . . . ?
C21 C22 C23 N3 -0.2(4) . . . . ?
C23 N3 C19 C18 -178.1(2) . . . . ?
C23 N3 C19 C20 -0.6(4) . . . . ?
C24 N4 C25 C26 162.0(2) . . . . ?
C24 N4 C31 C32 -91.8(2) . . . . ?
C25 N4 C24 C6 -175.3(2) . . . . ?
C25 N4 C31 C32 145.7(2) . . . . ?
C25 C26 C27 C28 178.8(3) . . . . ?
C26 N5 C30 C29 0.3(4) . . . . ?
C26 C27 C28 C29 1.5(4) . . . . ?
C27 C28 C29 C30 -2.9(4) . . . . ?
C28 C29 C30 N5 2.0(4) . . . . ?
C30 N5 C26 C25 -179.8(2) . . . . ?
C30 N5 C26 C27 -1.8(4) . . . . ?
C31 N4 C24 C6 62.7(3) . . . . ?
C31 N4 C25 C26 -75.9(3) . . . . ?
C31 C32 C33 C34 175.3(3) . . . . ?
C32 N6 C36 C35 0.5(4) . . . . ?
C32 C33 C34 C35 0.5(4) . . . . ?
C33 C34 C35 C36 1.2(4) . . . . ?
C34 C35 C36 N6 -1.7(4) . . . . ?
C36 N6 C32 C31 -175.9(2) . . . . ?
C36 N6 C32 C33 1.3(4) . . . . ?
C37 S1 O2 Ni1 -148.67(16) . . . . ?
C37 S1 O4 Ni2 163.41(19) . . . . ?
C38 S2 O5 Ni1 140.3(3) . . . . ?
C38 S2 O7 Ni2 -139.58(18) . . . . ?
O8 S3 C39 F7 177.3(2) . . . . ?
O8 S3 C39 F8 -63.4(3) . . . . ?
O8 S3 C39 F9 56.9(2) . . . . ?
O9 S3 C39 F7 57.5(3) . . . . ?
O9 S3 C39 F8 176.7(2) . . . . ?
O9 S3 C39 F9 -62.9(2) . . . . ?
O10 S3 C39 F7 -61.7(3) . . . . ?
O10 S3 C39 F8 57.6(3) . . . . ?
O10 S3 C39 F9 178.0(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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.768
_oxdiff_exptl_absorpt_empirical_full_min 0.563
####################################################################### 
# 
# 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_hll169
_database_code_depnum_ccdc_archive 'CCDC 2348001'
loop_
_audit_author_name
_audit_author_address
'Joshua Buss'
;University of Michigan
United States of America
;
_audit_update_record             
;
2024-06-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT420_hll169              
;
PROBLEM: D-H Bond Without Acceptor  O11      --H11D     .     Please Check 
RESPONSE: The crystals used for this difraction experiment were grown
in benchtop solvent and incorporated several water molecules into solvent voids
present in the lattice. One of these water molecules was solved discretely (O11)
but 6 were treated with SQUEEZE. The removal of the water network results
in the acceptorless H-bond.
;
# end Validation Reply Form

_audit_creation_date             2024-06-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C37 H43 N6 Ni2 O7, C F3 O3 S, H2 O, 6[H2O]'
_chemical_formula_sum            'C38 H57 F3 N6 Ni2 O17 S'
_chemical_formula_weight         1076.37
_chemical_melting_point          ?
_chemical_oxdiff_formula         C37H41F3N6O6SNi2
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'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 '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                   10.2519(3)
_cell_length_b                   11.2496(4)
_cell_length_c                   21.4920(7)
_cell_angle_alpha                77.624(3)
_cell_angle_beta                 79.248(3)
_cell_angle_gamma                80.429(3)
_cell_volume                     2357.88(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8497
_cell_measurement_temperature    85
_cell_measurement_theta_max      67.5780
_cell_measurement_theta_min      4.2250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.175
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34115
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.682
_diffrn_reflns_theta_min         2.131
_diffrn_ambient_temperature      85
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   1.00    5.00    --  -20.00   0.00-180.00  180
  2  ω    -45.00   0.00   1.00    5.00    --  -20.00  72.00   0.00   45
  3  ω    -45.00   0.00   1.00    5.00    --  -20.00  72.00   0.00   45
  4  ω    -25.00  43.00   1.00    5.00    --  -20.00  36.00 120.00   68
  5  ω    -45.00   0.00   1.00    5.00    --  -20.00  72.00-180.00   45
  6  ω   -173.00-128.00   1.00   35.00    --  -92.00 -36.00 120.00   45
  7  ω   -133.00 -88.00   1.00   35.00    --  -92.00 -36.00 -60.00   45
  8  ω   -104.00 -59.00   1.00   35.00    --  -92.00  36.00  60.00   45
  9  ω   -122.00 -77.00   1.00   35.00    --  -92.00 -72.00  60.00   45
 10  ω   -174.00 -78.00   1.00   35.00    --  -92.00 -72.00-120.00   96
 11  ω    -93.00 -35.00   1.00   35.00    --  -92.00  36.00-120.00   58
 12  ω   -176.00 -77.00   1.00   35.00    --  -92.00 -72.00 -60.00   99
 13  ω   -147.00 -75.00   1.00   35.00    --  -92.00 -72.00-180.00   72
 14  ω   -176.00 -77.00   1.00   35.00    --  -92.00 -72.00 120.00   99
 15  ω   -177.00-116.00   1.00   35.00    --  -92.00 -36.00  60.00   61
 16  ω    -87.00  -9.00   1.00   35.00    --  -92.00  36.00 -60.00   78
 17  ω   -102.00 -14.00   1.00   35.00    --  -92.00  36.00   0.00   88
 18  ω   -102.00 -21.00   1.00   35.00    --  -92.00  72.00 120.00   81
 19  ω   -175.00-104.00   1.00   35.00    --  -92.00 -36.00   0.00   71
 20  ω   -104.00 -52.00   1.00   35.00    --  -92.00  72.00  60.00   52
 21  ω   -109.00 -14.00   1.00   35.00    --  -92.00  72.00-120.00   95
 22  ω   -105.00 -24.00   1.00   35.00    --  -92.00  36.00-120.00   81
 23  ω   -105.00  -2.00   1.00   35.00    --  -92.00  36.00-180.00  103
 24  ω   -106.00  -2.00   1.00   35.00    --  -92.00  72.00 -60.00  104
 25  ω   -106.00  -2.00   1.00   35.00    --  -92.00  72.00 -60.00  104
 26  ω   -107.00 -29.00   1.00   35.00    --  -92.00  72.00   0.00   78
 27  ω   -117.00 -72.00   1.00   35.00    --  -92.00  72.00 180.00   45
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0510873000
_diffrn_orient_matrix_UB_12      -0.1043758000
_diffrn_orient_matrix_UB_13      0.0524780000
_diffrn_orient_matrix_UB_21      0.0631803000
_diffrn_orient_matrix_UB_22      -0.0772939000
_diffrn_orient_matrix_UB_23      -0.0517948000
_diffrn_orient_matrix_UB_31      0.1311733000
_diffrn_orient_matrix_UB_32      0.0559849000
_diffrn_orient_matrix_UB_33      -0.0091871000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6116
_reflns_number_total             8487
_reflns_odcompleteness_completeness 95.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.55
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         8487
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0798
_refine_ls_restrained_S_all      1.054
_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)+(0.1541P)²+1.0101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2531
_refine_special_details          ?
_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,H) groups
2. Restrained distances
 C4-C7A \\sim C4-C7B
 with sigma of 0.02
 C7A-C8A \\sim C7B-C8B
 with sigma of 0.02
 C7A-C9A \\sim C7B-C9B
 with sigma of 0.02
 C4-C8A \\sim C4-C8B
 with sigma of 0.04
 C7A-C10A \\sim C7B-C10B
 with sigma of 0.02
 C9A-C8A \\sim C9B-C8B
 with sigma of 0.04
 C10A-C8A \\sim C10B-C8B
 with sigma of 0.04
 C4-C9A \\sim C4-C9B
 with sigma of 0.04
 C4-C10A \\sim C4-C10B
 with sigma of 0.04
 C9A-C10A \\sim C9B-C10B
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C3, C4, C5, C7A, C8A, C9A, C10A, C7B, C8B, C9B, C10B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
 Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
5.a Free rotating group:
 O11(H11C,H11D)
5.b Rotating group:
 O6(H6A,H6B), O7(H7A,H7B)
5.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C25(H25A,
 H25B), C31(H31A,H31B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21),
 C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
  C35(H35), C36(H36)
5.e Idealised Me refined with everything fixed:
 C8B(H8BA,H8BB,H8BC)
5.f Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C9B(H9BA,H9BB,
 H9BC), C10B(H10D,H10E,H10F)
;
_atom_sites_solution_hydrogens   mixed
_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 0.78478(8) 0.28919(6) 0.85762(3) 0.0425(3) Uani 1 1 d . . . . .
Ni2 Ni 0.43022(8) 0.43280(6) 0.83158(3) 0.0402(3) Uani 1 1 d . . . . .
O1 O 0.6274(3) 0.3593(3) 0.80261(14) 0.0432(7) Uani 1 1 d . . . . .
O2 O 0.6588(4) 0.1845(3) 0.92050(17) 0.0635(10) Uani 1 1 d . . . . .
O3 O 0.6571(5) 0.2152(4) 0.9836(2) 0.0788(12) Uani 1 1 d . . . . .
O4 O 0.7201(4) 0.3975(3) 0.92461(18) 0.0595(9) Uani 1 1 d . . . . .
O5 O 0.6675(6) 0.3606(7) 1.0332(3) 0.118(2) Uani 1 1 d . . . . .
O6 O 0.4141(4) 0.2987(3) 0.91192(15) 0.0490(8) Uani 1 1 d . . . . .
H6A H 0.492382 0.262613 0.919403 0.073 Uiso 1 1 d R U . . .
H6B H 0.381674 0.330445 0.945724 0.073 Uiso 1 1 d R U . . .
O7 O 0.5123(3) 0.5473(3) 0.87465(15) 0.0466(7) Uani 1 1 d . . . . .
H7A H 0.457718 0.567372 0.908643 0.070 Uiso 1 1 d R U . . .
H7B H 0.583783 0.508461 0.891043 0.070 Uiso 1 1 d R U . . .
N1 N 0.8682(4) 0.1645(3) 0.79741(18) 0.0471(9) Uani 1 1 d . . . . .
N2 N 0.9448(4) 0.1946(3) 0.90554(17) 0.0433(9) Uani 1 1 d . . . . .
N3 N 0.8978(4) 0.4055(3) 0.78982(18) 0.0448(9) Uani 1 1 d . . . . .
N4 N 0.4248(4) 0.5634(3) 0.74661(18) 0.0449(9) Uani 1 1 d . . . . .
N5 N 0.3674(4) 0.3263(3) 0.77875(18) 0.0441(9) Uani 1 1 d . . . . .
N6 N 0.2465(4) 0.5360(3) 0.85442(17) 0.0413(8) Uani 1 1 d . . . . .
C1 C 0.6612(5) 0.3577(4) 0.7390(2) 0.0458(10) Uani 1 1 d . . . . .
C2 C 0.7230(5) 0.2516(5) 0.7171(2) 0.0506(11) Uani 1 1 d . . . . .
C3 C 0.7537(6) 0.2496(6) 0.6509(2) 0.0641(14) Uani 1 1 d . . . . .
H3 H 0.795269 0.175213 0.637573 0.077 Uiso 1 1 calc R U . . .
C4 C 0.7257(7) 0.3518(6) 0.6045(3) 0.0719(15) Uani 1 1 d D . . . .
C5 C 0.6666(6) 0.4591(6) 0.6270(2) 0.0627(14) Uani 1 1 d . . . . .
H5 H 0.648133 0.531815 0.596328 0.075 Uiso 1 1 calc R U . . .
C6 C 0.6335(5) 0.4640(5) 0.6926(2) 0.0496(11) Uani 1 1 d . . . . .
C11 C 0.7653(6) 0.1380(4) 0.7642(2) 0.0500(11) Uani 1 1 d . . . . .
H11A H 0.686961 0.113294 0.796171 0.060 Uiso 1 1 calc R U . . .
H11B H 0.802212 0.069593 0.741033 0.060 Uiso 1 1 calc R U . . .
C12 C 0.9204(5) 0.0520(4) 0.8402(2) 0.0506(11) Uani 1 1 d . . . . .
H12A H 0.981492 -0.002973 0.814003 0.061 Uiso 1 1 calc R U . . .
H12B H 0.845217 0.007622 0.864361 0.061 Uiso 1 1 calc R U . . .
C13 C 0.9945(5) 0.0862(4) 0.8867(2) 0.0446(10) Uani 1 1 d . . . . .
C14 C 1.1035(5) 0.0135(4) 0.9100(2) 0.0470(11) Uani 1 1 d . . . . .
H14 H 1.136698 -0.062364 0.896494 0.056 Uiso 1 1 calc R U . . .
C15 C 1.1642(5) 0.0517(4) 0.9532(2) 0.0504(11) Uani 1 1 d . . . . .
H15 H 1.240215 0.002952 0.969152 0.060 Uiso 1 1 calc R U . . .
C16 C 1.1134(5) 0.1609(4) 0.9729(2) 0.0481(11) Uani 1 1 d . . . . .
H16 H 1.153167 0.189301 1.002593 0.058 Uiso 1 1 calc R U . . .
C17 C 1.0026(5) 0.2282(4) 0.9482(2) 0.0450(11) Uani 1 1 d . . . . .
H17 H 0.965691 0.302671 0.962647 0.054 Uiso 1 1 calc R U . . .
C18 C 0.9815(5) 0.2165(5) 0.7511(2) 0.0525(12) Uani 1 1 d . . . . .
H18A H 0.987816 0.190287 0.709357 0.063 Uiso 1 1 calc R U . . .
H18B H 1.066438 0.183994 0.768009 0.063 Uiso 1 1 calc R U . . .
C19 C 0.9627(5) 0.3543(5) 0.7405(2) 0.0467(11) Uani 1 1 d . . . . .
C20 C 1.0154(6) 0.4263(5) 0.6824(2) 0.0587(13) Uani 1 1 d . . . . .
H20 H 1.059571 0.389463 0.646893 0.070 Uiso 1 1 calc R U . . .
C21 C 1.0017(6) 0.5515(6) 0.6780(3) 0.0642(14) Uani 1 1 d . . . . .
H21 H 1.037849 0.602306 0.639464 0.077 Uiso 1 1 calc R U . . .
C22 C 0.9350(6) 0.6027(5) 0.7301(3) 0.0613(14) Uani 1 1 d . . . . .
H22 H 0.925626 0.688841 0.727985 0.074 Uiso 1 1 calc R U . . .
C23 C 0.8824(5) 0.5272(4) 0.7848(2) 0.0489(11) Uani 1 1 d . . . . .
H23 H 0.833735 0.562433 0.820037 0.059 Uiso 1 1 calc R U . . .
C24 C 0.5634(5) 0.5809(5) 0.7139(2) 0.0502(11) Uani 1 1 d . . . . .
H24A H 0.613548 0.603440 0.743787 0.060 Uiso 1 1 calc R U . . .
H24B H 0.560324 0.648416 0.675890 0.060 Uiso 1 1 calc R U . . .
C25 C 0.3497(5) 0.5207(4) 0.7053(2) 0.0502(11) Uani 1 1 d . . . . .
H25A H 0.384956 0.550961 0.659518 0.060 Uiso 1 1 calc R U . . .
H25B H 0.254387 0.555983 0.713405 0.060 Uiso 1 1 calc R U . . .
C26 C 0.3593(5) 0.3822(5) 0.7173(2) 0.0486(11) Uani 1 1 d . . . . .
C27 C 0.3559(6) 0.3161(5) 0.6717(3) 0.0576(13) Uani 1 1 d . . . . .
H27 H 0.351889 0.356725 0.628420 0.069 Uiso 1 1 calc R U . . .
C28 C 0.3584(6) 0.1897(5) 0.6880(3) 0.0630(14) Uani 1 1 d . . . . .
H28 H 0.356829 0.143180 0.656167 0.076 Uiso 1 1 calc R U . . .
C29 C 0.3632(6) 0.1329(5) 0.7513(3) 0.0599(14) Uani 1 1 d . . . . .
H29 H 0.362273 0.046777 0.764474 0.072 Uiso 1 1 calc R U . . .
C30 C 0.3694(5) 0.2042(4) 0.7947(3) 0.0506(11) Uani 1 1 d . . . . .
H30 H 0.375305 0.165341 0.838102 0.061 Uiso 1 1 calc R U . . .
C31 C 0.3540(6) 0.6779(4) 0.7664(2) 0.0499(11) Uani 1 1 d . . . . .
H31A H 0.324468 0.736169 0.728523 0.060 Uiso 1 1 calc R U . . .
H31B H 0.415008 0.716711 0.784190 0.060 Uiso 1 1 calc R U . . .
C32 C 0.2341(5) 0.6485(4) 0.8168(2) 0.0443(10) Uani 1 1 d . . . . .
C33 C 0.1175(6) 0.7302(4) 0.8264(2) 0.0500(12) Uani 1 1 d . . . . .
H33 H 0.109384 0.808966 0.799390 0.060 Uiso 1 1 calc R U . . .
C34 C 0.0149(6) 0.6977(4) 0.8743(2) 0.0510(12) Uani 1 1 d . . . . .
H34 H -0.063920 0.754096 0.881274 0.061 Uiso 1 1 calc R U . . .
C35 C 0.0267(5) 0.5820(4) 0.9126(2) 0.0475(11) Uani 1 1 d . . . . .
H35 H -0.044022 0.557001 0.945834 0.057 Uiso 1 1 calc R U . . .
C36 C 0.1433(5) 0.5043(4) 0.9015(2) 0.0442(10) Uani 1 1 d . . . . .
H36 H 0.152038 0.424852 0.927815 0.053 Uiso 1 1 calc R U . . .
C37 C 0.6819(6) 0.3341(7) 0.9814(3) 0.0707(18) Uani 1 1 d . . . . .
C7A C 0.7478(12) 0.3345(11) 0.5323(4) 0.078(2) Uani 0.768(14) 1 d D . P A 1
C8A C 0.6471(13) 0.2559(11) 0.5217(5) 0.095(3) Uani 0.768(14) 1 d D . P A 1
H8AA H 0.660578 0.173748 0.548215 0.143 Uiso 0.768(14) 1 calc R U P A 1
H8AB H 0.661045 0.249408 0.476078 0.143 Uiso 0.768(14) 1 calc R U P A 1
H8AC H 0.555569 0.294672 0.533929 0.143 Uiso 0.768(14) 1 calc R U P A 1
C9A C 0.7227(13) 0.4540(11) 0.4883(4) 0.086(3) Uani 0.768(14) 1 d D . P A 1
H9AA H 0.628109 0.487637 0.497247 0.129 Uiso 0.768(14) 1 calc R U P A 1
H9AB H 0.744703 0.442039 0.443502 0.129 Uiso 0.768(14) 1 calc R U P A 1
H9AC H 0.778727 0.511215 0.495092 0.129 Uiso 0.768(14) 1 calc R U P A 1
C10A C 0.8856(10) 0.2691(9) 0.5156(4) 0.080(3) Uani 0.768(14) 1 d D . P A 1
H10A H 0.952211 0.320762 0.517620 0.120 Uiso 0.768(14) 1 calc R U P A 1
H10B H 0.896870 0.252263 0.471865 0.120 Uiso 0.768(14) 1 calc R U P A 1
H10C H 0.897716 0.191597 0.546313 0.120 Uiso 0.768(14) 1 calc R U P A 1
C7B C 0.791(2) 0.391(3) 0.5313(8) 0.081(5) Uani 0.232(14) 1 d D . P A 2
C8B C 0.730(5) 0.309(4) 0.4979(17) 0.130(10) Uani 0.232(14) 1 d D . P A 2
H8BA H 0.757216 0.222594 0.515347 0.195 Uiso 0.2322 1 calc . U P A 2
H8BB H 0.762298 0.326350 0.451373 0.195 Uiso 0.2322 1 calc . U P A 2
H8BC H 0.632153 0.327015 0.505659 0.195 Uiso 0.2322 1 calc . U P A 2
C9B C 0.748(4) 0.517(3) 0.4966(13) 0.101(8) Uani 0.232(14) 1 d D . P A 2
H9BA H 0.650554 0.536421 0.506902 0.152 Uiso 0.232(14) 1 calc R U P A 2
H9BB H 0.773719 0.520839 0.450039 0.152 Uiso 0.232(14) 1 calc R U P A 2
H9BC H 0.791626 0.576019 0.510195 0.152 Uiso 0.232(14) 1 calc R U P A 2
C10B C 0.940(2) 0.367(4) 0.5224(13) 0.097(8) Uani 0.232(14) 1 d D . P A 2
H10D H 0.976748 0.444131 0.505243 0.146 Uiso 0.232(14) 1 calc R U P A 2
H10E H 0.971669 0.310420 0.492013 0.146 Uiso 0.232(14) 1 calc R U P A 2
H10F H 0.968760 0.329506 0.563961 0.146 Uiso 0.232(14) 1 calc R U P A 2
S1 S 1.1162(2) -0.07482(13) 0.65352(7) 0.0761(5) Uani 1 1 d . . . . .
F1 F 1.1609(7) 0.1387(4) 0.5854(2) 0.1173(18) Uani 1 1 d . . . . .
F2 F 1.3221(8) -0.0061(6) 0.5691(3) 0.143(2) Uani 1 1 d . . . . .
F3 F 1.1409(9) 0.0047(5) 0.5299(2) 0.145(3) Uani 1 1 d . . . . .
O8 O 0.9803(7) -0.0416(7) 0.6583(5) 0.146(3) Uani 1 1 d . . . . .
O9 O 1.1762(7) -0.0406(4) 0.7020(2) 0.0992(19) Uani 1 1 d . . . . .
O10 O 1.1595(5) -0.1982(3) 0.6430(2) 0.0764(12) Uani 1 1 d . . . . .
C38 C 1.1867(12) 0.0213(7) 0.5803(4) 0.101(3) Uani 1 1 d . . . . .
O11 O 0.7041(5) 0.6371(4) 0.9741(2) 0.0738(11) Uani 1 1 d G . . . .
H11C H 0.708712 0.566677 0.964907 0.111 Uiso 1 1 d G U . . .
H11D H 0.697795 0.686913 0.938796 0.111 Uiso 1 1 d G 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 O1 2.124(3) . ?
Ni1 O2 2.013(4) . ?
Ni1 O4 2.031(3) . ?
Ni1 N1 2.083(4) . ?
Ni1 N2 2.113(4) . ?
Ni1 N3 2.058(4) . ?
Ni2 O1 2.086(3) . ?
Ni2 O6 2.036(3) . ?
Ni2 O7 2.095(3) . ?
Ni2 N4 2.088(4) . ?
Ni2 N5 2.062(4) . ?
Ni2 N6 2.075(4) . ?
O1 C1 1.350(5) . ?
O2 O3 1.466(6) . ?
O3 C37 1.392(9) . ?
O4 C37 1.301(8) . ?
O5 C37 1.191(7) . ?
O6 H6A 0.8643 . ?
O6 H6B 0.8646 . ?
O7 H7A 0.8799 . ?
O7 H7B 0.8805 . ?
N1 C11 1.480(7) . ?
N1 C12 1.481(6) . ?
N1 C18 1.492(6) . ?
N2 C13 1.356(6) . ?
N2 C17 1.328(6) . ?
N3 C19 1.331(6) . ?
N3 C23 1.335(6) . ?
N4 C24 1.488(6) . ?
N4 C25 1.474(7) . ?
N4 C31 1.474(6) . ?
N5 C26 1.347(6) . ?
N5 C30 1.340(6) . ?
N6 C32 1.347(6) . ?
N6 C36 1.357(6) . ?
C1 C2 1.387(7) . ?
C1 C6 1.409(7) . ?
C2 C3 1.403(7) . ?
C2 C11 1.507(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.380(9) . ?
C4 C5 1.398(9) . ?
C4 C7A 1.576(9) . ?
C4 C7B 1.589(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.399(7) . ?
C6 C24 1.508(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.507(7) . ?
C13 C14 1.377(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.382(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.374(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(7) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.502(7) . ?
C19 C20 1.402(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.376(9) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.372(7) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.513(7) . ?
C26 C27 1.359(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.381(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.370(8) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.511(7) . ?
C32 C33 1.392(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.365(7) . ?
C34 H34 0.9500 . ?
C34 C35 1.383(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.374(7) . ?
C36 H36 0.9500 . ?
C7A C8A 1.542(18) . ?
C7A C9A 1.482(13) . ?
C7A C10A 1.498(12) . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C7B C8B 1.54(3) . ?
C7B C9B 1.49(2) . ?
C7B C10B 1.49(2) . ?
C8B H8BA 0.9800 . ?
C8B H8BB 0.9800 . ?
C8B H8BC 0.9800 . ?
C9B H9BA 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
S1 O8 1.372(8) . ?
S1 O9 1.450(5) . ?
S1 O10 1.437(4) . ?
S1 C38 1.809(9) . ?
F1 C38 1.327(9) . ?
F2 C38 1.358(13) . ?
F3 C38 1.317(10) . ?
O11 H11C 0.8490 . ?
O11 H11D 0.8482 . ?

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
O2 Ni1 O1 88.56(15) . . ?
O2 Ni1 O4 79.99(16) . . ?
O2 Ni1 N1 98.49(16) . . ?
O2 Ni1 N2 89.57(15) . . ?
O2 Ni1 N3 174.56(17) . . ?
O4 Ni1 O1 95.81(14) . . ?
O4 Ni1 N1 172.28(16) . . ?
O4 Ni1 N2 92.66(15) . . ?
O4 Ni1 N3 99.20(16) . . ?
N1 Ni1 O1 91.70(14) . . ?
N1 Ni1 N2 79.74(16) . . ?
N2 Ni1 O1 170.87(13) . . ?
N3 Ni1 O1 86.17(14) . . ?
N3 Ni1 N1 83.01(15) . . ?
N3 Ni1 N2 95.85(15) . . ?
O1 Ni2 O7 86.15(13) . . ?
O1 Ni2 N4 93.21(14) . . ?
O6 Ni2 O1 91.10(13) . . ?
O6 Ni2 O7 94.19(13) . . ?
O6 Ni2 N4 172.61(16) . . ?
O6 Ni2 N5 91.36(15) . . ?
O6 Ni2 N6 96.84(14) . . ?
N4 Ni2 O7 92.10(14) . . ?
N5 Ni2 O1 88.80(14) . . ?
N5 Ni2 O7 172.57(14) . . ?
N5 Ni2 N4 82.73(15) . . ?
N5 Ni2 N6 97.44(15) . . ?
N6 Ni2 O1 169.75(14) . . ?
N6 Ni2 O7 86.81(14) . . ?
N6 Ni2 N4 79.61(14) . . ?
Ni2 O1 Ni1 129.94(14) . . ?
C1 O1 Ni1 114.8(3) . . ?
C1 O1 Ni2 115.3(3) . . ?
O3 O2 Ni1 105.8(3) . . ?
C37 O3 O2 114.7(4) . . ?
C37 O4 Ni1 112.0(4) . . ?
Ni2 O6 H6A 110.6 . . ?
Ni2 O6 H6B 110.3 . . ?
H6A O6 H6B 103.7 . . ?
Ni2 O7 H7A 111.4 . . ?
Ni2 O7 H7B 111.2 . . ?
H7A O7 H7B 102.8 . . ?
C11 N1 Ni1 110.5(3) . . ?
C11 N1 C12 110.4(4) . . ?
C11 N1 C18 112.2(4) . . ?
C12 N1 Ni1 105.6(3) . . ?
C12 N1 C18 109.6(4) . . ?
C18 N1 Ni1 108.2(3) . . ?
C13 N2 Ni1 112.4(3) . . ?
C17 N2 Ni1 129.4(3) . . ?
C17 N2 C13 118.1(4) . . ?
C19 N3 Ni1 113.0(3) . . ?
C19 N3 C23 120.1(4) . . ?
C23 N3 Ni1 124.5(3) . . ?
C24 N4 Ni2 110.0(3) . . ?
C25 N4 Ni2 108.1(3) . . ?
C25 N4 C24 111.4(4) . . ?
C25 N4 C31 110.9(4) . . ?
C31 N4 Ni2 105.9(3) . . ?
C31 N4 C24 110.4(4) . . ?
C26 N5 Ni2 113.6(3) . . ?
C30 N5 Ni2 125.1(3) . . ?
C30 N5 C26 118.9(4) . . ?
C32 N6 Ni2 113.1(3) . . ?
C32 N6 C36 118.7(4) . . ?
C36 N6 Ni2 128.3(3) . . ?
O1 C1 C2 121.3(4) . . ?
O1 C1 C6 120.8(4) . . ?
C2 C1 C6 117.9(4) . . ?
C1 C2 C3 120.9(5) . . ?
C1 C2 C11 120.3(4) . . ?
C3 C2 C11 118.7(4) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 C2 122.3(5) . . ?
C4 C3 H3 118.8 . . ?
C3 C4 C5 116.3(5) . . ?
C3 C4 C7A 117.8(6) . . ?
C3 C4 C7B 132.0(11) . . ?
C5 C4 C7A 125.6(6) . . ?
C5 C4 C7B 107.6(12) . . ?
C4 C5 H5 118.6 . . ?
C4 C5 C6 122.8(5) . . ?
C6 C5 H5 118.6 . . ?
C1 C6 C24 120.0(4) . . ?
C5 C6 C1 119.6(5) . . ?
C5 C6 C24 120.3(4) . . ?
N1 C11 C2 108.9(4) . . ?
N1 C11 H11A 109.9 . . ?
N1 C11 H11B 109.9 . . ?
C2 C11 H11A 109.9 . . ?
C2 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N1 C12 H12A 109.8 . . ?
N1 C12 H12B 109.8 . . ?
N1 C12 C13 109.6(4) . . ?
H12A C12 H12B 108.2 . . ?
C13 C12 H12A 109.8 . . ?
C13 C12 H12B 109.8 . . ?
N2 C13 C12 115.0(4) . . ?
N2 C13 C14 121.3(5) . . ?
C14 C13 C12 123.6(4) . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.6(4) . . ?
C15 C14 H14 120.2 . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.3(5) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 121.0 . . ?
C15 C16 C17 117.9(5) . . ?
C17 C16 H16 121.0 . . ?
N2 C17 C16 123.7(4) . . ?
N2 C17 H17 118.2 . . ?
C16 C17 H17 118.2 . . ?
N1 C18 H18A 109.4 . . ?
N1 C18 H18B 109.4 . . ?
N1 C18 C19 111.4(4) . . ?
H18A C18 H18B 108.0 . . ?
C19 C18 H18A 109.4 . . ?
C19 C18 H18B 109.4 . . ?
N3 C19 C18 116.9(4) . . ?
N3 C19 C20 121.1(5) . . ?
C20 C19 C18 122.0(4) . . ?
C19 C20 H20 120.8 . . ?
C21 C20 C19 118.5(5) . . ?
C21 C20 H20 120.8 . . ?
C20 C21 H21 120.3 . . ?
C20 C21 C22 119.5(5) . . ?
C22 C21 H21 120.3 . . ?
C21 C22 H22 120.5 . . ?
C23 C22 C21 119.0(5) . . ?
C23 C22 H22 120.5 . . ?
N3 C23 C22 121.8(5) . . ?
N3 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
N4 C24 C6 109.9(4) . . ?
N4 C24 H24A 109.7 . . ?
N4 C24 H24B 109.7 . . ?
C6 C24 H24A 109.7 . . ?
C6 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
N4 C25 H25A 109.1 . . ?
N4 C25 H25B 109.1 . . ?
N4 C25 C26 112.5(4) . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
N5 C26 C25 114.6(4) . . ?
N5 C26 C27 120.8(5) . . ?
C27 C26 C25 124.5(5) . . ?
C26 C27 H27 119.8 . . ?
C26 C27 C28 120.4(5) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 120.7 . . ?
C29 C28 C27 118.7(5) . . ?
C29 C28 H28 120.7 . . ?
C28 C29 H29 121.0 . . ?
C30 C29 C28 118.0(5) . . ?
C30 C29 H29 121.0 . . ?
N5 C30 C29 123.1(5) . . ?
N5 C30 H30 118.5 . . ?
C29 C30 H30 118.5 . . ?
N4 C31 H31A 109.9 . . ?
N4 C31 H31B 109.9 . . ?
N4 C31 C32 109.1(4) . . ?
H31A C31 H31B 108.3 . . ?
C32 C31 H31A 109.9 . . ?
C32 C31 H31B 109.9 . . ?
N6 C32 C31 115.6(4) . . ?
N6 C32 C33 120.4(4) . . ?
C33 C32 C31 124.0(4) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 C32 120.4(4) . . ?
C34 C33 H33 119.8 . . ?
C33 C34 H34 120.3 . . ?
C33 C34 C35 119.4(4) . . ?
C35 C34 H34 120.3 . . ?
C34 C35 H35 120.9 . . ?
C36 C35 C34 118.3(5) . . ?
C36 C35 H35 120.9 . . ?
N6 C36 C35 122.8(4) . . ?
N6 C36 H36 118.6 . . ?
C35 C36 H36 118.6 . . ?
O4 C37 O3 116.6(5) . . ?
O5 C37 O3 113.4(7) . . ?
O5 C37 O4 130.0(8) . . ?
C8A C7A C4 111.4(8) . . ?
C9A C7A C4 110.9(7) . . ?
C9A C7A C8A 105.1(9) . . ?
C9A C7A C10A 112.6(9) . . ?
C10A C7A C4 109.3(7) . . ?
C10A C7A C8A 107.5(9) . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
C7A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C7A C9A H9AA 109.5 . . ?
C7A C9A H9AB 109.5 . . ?
C7A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C7A C10A H10A 109.5 . . ?
C7A C10A H10B 109.5 . . ?
C7A C10A H10C 109.5 . . ?
H10A C10A H10B 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C8B C7B C4 101.9(19) . . ?
C9B C7B C4 118.1(18) . . ?
C9B C7B C8B 103(2) . . ?
C10B C7B C4 111.9(16) . . ?
C10B C7B C8B 112(2) . . ?
C10B C7B C9B 109(2) . . ?
C7B C8B H8BA 109.5 . . ?
C7B C8B H8BB 109.5 . . ?
C7B C8B H8BC 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
C7B C9B H9BA 109.5 . . ?
C7B C9B H9BB 109.5 . . ?
C7B C9B H9BC 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
C7B C10B H10D 109.5 . . ?
C7B C10B H10E 109.5 . . ?
C7B C10B H10F 109.5 . . ?
H10D C10B H10E 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
O8 S1 O9 114.5(5) . . ?
O8 S1 O10 113.7(4) . . ?
O8 S1 C38 105.2(6) . . ?
O9 S1 C38 102.1(4) . . ?
O10 S1 O9 115.0(3) . . ?
O10 S1 C38 104.6(3) . . ?
F1 C38 S1 110.7(6) . . ?
F1 C38 F2 106.7(8) . . ?
F2 C38 S1 110.7(6) . . ?
F3 C38 S1 111.2(7) . . ?
F3 C38 F1 110.2(7) . . ?
F3 C38 F2 107.2(8) . . ?
H11C O11 H11D 104.7 . . ?

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
O6 H6A O2 0.86 1.79 2.642(5) 169.9 . yes
O6 H6B O11 0.86 1.86 2.710(5) 166.2 2_667 yes
O7 H7A O5 0.88 1.83 2.696(5) 167.4 2_667 yes
O7 H7B O4 0.88 1.86 2.723(5) 168.0 . 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 C1 C2 51.6(6) . . . . ?
Ni1 O1 C1 C6 -129.0(4) . . . . ?
Ni1 O2 O3 C37 28.6(5) . . . . ?
Ni1 O4 C37 O3 -16.7(6) . . . . ?
Ni1 O4 C37 O5 161.2(6) . . . . ?
Ni1 N1 C11 C2 68.2(4) . . . . ?
Ni1 N1 C12 C13 -44.8(4) . . . . ?
Ni1 N1 C18 C19 -26.1(5) . . . . ?
Ni1 N2 C13 C12 -4.2(5) . . . . ?
Ni1 N2 C13 C14 176.8(4) . . . . ?
Ni1 N2 C17 C16 -175.4(3) . . . . ?
Ni1 N3 C19 C18 -19.4(6) . . . . ?
Ni1 N3 C19 C20 163.1(4) . . . . ?
Ni1 N3 C23 C22 -163.1(4) . . . . ?
Ni2 O1 C1 C2 -129.4(4) . . . . ?
Ni2 O1 C1 C6 49.9(6) . . . . ?
Ni2 N4 C24 C6 64.7(4) . . . . ?
Ni2 N4 C25 C26 -28.1(5) . . . . ?
Ni2 N4 C31 C32 -43.0(5) . . . . ?
Ni2 N5 C26 C25 -20.2(5) . . . . ?
Ni2 N5 C26 C27 161.8(4) . . . . ?
Ni2 N5 C30 C29 -161.2(4) . . . . ?
Ni2 N6 C32 C31 -0.3(5) . . . . ?
Ni2 N6 C32 C33 -179.1(4) . . . . ?
Ni2 N6 C36 C35 178.8(4) . . . . ?
O1 C1 C2 C3 177.8(5) . . . . ?
O1 C1 C2 C11 -5.6(8) . . . . ?
O1 C1 C6 C5 -178.4(5) . . . . ?
O1 C1 C6 C24 -1.0(8) . . . . ?
O2 O3 C37 O4 -8.5(7) . . . . ?
O2 O3 C37 O5 173.3(5) . . . . ?
N1 C12 C13 N2 33.5(5) . . . . ?
N1 C12 C13 C14 -147.6(4) . . . . ?
N1 C18 C19 N3 31.3(6) . . . . ?
N1 C18 C19 C20 -151.3(5) . . . . ?
N2 C13 C14 C15 -0.3(7) . . . . ?
N3 C19 C20 C21 1.7(8) . . . . ?
N4 C25 C26 N5 33.1(6) . . . . ?
N4 C25 C26 C27 -148.9(5) . . . . ?
N4 C31 C32 N6 29.8(6) . . . . ?
N4 C31 C32 C33 -151.5(5) . . . . ?
N5 C26 C27 C28 1.2(8) . . . . ?
N6 C32 C33 C34 0.5(7) . . . . ?
C1 C2 C3 C4 0.6(10) . . . . ?
C1 C2 C11 N1 -63.1(6) . . . . ?
C1 C6 C24 N4 -65.3(6) . . . . ?
C2 C1 C6 C5 1.0(8) . . . . ?
C2 C1 C6 C24 178.4(5) . . . . ?
C2 C3 C4 C5 1.0(10) . . . . ?
C2 C3 C4 C7A -172.4(8) . . . . ?
C2 C3 C4 C7B 155.0(16) . . . . ?
C3 C2 C11 N1 113.5(5) . . . . ?
C3 C4 C5 C6 -1.6(10) . . . . ?
C3 C4 C7A C8A 67.4(10) . . . . ?
C3 C4 C7A C9A -175.9(9) . . . . ?
C3 C4 C7A C10A -51.2(12) . . . . ?
C3 C4 C7B C8B 77(2) . . . . ?
C3 C4 C7B C9B -172(2) . . . . ?
C3 C4 C7B C10B -43(3) . . . . ?
C4 C5 C6 C1 0.6(9) . . . . ?
C4 C5 C6 C24 -176.8(6) . . . . ?
C5 C4 C7A C8A -105.3(10) . . . . ?
C5 C4 C7A C9A 11.4(14) . . . . ?
C5 C4 C7A C10A 136.1(9) . . . . ?
C5 C4 C7B C8B -128(2) . . . . ?
C5 C4 C7B C9B -16(3) . . . . ?
C5 C4 C7B C10B 112(2) . . . . ?
C5 C6 C24 N4 112.1(5) . . . . ?
C6 C1 C2 C3 -1.6(8) . . . . ?
C6 C1 C2 C11 175.0(5) . . . . ?
C11 N1 C12 C13 -164.3(4) . . . . ?
C11 N1 C18 C19 96.1(5) . . . . ?
C11 C2 C3 C4 -176.1(6) . . . . ?
C12 N1 C11 C2 -175.3(4) . . . . ?
C12 N1 C18 C19 -140.8(4) . . . . ?
C12 C13 C14 C15 -179.2(4) . . . . ?
C13 N2 C17 C16 2.3(6) . . . . ?
C13 C14 C15 C16 0.9(7) . . . . ?
C14 C15 C16 C17 0.0(7) . . . . ?
C15 C16 C17 N2 -1.7(7) . . . . ?
C17 N2 C13 C12 177.7(4) . . . . ?
C17 N2 C13 C14 -1.3(6) . . . . ?
C18 N1 C11 C2 -52.7(5) . . . . ?
C18 N1 C12 C13 71.6(5) . . . . ?
C18 C19 C20 C21 -175.6(5) . . . . ?
C19 N3 C23 C22 -1.7(8) . . . . ?
C19 C20 C21 C22 -1.1(9) . . . . ?
C20 C21 C22 C23 -0.8(9) . . . . ?
C21 C22 C23 N3 2.2(9) . . . . ?
C23 N3 C19 C18 177.1(5) . . . . ?
C23 N3 C19 C20 -0.3(8) . . . . ?
C24 N4 C25 C26 92.8(5) . . . . ?
C24 N4 C31 C32 -162.0(4) . . . . ?
C25 N4 C24 C6 -55.1(5) . . . . ?
C25 N4 C31 C32 74.0(5) . . . . ?
C25 C26 C27 C28 -176.6(5) . . . . ?
C26 N5 C30 C29 -0.1(8) . . . . ?
C26 C27 C28 C29 0.5(9) . . . . ?
C27 C28 C29 C30 -1.9(9) . . . . ?
C28 C29 C30 N5 1.8(8) . . . . ?
C30 N5 C26 C25 176.6(4) . . . . ?
C30 N5 C26 C27 -1.4(7) . . . . ?
C31 N4 C24 C6 -178.8(4) . . . . ?
C31 N4 C25 C26 -143.7(4) . . . . ?
C31 C32 C33 C34 -178.1(5) . . . . ?
C32 N6 C36 C35 -0.3(7) . . . . ?
C32 C33 C34 C35 -1.1(7) . . . . ?
C33 C34 C35 C36 1.0(7) . . . . ?
C34 C35 C36 N6 -0.3(7) . . . . ?
C36 N6 C32 C31 178.9(4) . . . . ?
C36 N6 C32 C33 0.2(7) . . . . ?
C7A C4 C5 C6 171.2(8) . . . . ?
C7B C4 C5 C6 -161.6(12) . . . . ?
O8 S1 C38 F1 63.9(8) . . . . ?
O8 S1 C38 F2 -178.0(6) . . . . ?
O8 S1 C38 F3 -58.9(8) . . . . ?
O9 S1 C38 F1 -55.9(8) . . . . ?
O9 S1 C38 F2 62.2(6) . . . . ?
O9 S1 C38 F3 -178.7(7) . . . . ?
O10 S1 C38 F1 -176.0(7) . . . . ?
O10 S1 C38 F2 -58.0(6) . . . . ?
O10 S1 C38 F3 61.1(8) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 124 electrons were 
found in a volume of 456Å³ in 1 void per unit cell. 
This is consistent with the presence of 
6[H2O] per Asymmetric Unit 
which account for 120 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 0.234 0.266 0.266 456.5 124.1 '12 H2O'

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.901
_oxdiff_exptl_absorpt_empirical_full_min 0.347
####################################################################### 
# 
# 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_hll273
_database_code_depnum_ccdc_archive 'CCDC 2348003'
loop_
_audit_author_name
_audit_author_address
'Joshua Buss'
;University of Michigan
United States of America
;
_audit_update_record             
;
2024-06-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT341_hll273              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01563 Ang.  
RESPONSE: This low bond precison is a result of sub-optimal crystal quality. 
Several samples were prepared under varying growth conditions, but more 
suitable single crystals were not obtained. The present dataset, in conjunction 
with the solution spectroscopy and mass spectrometry data supports the 
structural assignment presented and is discussed judiciously in the manuscript.
;
# end Validation Reply Form

_audit_creation_date             2024-06-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H82 N12 Ni4 O6, 2(C F3 O3 S), 3[C4H8O]'
_chemical_formula_sum            'C74 H82 F6 N12 Ni4 O12 S2'
_chemical_formula_weight         1744.47
_chemical_absolute_configuration Syn
_chemical_melting_point          ?
_chemical_oxdiff_formula         C74H82F6N12Ni4O12S2
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'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   13.7338(4)
_cell_length_b                   18.9753(5)
_cell_length_c                   33.7970(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8807.6(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31537
_cell_measurement_temperature    85
_cell_measurement_theta_max      66.2850
_cell_measurement_theta_min      2.6130
_shelx_estimated_absorpt_T_max   0.906
_shelx_estimated_absorpt_T_min   0.794
_exptl_absorpt_coefficient_mu    2.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       plate
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            130494
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.153
_diffrn_reflns_theta_min         2.615
_diffrn_ambient_temperature      85
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   1.00    1.00    --  -20.00   0.00-180.00  180
  2  ω    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  3  ω    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  4  ω    -25.00  43.00   1.00    1.00    --  -20.00  36.00 120.00   68
  5  ω    -45.00   0.00   1.00    1.00    --  -20.00  72.00-180.00   45
  6  ω   -173.00-128.00   1.00    6.00    --  -92.00 -36.00 120.00   45
  7  ω   -133.00 -88.00   1.00    6.00    --  -92.00 -36.00 -60.00   45
  8  ω   -104.00 -59.00   1.00    6.00    --  -92.00  36.00  60.00   45
  9  ω   -122.00 -77.00   1.00    6.00    --  -92.00 -72.00  60.00   45
 10  ω   -174.00 -78.00   1.00    6.00    --  -92.00 -72.00-120.00   96
 11  ω    -93.00 -35.00   1.00    6.00    --  -92.00  36.00-120.00   58
 12  ω   -176.00 -77.00   1.00    6.00    --  -92.00 -72.00 -60.00   99
 13  ω   -147.00 -75.00   1.00    6.00    --  -92.00 -72.00-180.00   72
 14  ω   -176.00 -77.00   1.00    6.00    --  -92.00 -72.00 120.00   99
 15  ω   -177.00-116.00   1.00    6.00    --  -92.00 -36.00  60.00   61
 16  ω    -87.00  -9.00   1.00    6.00    --  -92.00  36.00 -60.00   78
 17  ω   -102.00 -14.00   1.00    6.00    --  -92.00  36.00   0.00   88
 18  ω   -102.00 -21.00   1.00    6.00    --  -92.00  72.00 120.00   81
 19  ω   -175.00-104.00   1.00    6.00    --  -92.00 -36.00   0.00   71
 20  ω   -104.00 -52.00   1.00    6.00    --  -92.00  72.00  60.00   52
 21  ω   -109.00 -14.00   1.00    6.00    --  -92.00  72.00-120.00   95
 22  ω   -105.00 -24.00   1.00    6.00    --  -92.00  36.00-120.00   81
 23  ω   -105.00  -2.00   1.00    6.00    --  -92.00  36.00-180.00  103
 24  ω   -106.00  -2.00   1.00    6.00    --  -92.00  72.00 -60.00  104
 25  ω   -106.00  -2.00   1.00    6.00    --  -92.00  72.00 -60.00  104
 26  ω   -107.00 -29.00   1.00    6.00    --  -92.00  72.00   0.00   78
 27  ω   -117.00 -72.00   1.00    6.00    --  -92.00  72.00 180.00   45
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0227639000
_diffrn_orient_matrix_UB_12      0.0200708000
_diffrn_orient_matrix_UB_13      -0.0431867000
_diffrn_orient_matrix_UB_21      -0.1070717000
_diffrn_orient_matrix_UB_22      -0.0215799000
_diffrn_orient_matrix_UB_23      0.0061392000
_diffrn_orient_matrix_UB_31      -0.0242991000
_diffrn_orient_matrix_UB_32      0.0756557000
_diffrn_orient_matrix_UB_33      0.0132861000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                14084
_reflns_number_total             16461
_reflns_odcompleteness_completeness 98.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.03
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_coef       0.00042(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         16461
_refine_ls_number_restraints     652
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0795
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1177P)²+12.2463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2111
_refine_ls_wR_factor_ref         0.2216
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.92(4)
 0.08(4)
2. 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 C(H,H,H,H) groups
3. Restrained distances
 C49A-F5A = C49A-F6A = C49A-F4A
 1.33 with sigma of 0.02
 C49A-S2A
 1.82 with sigma of 0.02
 S2A-O10A = S2A-O11A = S2A-O12A
 1.44 with sigma of 0.02
 O4-H4 = O5-H5 = O3-H3 = O2-H2
 0.99 with sigma of 0.02
 C49A-O12A
 2.57 with sigma of 0.04
 C49A-O10A
 2.58 with sigma of 0.04
 C49A-O11A
 2.56 with sigma of 0.04
 H4-Ni2
 2.5 with sigma of 0.04
 Ni3-H4
 2.5 with sigma of 0.04
 Ni3-H2
 2.45 with sigma of 0.04
 H2-Ni1
 2.45 with sigma of 0.04
 H5-Ni2
 2.35 with sigma of 0.04
 H5-Ni4
 2.35 with sigma of 0.04
 Ni1-H3
 2.45 with sigma of 0.04
 H3-Ni4
 2.45 with sigma of 0.04
 F2A-C48A \\sim F2B-C48B
 with sigma of 0.02
 F2A-F3A \\sim F2B-F3B
 with sigma of 0.04
 S1-O7 \\sim S1A-O7A
 with sigma of 0.02
 F1A-C48A \\sim F1B-C48B
 with sigma of 0.02
 F1A-F2A \\sim F1B-F2B
 with sigma of 0.04
 S1-F2A \\sim S1A-F2B
 with sigma of 0.04
 S1-F3A \\sim S1A-F3B
 with sigma of 0.04
 F1A-F3A \\sim F1B-F3B
 with sigma of 0.04
 F3A-C48A \\sim F3B-C48B
 with sigma of 0.04
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
 O7-O9 \\sim O7A-O9A
 with sigma of 0.04
 O7-C48A \\sim O7A-C48B
 with sigma of 0.04
 O8-O9 \\sim O8A-O9A
 with sigma of 0.04
 O8-C48A \\sim O8A-C48B
 with sigma of 0.04
 S1-O8 \\sim S1A-O8A
 with sigma of 0.02
 S1-O9 \\sim S1A-O9A
 with sigma of 0.04
 O9-C48A \\sim O9A-C48B
 with sigma of 0.04
 S1-F1A \\sim S1A-F1B
 with sigma of 0.04
 S1-C48A \\sim S1A-C48B
 with sigma of 0.02
 C40-C43A \\sim C40-C43B
 with sigma of 0.02
 S2A-O10A \\sim S2A-O11A \\sim S2A-O12A
 with sigma of 0.02
 O10A-O11A \\sim O11A-O12A \\sim O10A-O12A
 with sigma of 0.04
 C49A-F5A \\sim C49A-F6A \\sim C49A-F4A
 with sigma of 0.02
 C43A-C46A \\sim C43B-C45B
 with sigma of 0.02
 C49A-O10A \\sim C49A-O11A \\sim C49A-O12A
 with sigma of 0.04
 F5A-F6A \\sim F6A-F4A \\sim F4A-F5A
 with sigma of 0.04
 S2A-F5A \\sim S2A-F6A \\sim S2A-F4A
 with sigma of 0.04
 C43A-C45A \\sim C43B-C44B
 with sigma of 0.02
 S2A-O12A \\sim S2B-O12B
 with sigma of 0.02
 C49A-O12A \\sim C43-O12B
 with sigma of 0.04
 O10A-O12A \\sim O10B-O12B
 with sigma of 0.04
 O11A-O12A \\sim O11B-O12B
 with sigma of 0.04
 C49A-F5A \\sim C43-F4B
 with sigma of 0.02
 C49A-F6A \\sim C43-F5B
 with sigma of 0.02
 C49A-F4A \\sim C43-F6B
 with sigma of 0.02
 C49A-S2A \\sim C43-S2B
 with sigma of 0.02
 S2A-O10A \\sim S2B-O10B
 with sigma of 0.02
 C43A-C44A \\sim C43B-C46B
 with sigma of 0.02
 S2A-O11A \\sim S2B-O11B
 with sigma of 0.02
 C49A-O10A \\sim C43-O10B
 with sigma of 0.04
 C49A-O11A \\sim C43-O11B
 with sigma of 0.04
 F5A-F6A \\sim F4B-F5B
 with sigma of 0.04
 F5A-F4A \\sim F4B-F6B
 with sigma of 0.04
 C40-C46A \\sim C40-C45B
 with sigma of 0.04
 F5A-S2A \\sim F4B-S2B
 with sigma of 0.04
 F6A-F4A \\sim F5B-F6B
 with sigma of 0.04
 F6A-S2A \\sim F5B-S2B
 with sigma of 0.04
 F4A-S2A \\sim F6B-S2B
 with sigma of 0.04
 O10A-O11A \\sim O10B-O11B
 with sigma of 0.04
 C40-C45A \\sim C40-C44B
 with sigma of 0.04
 C40-C44A \\sim C40-C46B
 with sigma of 0.04
 C46A-C45A \\sim C45B-C44B
 with sigma of 0.04
 C46A-C44A \\sim C45B-C46B
 with sigma of 0.04
 C45A-C44A \\sim C44B-C46B
 with sigma of 0.04
4. Restrained angles
 Ni2-O5-H5
 fixed at 120 with sigma of 0.02
 Ni2-O4-H4
 fixed at 120 with sigma of 0.02
5. Rigid bond restraints
 S1A, S1, O7, O8, O9, C48A, F1A, F2A, F3A, F2B, F3B, C48B, O7A, O8A, O9A, F1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2A, F4A, F5A, F6A, O10A, O11A, O12A, C49A, S2B, F4B, F5B, F6B, O10B, O11B,
 O12B, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
S2A \\sim F4A \\sim F5A \\sim F6A \\sim O10A \\sim O11A \\sim O12A \\sim C49A
\\sim S2B \\sim F4B \\sim F5B \\sim F6B \\sim O10B \\sim O11B \\sim O12B \\sim
C43: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
7. Rigid body (RIGU) restrains
 S1A, S1, O7, O8, O9, C48A, F1A, F2A, F3A, O8A, O7A, C48B, F1B, F2B, F3B, O9A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2A, F4A, F5A, F6A, O10A, O11A, O12A, C49A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2A, F4A, F5A, F6A, O10A, O11A, O12A, C49A, S2B, F4B, F5B, F6B, O10B, O11B,
 O12B, C43
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C43A, C44A, H44A, H44B, H44C, C45A, H45A, H45B, H45C, C46A, H46A, H46B, H46C,
 C43B, C44B, C45B, H45D, H45E, H45F, C46B, H46D, H46E, H46F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Sof(C43B)=Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45B)=Sof(H45D)=
 Sof(H45E)=Sof(H45F)=Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(C43A)=Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45A)=Sof(H45A)=
 Sof(H45B)=Sof(H45C)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
 Sof(S2B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=Sof(C43)=1-
 FVAR(2)
 Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(C49A)=
 FVAR(2)
 Sof(S1A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(C48B)=1-
 FVAR(3)
 Sof(S1)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C48A)=FVAR(3)
9.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C25(H25A,
 H25B), C31(H31A,H31B), C47(H47A,H47B), C48(H48A,H48B), C54(H54A,H54B),
 C60(H60A,H60B), C61(H61A,H61B), C67(H67A,H67B)
9.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5A), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21),
 C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
  C35(H35), C36(H36), C39(H39), C41(H41), C50(H50), C51(H51), C52(H52),
 C53(H53), C56(H56), C57(H57), C58(H58), C59(H59), C63(H63), C64(H64), C65(H65),
  C66(H66), C69(H69), C70(H70), C71(H71), C72(H72)
9.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C44A(H44A,H44B,H44C),
 C45A(H45A,H45B,H45C), C46A(H46A,H46B,H46C), C44B(H44D,H44E,H44F), C45B(H45D,
 H45E,H45F), C46B(H46D,H46E,H46F)
;
_atom_sites_solution_hydrogens   mixed
_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 0.38487(10) 0.58964(8) 0.30756(4) 0.0534(4) Uani 1 1 d D . . . .
Ni2 Ni 0.46543(10) 0.39583(8) 0.32554(4) 0.0553(4) Uani 1 1 d D . . . .
Ni3 Ni 0.35406(11) 0.50403(9) 0.40705(4) 0.0614(4) Uani 1 1 d D . . . .
Ni4 Ni 0.20112(10) 0.44391(8) 0.31542(5) 0.0584(4) Uani 1 1 d D . . . .
O1 O 0.4816(4) 0.5008(3) 0.29940(16) 0.0528(13) Uani 1 1 d . . . . .
O2 O 0.3468(5) 0.5794(4) 0.3644(2) 0.0638(15) Uani 1 1 d D . . . .
O3 O 0.2811(4) 0.5199(3) 0.28981(18) 0.0580(15) Uani 1 1 d D . . . .
O4 O 0.4561(5) 0.4487(4) 0.3770(2) 0.0663(16) Uani 1 1 d D . . . .
O5 O 0.3208(4) 0.3820(4) 0.3227(2) 0.0635(16) Uani 1 1 d D . . . .
O6 O 0.2222(4) 0.4650(4) 0.37902(19) 0.0617(16) Uani 1 1 d . . . . .
N1 N 0.4145(5) 0.6194(4) 0.2473(2) 0.0537(16) Uani 1 1 d . . . . .
N2 N 0.5083(5) 0.6505(4) 0.3175(2) 0.0521(16) Uani 1 1 d . . . . .
N3 N 0.2887(5) 0.6753(4) 0.2999(2) 0.0547(16) Uani 1 1 d . . . . .
N4 N 0.6216(5) 0.3884(4) 0.3302(2) 0.0571(17) Uani 1 1 d . . . . .
N5 N 0.4845(5) 0.2980(5) 0.3544(2) 0.0620(19) Uani 1 1 d . . . . .
N6 N 0.4941(5) 0.3589(4) 0.2694(2) 0.0543(16) Uani 1 1 d . . . . .
N7 N 0.2680(7) 0.5656(5) 0.4471(2) 0.073(2) Uani 1 1 d . . . . .
N8 N 0.4608(6) 0.5620(5) 0.4380(2) 0.0657(19) Uani 1 1 d . . . . .
N9 N 0.3314(7) 0.4293(5) 0.4490(3) 0.073(2) Uani 1 1 d . . . . .
N10 N 0.1056(6) 0.3585(4) 0.3315(3) 0.0630(19) Uani 1 1 d . . . . .
N11 N 0.0721(5) 0.5025(5) 0.3204(2) 0.0634(19) Uani 1 1 d . . . . .
N12 N 0.1659(5) 0.4015(4) 0.2603(2) 0.0562(17) Uani 1 1 d . . . . .
C1 C 0.5595(6) 0.5115(4) 0.2773(2) 0.0493(18) Uani 1 1 d . . . . .
C2 C 0.5521(6) 0.5402(5) 0.2379(2) 0.0509(18) Uani 1 1 d . . . . .
C3 C 0.6365(6) 0.5517(5) 0.2161(3) 0.0556(19) Uani 1 1 d . . . . .
H3A H 0.629797 0.571448 0.190409 0.067 Uiso 1 1 calc R U . . .
C4 C 0.7297(6) 0.5362(5) 0.2292(3) 0.058(2) Uani 1 1 d . . . . .
C5 C 0.7350(7) 0.5094(4) 0.2687(3) 0.0541(19) Uani 1 1 d . . . . .
H5A H 0.797415 0.500970 0.279921 0.065 Uiso 1 1 calc R U . . .
C6 C 0.6540(6) 0.4953(5) 0.2912(3) 0.0544(19) Uani 1 1 d . . . . .
C7 C 0.8227(7) 0.5515(5) 0.2067(3) 0.062(2) Uani 1 1 d . . . . .
C8 C 0.8797(8) 0.4811(6) 0.2010(4) 0.086(3) Uani 1 1 d . . . . .
H8A H 0.897444 0.461800 0.226871 0.130 Uiso 1 1 calc R U . . .
H8B H 0.938896 0.490157 0.185580 0.130 Uiso 1 1 calc R U . . .
H8C H 0.838629 0.447244 0.186819 0.130 Uiso 1 1 calc R U . . .
C9 C 0.8048(8) 0.5864(6) 0.1670(4) 0.078(3) Uani 1 1 d . . . . .
H9A H 0.764715 0.555417 0.150470 0.117 Uiso 1 1 calc R U . . .
H9B H 0.867300 0.594969 0.153819 0.117 Uiso 1 1 calc R U . . .
H9C H 0.770999 0.631282 0.170997 0.117 Uiso 1 1 calc R U . . .
C10 C 0.8898(9) 0.6014(7) 0.2305(4) 0.087(3) Uani 1 1 d . . . . .
H10A H 0.858002 0.647385 0.233514 0.130 Uiso 1 1 calc R U . . .
H10B H 0.951558 0.607399 0.216402 0.130 Uiso 1 1 calc R U . . .
H10C H 0.902273 0.581211 0.256711 0.130 Uiso 1 1 calc R U . . .
C11 C 0.4544(6) 0.5603(5) 0.2230(2) 0.0547(19) Uani 1 1 d . . . . .
H11A H 0.410011 0.519224 0.224450 0.066 Uiso 1 1 calc R U . . .
H11B H 0.459198 0.575068 0.194956 0.066 Uiso 1 1 calc R U . . .
C12 C 0.4820(6) 0.6798(5) 0.2488(3) 0.056(2) Uani 1 1 d . . . . .
H12A H 0.444322 0.724164 0.250851 0.067 Uiso 1 1 calc R U . . .
H12B H 0.520566 0.681661 0.224026 0.067 Uiso 1 1 calc R U . . .
C13 C 0.5508(6) 0.6734(5) 0.2843(3) 0.056(2) Uani 1 1 d . . . . .
C14 C 0.6476(6) 0.6947(5) 0.2837(3) 0.0554(19) Uani 1 1 d . . . . .
H14 H 0.676440 0.712044 0.260045 0.066 Uiso 1 1 calc R U . . .
C15 C 0.7009(7) 0.6902(5) 0.3182(3) 0.069(3) Uani 1 1 d . . . . .
H15 H 0.768237 0.701663 0.318204 0.083 Uiso 1 1 calc R U . . .
C16 C 0.6565(6) 0.6692(5) 0.3524(3) 0.057(2) Uani 1 1 d . . . . .
H16 H 0.691679 0.668438 0.376590 0.068 Uiso 1 1 calc R U . . .
C17 C 0.5586(7) 0.6488(5) 0.3513(3) 0.062(2) Uani 1 1 d . . . . .
H17 H 0.527593 0.633456 0.374898 0.075 Uiso 1 1 calc R U . . .
C18 C 0.3175(6) 0.6414(5) 0.2317(3) 0.057(2) Uani 1 1 d . . . . .
H18A H 0.278938 0.598945 0.225054 0.068 Uiso 1 1 calc R U . . .
H18B H 0.326778 0.668929 0.207084 0.068 Uiso 1 1 calc R U . . .
C19 C 0.2627(6) 0.6849(5) 0.2610(3) 0.056(2) Uani 1 1 d . . . . .
C20 C 0.1876(6) 0.7292(5) 0.2512(3) 0.064(2) Uani 1 1 d . . . . .
H20 H 0.168314 0.734754 0.224388 0.076 Uiso 1 1 calc R U . . .
C21 C 0.1404(7) 0.7660(6) 0.2811(3) 0.068(2) Uani 1 1 d . . . . .
H21 H 0.088014 0.796681 0.274780 0.081 Uiso 1 1 calc R U . . .
C22 C 0.1694(6) 0.7579(6) 0.3204(3) 0.066(2) Uani 1 1 d . . . . .
H22 H 0.138913 0.783501 0.341171 0.080 Uiso 1 1 calc R U . . .
C23 C 0.2427(7) 0.7121(5) 0.3278(3) 0.061(2) Uani 1 1 d . . . . .
H23 H 0.262674 0.705805 0.354451 0.073 Uiso 1 1 calc R U . . .
C24 C 0.6650(6) 0.4602(4) 0.3309(3) 0.0509(18) Uani 1 1 d . . . . .
H24A H 0.734887 0.456922 0.337836 0.061 Uiso 1 1 calc R U . . .
H24B H 0.632207 0.488975 0.351420 0.061 Uiso 1 1 calc R U . . .
C25 C 0.6379(6) 0.3517(5) 0.3678(3) 0.056(2) Uani 1 1 d . . . . .
H25A H 0.627562 0.385042 0.389965 0.068 Uiso 1 1 calc R U . . .
H25B H 0.706125 0.335089 0.369010 0.068 Uiso 1 1 calc R U . . .
C26 C 0.5715(7) 0.2908(5) 0.3725(3) 0.059(2) Uani 1 1 d . . . . .
C27 C 0.5941(7) 0.2307(6) 0.3938(3) 0.066(2) Uani 1 1 d . . . . .
H27 H 0.655207 0.227002 0.406803 0.079 Uiso 1 1 calc R U . . .
C28 C 0.5289(8) 0.1771(6) 0.3960(3) 0.071(3) Uani 1 1 d . . . . .
H28 H 0.545010 0.134970 0.409654 0.085 Uiso 1 1 calc R U . . .
C29 C 0.4394(8) 0.1844(6) 0.3783(3) 0.072(3) Uani 1 1 d . . . . .
H29 H 0.392284 0.147968 0.380259 0.086 Uiso 1 1 calc R U . . .
C30 C 0.4189(7) 0.2455(5) 0.3576(3) 0.059(2) Uani 1 1 d . . . . .
H30 H 0.356953 0.250654 0.345430 0.071 Uiso 1 1 calc R U . . .
C31 C 0.6552(7) 0.3464(5) 0.2961(3) 0.058(2) Uani 1 1 d . . . . .
H31A H 0.722323 0.360976 0.289186 0.069 Uiso 1 1 calc R U . . .
H31B H 0.657234 0.296055 0.303755 0.069 Uiso 1 1 calc R U . . .
C32 C 0.5925(6) 0.3544(5) 0.2611(3) 0.057(2) Uani 1 1 d . . . . .
C33 C 0.6242(7) 0.3517(5) 0.2219(3) 0.059(2) Uani 1 1 d . . . . .
H33 H 0.691893 0.350004 0.216186 0.070 Uiso 1 1 calc R U . . .
C34 C 0.5574(7) 0.3513(5) 0.1916(3) 0.064(2) Uani 1 1 d . . . . .
H34 H 0.578242 0.347499 0.164854 0.077 Uiso 1 1 calc R U . . .
C35 C 0.4604(7) 0.3567(5) 0.2004(3) 0.064(2) Uani 1 1 d . . . . .
H35 H 0.413354 0.357439 0.179841 0.077 Uiso 1 1 calc R U . . .
C36 C 0.4311(7) 0.3609(5) 0.2397(3) 0.062(2) Uani 1 1 d . . . . .
H36 H 0.363665 0.365388 0.245513 0.074 Uiso 1 1 calc R U . . .
C37 C 0.1466(7) 0.4553(6) 0.4029(3) 0.067(2) Uani 1 1 d . . . . .
C38 C 0.1159(8) 0.5084(6) 0.4286(3) 0.073(3) Uani 1 1 d . . . . .
C39 C 0.0328(8) 0.4947(7) 0.4521(3) 0.079(3) Uani 1 1 d . . . . .
H39 H 0.011379 0.530602 0.469599 0.095 Uiso 1 1 calc R U . . .
C40 C -0.0205(8) 0.4310(7) 0.4511(3) 0.081(3) Uani 1 1 d D . . . .
C41 C 0.0135(8) 0.3789(7) 0.4251(4) 0.079(3) Uani 1 1 d . . . . .
H41 H -0.020363 0.335410 0.423311 0.095 Uiso 1 1 calc R U . . .
C42 C 0.0961(7) 0.3898(5) 0.4019(3) 0.067(2) Uani 1 1 d . . . . .
C47 C 0.1669(8) 0.5758(6) 0.4321(3) 0.071(3) Uani 1 1 d . . . . .
H47A H 0.130738 0.606900 0.450515 0.086 Uiso 1 1 calc R U . . .
H47B H 0.169062 0.599145 0.405954 0.086 Uiso 1 1 calc R U . . .
C48 C 0.3170(8) 0.6339(7) 0.4491(3) 0.077(3) Uani 1 1 d . . . . .
H48A H 0.293735 0.660067 0.472603 0.092 Uiso 1 1 calc R U . . .
H48B H 0.300820 0.661885 0.425281 0.092 Uiso 1 1 calc R U . . .
C49 C 0.4303(9) 0.6239(6) 0.4518(3) 0.074(3) Uani 1 1 d . . . . .
C50 C 0.4897(10) 0.6755(9) 0.4663(4) 0.092(4) Uani 1 1 d . . . . .
H50 H 0.463892 0.718982 0.475482 0.111 Uiso 1 1 calc R U . . .
C51 C 0.5874(9) 0.6626(7) 0.4672(4) 0.085(3) Uani 1 1 d . . . . .
H51 H 0.630650 0.696899 0.477715 0.102 Uiso 1 1 calc R U . . .
C52 C 0.6237(9) 0.5993(7) 0.4527(3) 0.080(3) Uani 1 1 d . . . . .
H52 H 0.691675 0.589931 0.452256 0.096 Uiso 1 1 calc R U . . .
C53 C 0.5583(7) 0.5514(7) 0.4392(3) 0.072(3) Uani 1 1 d . . . . .
H53 H 0.582514 0.507420 0.430015 0.087 Uiso 1 1 calc R U . . .
C54 C 0.2675(10) 0.5263(7) 0.4854(3) 0.084(3) Uani 1 1 d . . . . .
H54A H 0.321890 0.543424 0.502031 0.101 Uiso 1 1 calc R U . . .
H54B H 0.205978 0.536520 0.499538 0.101 Uiso 1 1 calc R U . . .
C55 C 0.2769(10) 0.4494(7) 0.4803(3) 0.086(4) Uani 1 1 d . . . . .
C56 C 0.2411(12) 0.3998(9) 0.5088(4) 0.104(4) Uani 1 1 d . . . . .
H56 H 0.205740 0.413510 0.531678 0.125 Uiso 1 1 calc R U . . .
C57 C 0.262(2) 0.3325(10) 0.5003(6) 0.157(9) Uani 1 1 d . . . . .
H57 H 0.238606 0.297878 0.518275 0.189 Uiso 1 1 calc R U . . .
C58 C 0.3135(18) 0.3086(10) 0.4685(6) 0.141(8) Uani 1 1 d . . . . .
H58 H 0.325905 0.260210 0.463276 0.169 Uiso 1 1 calc R U . . .
C59 C 0.3458(11) 0.3637(6) 0.4444(4) 0.084(3) Uani 1 1 d . . . . .
H59 H 0.383084 0.350590 0.421882 0.101 Uiso 1 1 calc R U . . .
C60 C 0.1241(7) 0.3331(6) 0.3728(3) 0.075(3) Uani 1 1 d . . . . .
H60A H 0.193836 0.321208 0.375998 0.091 Uiso 1 1 calc R U . . .
H60B H 0.085380 0.290014 0.377954 0.091 Uiso 1 1 calc R U . . .
C61 C 0.0032(6) 0.3875(6) 0.3272(3) 0.068(3) Uani 1 1 d . . . . .
H61A H -0.020683 0.377660 0.300147 0.082 Uiso 1 1 calc R U . . .
H61B H -0.040326 0.363064 0.346103 0.082 Uiso 1 1 calc R U . . .
C62 C -0.0010(6) 0.4631(6) 0.3345(3) 0.061(2) Uani 1 1 d . . . . .
C63 C -0.0768(7) 0.4964(7) 0.3558(3) 0.075(3) Uani 1 1 d . . . . .
H63 H -0.127078 0.468749 0.367199 0.090 Uiso 1 1 calc R U . . .
C64 C -0.0785(6) 0.5682(6) 0.3600(3) 0.067(3) Uani 1 1 d . . . . .
H64 H -0.129225 0.591223 0.374097 0.080 Uiso 1 1 calc R U . . .
C65 C -0.0052(7) 0.6045(7) 0.3434(3) 0.071(3) Uani 1 1 d . . . . .
H65 H -0.004902 0.654426 0.345341 0.086 Uiso 1 1 calc R U . . .
C66 C 0.0689(7) 0.5716(5) 0.3237(3) 0.064(2) Uani 1 1 d . . . . .
H66 H 0.119172 0.599186 0.312094 0.077 Uiso 1 1 calc R U . . .
C67 C 0.1270(7) 0.3040(5) 0.3026(3) 0.066(2) Uani 1 1 d . . . . .
H67A H 0.074662 0.268195 0.303179 0.079 Uiso 1 1 calc R U . . .
H67B H 0.188798 0.280416 0.309888 0.079 Uiso 1 1 calc R U . . .
C68 C 0.1357(7) 0.3332(5) 0.2615(3) 0.064(2) Uani 1 1 d . . . . .
C69 C 0.1098(7) 0.2969(5) 0.2272(4) 0.071(3) Uani 1 1 d . . . . .
H69 H 0.085590 0.250063 0.228721 0.086 Uiso 1 1 calc R U . . .
C70 C 0.1196(6) 0.3293(6) 0.1915(3) 0.063(2) Uani 1 1 d . . . . .
H70 H 0.105708 0.304036 0.167853 0.076 Uiso 1 1 calc R U . . .
C71 C 0.1500(6) 0.3992(5) 0.1893(3) 0.059(2) Uani 1 1 d . . . . .
H71 H 0.154917 0.423145 0.164656 0.071 Uiso 1 1 calc R U . . .
C72 C 0.1728(6) 0.4326(5) 0.2249(3) 0.060(2) Uani 1 1 d . . . . .
H72 H 0.194435 0.480062 0.223902 0.072 Uiso 1 1 calc R U . . .
C43A C -0.1148(13) 0.4121(14) 0.4736(6) 0.082(8) Uani 0.56(2) 1 d D . P A 1
C44A C -0.1870(12) 0.4718(13) 0.4653(8) 0.093(10) Uani 0.56(2) 1 d D . P A 1
H44A H -0.225400 0.481224 0.489171 0.139 Uiso 0.56(2) 1 calc R U P A 1
H44B H -0.230578 0.457956 0.443706 0.139 Uiso 0.56(2) 1 calc R U P A 1
H44C H -0.151215 0.514403 0.457765 0.139 Uiso 0.56(2) 1 calc R U P A 1
C45A C -0.1677(13) 0.3435(11) 0.4631(7) 0.093(7) Uani 0.56(2) 1 d D . P A 1
H45A H -0.183540 0.343383 0.434828 0.139 Uiso 0.56(2) 1 calc R U P A 1
H45B H -0.227766 0.339992 0.478594 0.139 Uiso 0.56(2) 1 calc R U P A 1
H45C H -0.125447 0.303303 0.469157 0.139 Uiso 0.56(2) 1 calc R U P A 1
C46A C -0.084(2) 0.409(2) 0.5164(7) 0.097(9) Uani 0.56(2) 1 d D . P A 1
H46A H -0.054559 0.362686 0.521811 0.146 Uiso 0.56(2) 1 calc R U P A 1
H46B H -0.140833 0.415467 0.533426 0.146 Uiso 0.56(2) 1 calc R U P A 1
H46C H -0.036118 0.445961 0.521663 0.146 Uiso 0.56(2) 1 calc R U P A 1
C43B C -0.1111(15) 0.4302(14) 0.4780(7) 0.070(9) Uani 0.44(2) 1 d D . P A 2
C44B C -0.1989(15) 0.4111(18) 0.4513(8) 0.081(9) Uani 0.44(2) 1 d D . P A 2
H44D H -0.209239 0.448630 0.431865 0.122 Uiso 0.44(2) 1 calc R U P A 2
H44E H -0.257325 0.405786 0.467666 0.122 Uiso 0.44(2) 1 calc R U P A 2
H44F H -0.185538 0.366671 0.437518 0.122 Uiso 0.44(2) 1 calc R U P A 2
C45B C -0.096(3) 0.370(2) 0.5062(12) 0.116(16) Uani 0.44(2) 1 d D . P A 2
H45D H -0.032333 0.375186 0.518942 0.174 Uiso 0.44(2) 1 calc R U P A 2
H45E H -0.098986 0.325727 0.491787 0.174 Uiso 0.44(2) 1 calc R U P A 2
H45F H -0.147264 0.371352 0.526443 0.174 Uiso 0.44(2) 1 calc R U P A 2
C46B C -0.137(2) 0.4987(17) 0.4996(10) 0.107(11) Uani 0.44(2) 1 d D . P A 2
H46D H -0.205578 0.496944 0.507987 0.161 Uiso 0.44(2) 1 calc R U P A 2
H46E H -0.127609 0.538810 0.481800 0.161 Uiso 0.44(2) 1 calc R U P A 2
H46F H -0.095434 0.504061 0.522916 0.161 Uiso 0.44(2) 1 calc R U P A 2
S1 S 0.1272(2) 0.69480(16) 0.13019(10) 0.0603(8) Uani 0.870(8) 1 d D U P B 1
O7 O 0.0265(7) 0.6978(5) 0.1428(4) 0.090(3) Uani 0.870(8) 1 d D U P B 1
O8 O 0.1457(8) 0.7095(6) 0.0888(3) 0.094(3) Uani 0.870(8) 1 d D U P B 1
O9 O 0.1940(10) 0.7287(5) 0.1572(4) 0.070(2) Uani 0.870(8) 1 d D U P B 1
S2A S -0.0956(7) 0.7563(5) 0.4288(2) 0.117(2) Uani 0.578(8) 1 d D U P C 1
F1A F 0.1414(7) 0.5800(4) 0.1729(3) 0.108(2) Uani 0.870(8) 1 d D U P B 1
F2A F 0.0997(11) 0.5613(5) 0.1138(4) 0.143(4) Uani 0.870(8) 1 d D U P B 1
F3A F 0.2518(8) 0.5924(5) 0.1278(5) 0.133(4) Uani 0.870(8) 1 d D U P B 1
F4A F 0.0115(15) 0.8541(10) 0.3911(5) 0.150(5) Uani 0.578(8) 1 d D U P C 1
F5A F -0.0247(16) 0.8818(9) 0.4502(5) 0.143(5) Uani 0.578(8) 1 d D U P C 1
F6A F -0.1348(16) 0.8844(9) 0.4055(6) 0.154(5) Uani 0.578(8) 1 d D U P C 1
O10A O -0.1215(18) 0.7284(11) 0.3913(5) 0.122(5) Uani 0.578(8) 1 d D U P C 1
O11A O -0.0163(15) 0.7223(10) 0.4477(6) 0.134(4) Uani 0.578(8) 1 d D U P C 1
O12A O -0.1740(17) 0.7685(15) 0.4570(6) 0.131(5) Uani 0.578(8) 1 d D U P C 1
C48A C 0.1537(11) 0.6035(7) 0.1359(5) 0.088(2) Uani 0.870(8) 1 d D U P B 1
C49A C -0.0590(14) 0.8465(10) 0.4189(5) 0.131(4) Uani 0.578(8) 1 d D U P C 1
S2B S -0.1265(10) 0.7172(7) 0.4329(3) 0.119(3) Uani 0.422(8) 1 d D U P C 2
F4B F 0.0530(18) 0.7110(14) 0.4051(7) 0.151(6) Uani 0.422(8) 1 d D U P C 2
F5B F 0.0404(19) 0.7178(13) 0.4686(7) 0.145(5) Uani 0.422(8) 1 d D U P C 2
F6B F 0.0078(19) 0.8089(11) 0.4356(8) 0.144(4) Uani 0.422(8) 1 d D U P C 2
O10B O -0.151(3) 0.7412(18) 0.3939(7) 0.130(6) Uani 0.422(8) 1 d D U P C 2
O11B O -0.141(3) 0.6436(10) 0.4366(9) 0.149(7) Uani 0.422(8) 1 d D U P C 2
O12B O -0.161(3) 0.7586(18) 0.4659(8) 0.126(6) Uani 0.422(8) 1 d D U P C 2
C43 C 0.002(2) 0.7383(13) 0.4345(7) 0.127(4) Uani 0.422(8) 1 d D U P C 2
H2 H 0.375(10) 0.620(3) 0.3780(14) 0.191 Uiso 1 1 d D U . . .
H3 H 0.323(6) 0.490(3) 0.272(3) 0.191 Uiso 1 1 d D U . . .
H4 H 0.481(9) 0.414(5) 0.3969(13) 0.191 Uiso 1 1 d D U . . .
H5 H 0.310(4) 0.376(6) 0.3514(12) 0.191 Uiso 1 1 d D U . D 1
S1A S 0.1307(15) 0.6704(16) 0.1472(7) 0.080(6) Uani 0.130(8) 1 d D U P B 2
O7A O 0.196(4) 0.728(3) 0.1498(14) 0.062(8) Uani 0.130(8) 1 d D U P B 2
O8A O 0.102(3) 0.636(2) 0.1840(9) 0.067(7) Uani 0.130(8) 1 d D U P B 2
O9A O 0.050(3) 0.680(3) 0.1199(14) 0.081(8) Uani 0.130(8) 1 d D U P B 2
F1B F 0.236(3) 0.626(3) 0.0879(10) 0.081(8) Uani 0.130(8) 1 d D U P B 2
F2B F 0.285(3) 0.587(3) 0.1434(13) 0.079(8) Uani 0.130(8) 1 d D U P B 2
F3B F 0.148(3) 0.546(2) 0.1168(13) 0.081(9) Uani 0.130(8) 1 d D U P B 2
C48B C 0.205(3) 0.605(2) 0.1233(11) 0.078(7) Uani 0.130(8) 1 d D 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 O1 2.165(6) . ?
Ni1 O2 1.999(7) . ?
Ni1 O3 2.036(6) . ?
Ni1 N1 2.153(8) . ?
Ni1 N2 2.078(7) . ?
Ni1 N3 2.110(7) . ?
Ni2 O1 2.190(6) . ?
Ni2 O4 2.010(7) . ?
Ni2 O5 2.005(6) . ?
Ni2 N4 2.155(7) . ?
Ni2 N5 2.114(8) . ?
Ni2 N6 2.062(8) . ?
Ni3 O2 2.033(7) . ?
Ni3 O4 2.026(7) . ?
Ni3 O6 2.174(7) . ?
Ni3 N7 2.142(9) . ?
Ni3 N8 2.110(9) . ?
Ni3 N9 2.029(9) . ?
Ni4 O3 2.008(6) . ?
Ni4 O5 2.035(6) . ?
Ni4 O6 2.206(7) . ?
Ni4 N10 2.155(8) . ?
Ni4 N11 2.099(8) . ?
Ni4 N12 2.086(8) . ?
O1 C1 1.321(10) . ?
O2 H2 0.98(3) . ?
O3 H3 1.01(3) . ?
O4 H4 1.00(3) . ?
O5 H5 0.99(3) . ?
O6 C37 1.328(11) . ?
N1 C11 1.494(12) . ?
N1 C12 1.476(11) . ?
N1 C18 1.492(11) . ?
N2 C13 1.338(12) . ?
N2 C17 1.336(12) . ?
N3 C19 1.373(11) . ?
N3 C23 1.333(12) . ?
N4 C24 1.488(12) . ?
N4 C25 1.466(11) . ?
N4 C31 1.475(11) . ?
N5 C26 1.349(12) . ?
N5 C30 1.348(13) . ?
N6 C32 1.383(11) . ?
N6 C36 1.324(12) . ?
N7 C47 1.490(14) . ?
N7 C48 1.462(16) . ?
N7 C54 1.494(13) . ?
N8 C49 1.333(14) . ?
N8 C53 1.355(14) . ?
N9 C55 1.350(14) . ?
N9 C59 1.269(15) . ?
N10 C60 1.497(13) . ?
N10 C61 1.517(11) . ?
N10 C67 1.452(14) . ?
N11 C62 1.338(12) . ?
N11 C66 1.317(14) . ?
N12 C68 1.360(13) . ?
N12 C72 1.339(12) . ?
C1 C2 1.441(12) . ?
C1 C6 1.414(11) . ?
C2 C3 1.392(12) . ?
C2 C11 1.483(12) . ?
C3 H3A 0.9500 . ?
C3 C4 1.385(13) . ?
C4 C5 1.432(13) . ?
C4 C7 1.513(12) . ?
C5 H5A 0.9500 . ?
C5 C6 1.373(13) . ?
C6 C24 1.508(12) . ?
C7 C8 1.560(15) . ?
C7 C9 1.518(16) . ?
C7 C10 1.547(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
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 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.532(13) . ?
C13 C14 1.390(12) . ?
C14 H14 0.9500 . ?
C14 C15 1.380(14) . ?
C15 H15 0.9500 . ?
C15 C16 1.365(15) . ?
C16 H16 0.9500 . ?
C16 C17 1.400(13) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.494(13) . ?
C19 C20 1.371(13) . ?
C20 H20 0.9500 . ?
C20 C21 1.389(15) . ?
C21 H21 0.9500 . ?
C21 C22 1.396(15) . ?
C22 H22 0.9500 . ?
C22 C23 1.354(14) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.481(13) . ?
C26 C27 1.382(13) . ?
C27 H27 0.9500 . ?
C27 C28 1.357(15) . ?
C28 H28 0.9500 . ?
C28 C29 1.373(16) . ?
C29 H29 0.9500 . ?
C29 C30 1.383(14) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.472(13) . ?
C32 C33 1.395(13) . ?
C33 H33 0.9500 . ?
C33 C34 1.376(14) . ?
C34 H34 0.9500 . ?
C34 C35 1.369(14) . ?
C35 H35 0.9500 . ?
C35 C36 1.390(15) . ?
C36 H36 0.9500 . ?
C37 C38 1.396(15) . ?
C37 C42 1.423(16) . ?
C38 C39 1.414(14) . ?
C38 C47 1.463(17) . ?
C39 H39 0.9500 . ?
C39 C40 1.413(19) . ?
C40 C41 1.401(18) . ?
C40 C43A 1.545(18) . ?
C40 C43B 1.54(2) . ?
C41 H41 0.9500 . ?
C41 C42 1.395(14) . ?
C42 C60 1.506(17) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.570(16) . ?
C49 C50 1.365(18) . ?
C50 H50 0.9500 . ?
C50 C51 1.364(18) . ?
C51 H51 0.9500 . ?
C51 C52 1.390(18) . ?
C52 H52 0.9500 . ?
C52 C53 1.357(17) . ?
C53 H53 0.9500 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C55 1.47(2) . ?
C55 C56 1.433(17) . ?
C56 H56 0.9500 . ?
C56 C57 1.34(3) . ?
C57 H57 0.9500 . ?
C57 C58 1.37(3) . ?
C58 H58 0.9500 . ?
C58 C59 1.398(19) . ?
C59 H59 0.9500 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.456(16) . ?
C62 C63 1.415(15) . ?
C63 H63 0.9500 . ?
C63 C64 1.369(17) . ?
C64 H64 0.9500 . ?
C64 C65 1.343(15) . ?
C65 H65 0.9500 . ?
C65 C66 1.367(14) . ?
C66 H66 0.9500 . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.502(14) . ?
C68 C69 1.395(16) . ?
C69 H69 0.9500 . ?
C69 C70 1.362(15) . ?
C70 H70 0.9500 . ?
C70 C71 1.393(14) . ?
C71 H71 0.9500 . ?
C71 C72 1.395(14) . ?
C72 H72 0.9500 . ?
C43A C44A 1.53(3) . ?
C43A C45A 1.53(3) . ?
C43A C46A 1.51(3) . ?
C44A H44A 0.9800 . ?
C44A H44B 0.9800 . ?
C44A H44C 0.9800 . ?
C45A H45A 0.9800 . ?
C45A H45B 0.9800 . ?
C45A H45C 0.9800 . ?
C46A H46A 0.9800 . ?
C46A H46B 0.9800 . ?
C46A H46C 0.9800 . ?
C43B C44B 1.55(3) . ?
C43B C45B 1.50(3) . ?
C43B C46B 1.53(3) . ?
C44B H44D 0.9800 . ?
C44B H44E 0.9800 . ?
C44B H44F 0.9800 . ?
C45B H45D 0.9800 . ?
C45B H45E 0.9800 . ?
C45B H45F 0.9800 . ?
C46B H46D 0.9800 . ?
C46B H46E 0.9800 . ?
C46B H46F 0.9800 . ?
S1 O7 1.448(10) . ?
S1 O8 1.447(9) . ?
S1 O9 1.445(11) . ?
S1 C48A 1.780(14) . ?
S2A O10A 1.418(13) . ?
S2A O11A 1.418(13) . ?
S2A O12A 1.456(14) . ?
S2A C49A 1.815(19) . ?
F1A C48A 1.337(19) . ?
F2A C48A 1.324(17) . ?
F3A C48A 1.390(18) . ?
F4A C49A 1.357(16) . ?
F5A C49A 1.339(16) . ?
F6A C49A 1.343(16) . ?
S2B O10B 1.434(18) . ?
S2B O11B 1.414(18) . ?
S2B O12B 1.442(19) . ?
S2B C43 1.82(3) . ?
F4B C43 1.32(2) . ?
F5B C43 1.32(2) . ?
F6B C43 1.34(2) . ?
S1A O7A 1.42(3) . ?
S1A O8A 1.46(3) . ?
S1A O9A 1.45(3) . ?
S1A C48B 1.79(3) . ?
F1B C48B 1.33(3) . ?
F2B C48B 1.34(3) . ?
F3B C48B 1.39(4) . ?

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
O2 Ni1 O1 101.9(2) . . ?
O2 Ni1 O3 92.1(3) . . ?
O2 Ni1 N1 169.7(3) . . ?
O2 Ni1 N2 96.5(3) . . ?
O2 Ni1 N3 91.7(3) . . ?
O3 Ni1 O1 83.4(2) . . ?
O3 Ni1 N1 91.4(3) . . ?
O3 Ni1 N2 168.5(3) . . ?
O3 Ni1 N3 91.5(3) . . ?
N1 Ni1 O1 88.1(2) . . ?
N2 Ni1 O1 87.3(2) . . ?
N2 Ni1 N1 81.5(3) . . ?
N2 Ni1 N3 95.9(3) . . ?
N3 Ni1 O1 165.6(3) . . ?
N3 Ni1 N1 78.5(3) . . ?
O4 Ni2 O1 84.4(3) . . ?
O4 Ni2 N4 91.9(3) . . ?
O4 Ni2 N5 92.7(3) . . ?
O4 Ni2 N6 167.9(3) . . ?
O5 Ni2 O1 101.5(2) . . ?
O5 Ni2 O4 92.5(3) . . ?
O5 Ni2 N4 168.6(3) . . ?
O5 Ni2 N5 91.8(3) . . ?
O5 Ni2 N6 95.8(3) . . ?
N4 Ni2 O1 89.3(3) . . ?
N5 Ni2 O1 166.5(3) . . ?
N5 Ni2 N4 77.6(3) . . ?
N6 Ni2 O1 85.3(3) . . ?
N6 Ni2 N4 81.7(3) . . ?
N6 Ni2 N5 95.9(3) . . ?
O2 Ni3 O6 83.7(3) . . ?
O2 Ni3 N7 92.2(3) . . ?
O2 Ni3 N8 91.1(3) . . ?
O4 Ni3 O2 92.4(3) . . ?
O4 Ni3 O6 100.4(3) . . ?
O4 Ni3 N7 168.9(3) . . ?
O4 Ni3 N8 92.2(3) . . ?
O4 Ni3 N9 95.4(3) . . ?
N7 Ni3 O6 90.1(3) . . ?
N8 Ni3 O6 166.5(3) . . ?
N8 Ni3 N7 77.7(3) . . ?
N9 Ni3 O2 168.4(3) . . ?
N9 Ni3 O6 86.5(3) . . ?
N9 Ni3 N7 81.7(4) . . ?
N9 Ni3 N8 97.2(4) . . ?
O3 Ni4 O5 91.4(3) . . ?
O3 Ni4 O6 102.6(3) . . ?
O3 Ni4 N10 169.0(3) . . ?
O3 Ni4 N11 96.7(3) . . ?
O3 Ni4 N12 91.1(3) . . ?
O5 Ni4 O6 83.2(3) . . ?
O5 Ni4 N10 91.6(3) . . ?
O5 Ni4 N11 167.9(3) . . ?
O5 Ni4 N12 94.2(3) . . ?
N10 Ni4 O6 88.3(3) . . ?
N11 Ni4 O6 86.3(3) . . ?
N11 Ni4 N10 82.2(3) . . ?
N12 Ni4 O6 166.1(3) . . ?
N12 Ni4 N10 78.1(3) . . ?
N12 Ni4 N11 94.6(3) . . ?
Ni1 O1 Ni2 126.5(2) . . ?
C1 O1 Ni1 116.7(5) . . ?
C1 O1 Ni2 116.8(5) . . ?
Ni1 O2 Ni3 137.5(3) . . ?
Ni1 O2 H2 106(4) . . ?
Ni3 O2 H2 102(4) . . ?
Ni1 O3 H3 99(4) . . ?
Ni4 O3 Ni1 136.3(3) . . ?
Ni4 O3 H3 99(4) . . ?
Ni2 O4 Ni3 137.4(3) . . ?
Ni2 O4 H4 104(4) . . ?
Ni3 O4 H4 104(4) . . ?
Ni2 O5 Ni4 136.9(4) . . ?
Ni2 O5 H5 97(4) . . ?
Ni4 O5 H5 93(4) . . ?
Ni3 O6 Ni4 126.6(3) . . ?
C37 O6 Ni3 115.7(6) . . ?
C37 O6 Ni4 117.7(6) . . ?
C11 N1 Ni1 113.1(5) . . ?
C12 N1 Ni1 106.9(6) . . ?
C12 N1 C11 111.9(7) . . ?
C12 N1 C18 110.8(7) . . ?
C18 N1 Ni1 103.8(5) . . ?
C18 N1 C11 110.0(7) . . ?
C13 N2 Ni1 113.7(6) . . ?
C17 N2 Ni1 123.1(6) . . ?
C17 N2 C13 120.0(8) . . ?
C19 N3 Ni1 112.6(6) . . ?
C23 N3 Ni1 127.8(6) . . ?
C23 N3 C19 118.9(8) . . ?
C24 N4 Ni2 109.8(5) . . ?
C25 N4 Ni2 104.3(5) . . ?
C25 N4 C24 111.1(7) . . ?
C25 N4 C31 111.9(7) . . ?
C31 N4 Ni2 106.9(5) . . ?
C31 N4 C24 112.4(7) . . ?
C26 N5 Ni2 114.1(6) . . ?
C30 N5 Ni2 127.1(6) . . ?
C30 N5 C26 118.7(8) . . ?
C32 N6 Ni2 113.2(6) . . ?
C36 N6 Ni2 124.2(6) . . ?
C36 N6 C32 119.2(8) . . ?
C47 N7 Ni3 111.8(7) . . ?
C47 N7 C54 110.7(9) . . ?
C48 N7 Ni3 105.0(6) . . ?
C48 N7 C47 109.2(9) . . ?
C48 N7 C54 113.8(10) . . ?
C54 N7 Ni3 106.1(7) . . ?
C49 N8 Ni3 114.5(7) . . ?
C49 N8 C53 115.5(10) . . ?
C53 N8 Ni3 128.7(7) . . ?
C55 N9 Ni3 115.7(8) . . ?
C59 N9 Ni3 125.1(8) . . ?
C59 N9 C55 117.4(11) . . ?
C60 N10 Ni4 112.0(6) . . ?
C60 N10 C61 111.3(7) . . ?
C61 N10 Ni4 105.5(6) . . ?
C67 N10 Ni4 104.0(5) . . ?
C67 N10 C60 111.3(8) . . ?
C67 N10 C61 112.4(8) . . ?
C62 N11 Ni4 111.4(7) . . ?
C66 N11 Ni4 124.2(6) . . ?
C66 N11 C62 120.2(9) . . ?
C68 N12 Ni4 114.4(6) . . ?
C72 N12 Ni4 127.8(6) . . ?
C72 N12 C68 117.8(9) . . ?
O1 C1 C2 121.6(7) . . ?
O1 C1 C6 121.5(7) . . ?
C6 C1 C2 117.0(8) . . ?
C1 C2 C11 118.4(7) . . ?
C3 C2 C1 119.3(8) . . ?
C3 C2 C11 122.2(8) . . ?
C2 C3 H3A 117.7 . . ?
C4 C3 C2 124.6(8) . . ?
C4 C3 H3A 117.7 . . ?
C3 C4 C5 114.9(8) . . ?
C3 C4 C7 125.4(9) . . ?
C5 C4 C7 119.5(8) . . ?
C4 C5 H5A 118.6 . . ?
C6 C5 C4 122.9(8) . . ?
C6 C5 H5A 118.6 . . ?
C1 C6 C24 118.9(7) . . ?
C5 C6 C1 121.2(8) . . ?
C5 C6 C24 119.8(8) . . ?
C4 C7 C8 108.8(8) . . ?
C4 C7 C9 113.0(8) . . ?
C4 C7 C10 111.1(9) . . ?
C9 C7 C8 110.1(9) . . ?
C9 C7 C10 106.8(9) . . ?
C10 C7 C8 106.9(9) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 H11A 109.7 . . ?
N1 C11 H11B 109.7 . . ?
C2 C11 N1 109.7(7) . . ?
C2 C11 H11A 109.7 . . ?
C2 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
N1 C12 C13 110.6(7) . . ?
H12A C12 H12B 108.1 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
N2 C13 C12 114.4(7) . . ?
N2 C13 C14 121.6(9) . . ?
C14 C13 C12 123.7(8) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 C13 118.5(9) . . ?
C15 C14 H14 120.8 . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.8(9) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.2(9) . . ?
C17 C16 H16 120.4 . . ?
N2 C17 C16 120.9(10) . . ?
N2 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
N1 C18 H18A 109.3 . . ?
N1 C18 H18B 109.3 . . ?
N1 C18 C19 111.7(8) . . ?
H18A C18 H18B 107.9 . . ?
C19 C18 H18A 109.3 . . ?
C19 C18 H18B 109.3 . . ?
N3 C19 C18 115.4(8) . . ?
C20 C19 N3 120.6(9) . . ?
C20 C19 C18 123.9(8) . . ?
C19 C20 H20 120.6 . . ?
C19 C20 C21 118.9(9) . . ?
C21 C20 H20 120.6 . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.3(9) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 121.4 . . ?
C23 C22 C21 117.2(10) . . ?
C23 C22 H22 121.4 . . ?
N3 C23 C22 124.0(10) . . ?
N3 C23 H23 118.0 . . ?
C22 C23 H23 118.0 . . ?
N4 C24 C6 110.5(7) . . ?
N4 C24 H24A 109.6 . . ?
N4 C24 H24B 109.6 . . ?
C6 C24 H24A 109.6 . . ?
C6 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
N4 C25 H25A 109.3 . . ?
N4 C25 H25B 109.3 . . ?
N4 C25 C26 111.7(7) . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
N5 C26 C25 114.6(8) . . ?
N5 C26 C27 121.3(9) . . ?
C27 C26 C25 124.1(8) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.8(9) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 120.3 . . ?
C27 C28 C29 119.4(10) . . ?
C29 C28 H28 120.3 . . ?
C28 C29 H29 120.4 . . ?
C28 C29 C30 119.2(11) . . ?
C30 C29 H29 120.4 . . ?
N5 C30 C29 121.6(9) . . ?
N5 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
N4 C31 H31A 109.0 . . ?
N4 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C32 C31 N4 112.9(7) . . ?
C32 C31 H31A 109.0 . . ?
C32 C31 H31B 109.0 . . ?
N6 C32 C31 114.6(8) . . ?
N6 C32 C33 120.0(9) . . ?
C33 C32 C31 125.2(8) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 119.9(9) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 120.5 . . ?
C35 C34 C33 119.0(9) . . ?
C35 C34 H34 120.5 . . ?
C34 C35 H35 120.1 . . ?
C34 C35 C36 119.7(10) . . ?
C36 C35 H35 120.1 . . ?
N6 C36 C35 122.1(9) . . ?
N6 C36 H36 118.9 . . ?
C35 C36 H36 118.9 . . ?
O6 C37 C38 120.9(10) . . ?
O6 C37 C42 119.2(10) . . ?
C38 C37 C42 120.0(9) . . ?
C37 C38 C39 117.3(12) . . ?
C37 C38 C47 122.6(9) . . ?
C39 C38 C47 120.1(10) . . ?
C38 C39 H39 117.9 . . ?
C40 C39 C38 124.2(12) . . ?
C40 C39 H39 117.9 . . ?
C39 C40 C43A 128.4(15) . . ?
C39 C40 C43B 114.4(14) . . ?
C41 C40 C39 116.5(10) . . ?
C41 C40 C43A 115.1(15) . . ?
C41 C40 C43B 129.1(15) . . ?
C40 C41 H41 119.4 . . ?
C42 C41 C40 121.3(12) . . ?
C42 C41 H41 119.4 . . ?
C37 C42 C60 121.0(9) . . ?
C41 C42 C37 120.7(11) . . ?
C41 C42 C60 118.0(10) . . ?
N7 C47 H47A 109.4 . . ?
N7 C47 H47B 109.4 . . ?
C38 C47 N7 111.1(9) . . ?
C38 C47 H47A 109.4 . . ?
C38 C47 H47B 109.4 . . ?
H47A C47 H47B 108.0 . . ?
N7 C48 H48A 109.5 . . ?
N7 C48 H48B 109.5 . . ?
N7 C48 C49 110.6(10) . . ?
H48A C48 H48B 108.1 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
N8 C49 C48 113.4(11) . . ?
N8 C49 C50 124.8(11) . . ?
C50 C49 C48 121.8(10) . . ?
C49 C50 H50 121.1 . . ?
C51 C50 C49 117.8(13) . . ?
C51 C50 H50 121.1 . . ?
C50 C51 H51 120.0 . . ?
C50 C51 C52 120.0(12) . . ?
C52 C51 H51 120.0 . . ?
C51 C52 H52 121.3 . . ?
C53 C52 C51 117.4(11) . . ?
C53 C52 H52 121.3 . . ?
N8 C53 C52 124.4(11) . . ?
N8 C53 H53 117.8 . . ?
C52 C53 H53 117.8 . . ?
N7 C54 H54A 109.0 . . ?
N7 C54 H54B 109.0 . . ?
H54A C54 H54B 107.8 . . ?
C55 C54 N7 113.0(10) . . ?
C55 C54 H54A 109.0 . . ?
C55 C54 H54B 109.0 . . ?
N9 C55 C54 114.8(10) . . ?
N9 C55 C56 122.0(13) . . ?
C56 C55 C54 122.7(12) . . ?
C55 C56 H56 122.9 . . ?
C57 C56 C55 114.1(14) . . ?
C57 C56 H56 122.9 . . ?
C56 C57 H57 116.7 . . ?
C56 C57 C58 126.5(15) . . ?
C58 C57 H57 116.7 . . ?
C57 C58 H58 124.0 . . ?
C57 C58 C59 112.0(16) . . ?
C59 C58 H58 124.0 . . ?
N9 C59 C58 127.8(14) . . ?
N9 C59 H59 116.1 . . ?
C58 C59 H59 116.1 . . ?
N10 C60 C42 109.5(8) . . ?
N10 C60 H60A 109.8 . . ?
N10 C60 H60B 109.8 . . ?
C42 C60 H60A 109.8 . . ?
C42 C60 H60B 109.8 . . ?
H60A C60 H60B 108.2 . . ?
N10 C61 H61A 109.2 . . ?
N10 C61 H61B 109.2 . . ?
H61A C61 H61B 107.9 . . ?
C62 C61 N10 112.2(8) . . ?
C62 C61 H61A 109.2 . . ?
C62 C61 H61B 109.2 . . ?
N11 C62 C61 117.4(9) . . ?
N11 C62 C63 118.8(10) . . ?
C63 C62 C61 123.8(9) . . ?
C62 C63 H63 119.6 . . ?
C64 C63 C62 120.7(10) . . ?
C64 C63 H63 119.6 . . ?
C63 C64 H64 121.5 . . ?
C65 C64 C63 116.9(10) . . ?
C65 C64 H64 121.5 . . ?
C64 C65 H65 119.1 . . ?
C64 C65 C66 121.9(12) . . ?
C66 C65 H65 119.1 . . ?
N11 C66 C65 121.3(10) . . ?
N11 C66 H66 119.4 . . ?
C65 C66 H66 119.4 . . ?
N10 C67 H67A 109.2 . . ?
N10 C67 H67B 109.2 . . ?
N10 C67 C68 112.1(8) . . ?
H67A C67 H67B 107.9 . . ?
C68 C67 H67A 109.2 . . ?
C68 C67 H67B 109.2 . . ?
N12 C68 C67 113.7(9) . . ?
N12 C68 C69 121.7(9) . . ?
C69 C68 C67 124.5(9) . . ?
C68 C69 H69 120.4 . . ?
C70 C69 C68 119.2(10) . . ?
C70 C69 H69 120.4 . . ?
C69 C70 H70 119.8 . . ?
C69 C70 C71 120.5(10) . . ?
C71 C70 H70 119.8 . . ?
C70 C71 H71 121.5 . . ?
C70 C71 C72 117.0(8) . . ?
C72 C71 H71 121.5 . . ?
N12 C72 C71 123.8(9) . . ?
N12 C72 H72 118.1 . . ?
C71 C72 H72 118.1 . . ?
C44A C43A C40 106.3(15) . . ?
C44A C43A C45A 106.3(18) . . ?
C45A C43A C40 118.7(17) . . ?
C46A C43A C40 104.2(17) . . ?
C46A C43A C44A 113(2) . . ?
C46A C43A C45A 109(2) . . ?
C43A C44A H44A 109.5 . . ?
C43A C44A H44B 109.5 . . ?
C43A C44A H44C 109.5 . . ?
H44A C44A H44B 109.5 . . ?
H44A C44A H44C 109.5 . . ?
H44B C44A H44C 109.5 . . ?
C43A C45A H45A 109.5 . . ?
C43A C45A H45B 109.5 . . ?
C43A C45A H45C 109.5 . . ?
H45A C45A H45B 109.5 . . ?
H45A C45A H45C 109.5 . . ?
H45B C45A H45C 109.5 . . ?
C43A C46A H46A 109.5 . . ?
C43A C46A H46B 109.5 . . ?
C43A C46A H46C 109.5 . . ?
H46A C46A H46B 109.5 . . ?
H46A C46A H46C 109.5 . . ?
H46B C46A H46C 109.5 . . ?
C40 C43B C44B 106.7(17) . . ?
C45B C43B C40 106(2) . . ?
C45B C43B C44B 108(3) . . ?
C45B C43B C46B 112(3) . . ?
C46B C43B C40 117.5(19) . . ?
C46B C43B C44B 107(2) . . ?
C43B C44B H44D 109.5 . . ?
C43B C44B H44E 109.5 . . ?
C43B C44B H44F 109.5 . . ?
H44D C44B H44E 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H44E C44B H44F 109.5 . . ?
C43B C45B H45D 109.5 . . ?
C43B C45B H45E 109.5 . . ?
C43B C45B H45F 109.5 . . ?
H45D C45B H45E 109.5 . . ?
H45D C45B H45F 109.5 . . ?
H45E C45B H45F 109.5 . . ?
C43B C46B H46D 109.5 . . ?
C43B C46B H46E 109.5 . . ?
C43B C46B H46F 109.5 . . ?
H46D C46B H46E 109.5 . . ?
H46D C46B H46F 109.5 . . ?
H46E C46B H46F 109.5 . . ?
O7 S1 C48A 101.6(7) . . ?
O8 S1 O7 116.3(7) . . ?
O8 S1 C48A 104.9(7) . . ?
O9 S1 O7 113.8(8) . . ?
O9 S1 O8 114.4(7) . . ?
O9 S1 C48A 103.6(7) . . ?
O10A S2A O12A 117.3(15) . . ?
O10A S2A C49A 104.9(12) . . ?
O11A S2A O10A 115.1(12) . . ?
O11A S2A O12A 110.2(14) . . ?
O11A S2A C49A 107.4(12) . . ?
O12A S2A C49A 100.0(12) . . ?
F1A C48A S1 113.6(11) . . ?
F1A C48A F3A 104.9(13) . . ?
F2A C48A S1 114.4(11) . . ?
F2A C48A F1A 104.7(13) . . ?
F2A C48A F3A 109.9(14) . . ?
F3A C48A S1 108.9(10) . . ?
F4A C49A S2A 115.1(15) . . ?
F5A C49A S2A 115.1(14) . . ?
F5A C49A F4A 104.0(17) . . ?
F5A C49A F6A 105.8(17) . . ?
F6A C49A S2A 110.6(14) . . ?
F6A C49A F4A 105.3(18) . . ?
O10B S2B O12B 117.4(19) . . ?
O10B S2B C43 100.7(16) . . ?
O11B S2B O10B 111.2(18) . . ?
O11B S2B O12B 115.2(19) . . ?
O11B S2B C43 110.4(17) . . ?
O12B S2B C43 100.1(16) . . ?
F4B C43 S2B 114(2) . . ?
F4B C43 F5B 110(2) . . ?
F4B C43 F6B 113(2) . . ?
F5B C43 S2B 110(2) . . ?
F5B C43 F6B 104(2) . . ?
F6B C43 S2B 105.9(18) . . ?
O7A S1A O8A 118(3) . . ?
O7A S1A O9A 115(3) . . ?
O7A S1A C48B 102(3) . . ?
O8A S1A C48B 103(2) . . ?
O9A S1A O8A 113(3) . . ?
O9A S1A C48B 103(2) . . ?
F1B C48B S1A 113(3) . . ?
F1B C48B F2B 106(3) . . ?
F1B C48B F3B 106(3) . . ?
F2B C48B S1A 115(3) . . ?
F2B C48B F3B 109(3) . . ?
F3B C48B S1A 108(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 O1 C1 C2 -53.2(9) . . . . ?
Ni1 O1 C1 C6 126.8(7) . . . . ?
Ni1 N1 C11 C2 -66.1(8) . . . . ?
Ni1 N1 C12 C13 33.4(8) . . . . ?
Ni1 N1 C18 C19 42.3(8) . . . . ?
Ni1 N2 C13 C12 25.8(9) . . . . ?
Ni1 N2 C13 C14 -159.2(7) . . . . ?
Ni1 N2 C17 C16 156.9(7) . . . . ?
Ni1 N3 C19 C18 -8.8(9) . . . . ?
Ni1 N3 C19 C20 168.0(7) . . . . ?
Ni1 N3 C23 C22 -167.8(7) . . . . ?
Ni2 O1 C1 C2 128.5(7) . . . . ?
Ni2 O1 C1 C6 -51.5(10) . . . . ?
Ni2 N4 C24 C6 -69.2(7) . . . . ?
Ni2 N4 C25 C26 44.3(8) . . . . ?
Ni2 N4 C31 C32 30.3(9) . . . . ?
Ni2 N5 C26 C25 -1.6(10) . . . . ?
Ni2 N5 C26 C27 177.9(8) . . . . ?
Ni2 N5 C30 C29 -178.3(8) . . . . ?
Ni2 N6 C32 C31 25.1(10) . . . . ?
Ni2 N6 C32 C33 -160.3(7) . . . . ?
Ni2 N6 C36 C35 159.4(8) . . . . ?
Ni3 O6 C37 C38 50.8(10) . . . . ?
Ni3 O6 C37 C42 -129.7(8) . . . . ?
Ni3 N7 C47 C38 62.6(9) . . . . ?
Ni3 N7 C48 C49 -42.4(10) . . . . ?
Ni3 N7 C54 C55 -29.4(12) . . . . ?
Ni3 N8 C49 C48 11.0(12) . . . . ?
Ni3 N8 C49 C50 -167.7(10) . . . . ?
Ni3 N8 C53 C52 165.1(9) . . . . ?
Ni3 N9 C55 C54 -17.8(15) . . . . ?
Ni3 N9 C55 C56 169.4(12) . . . . ?
Ni3 N9 C59 C58 -165.6(16) . . . . ?
Ni4 O6 C37 C38 -127.2(8) . . . . ?
Ni4 O6 C37 C42 52.3(10) . . . . ?
Ni4 N10 C60 C42 66.9(8) . . . . ?
Ni4 N10 C61 C62 -29.7(9) . . . . ?
Ni4 N10 C67 C68 -43.6(8) . . . . ?
Ni4 N11 C62 C61 -26.8(11) . . . . ?
Ni4 N11 C62 C63 152.5(7) . . . . ?
Ni4 N11 C66 C65 -151.0(8) . . . . ?
Ni4 N12 C68 C67 4.2(10) . . . . ?
Ni4 N12 C68 C69 -179.7(7) . . . . ?
Ni4 N12 C72 C71 178.1(7) . . . . ?
O1 C1 C2 C3 178.9(8) . . . . ?
O1 C1 C2 C11 2.1(12) . . . . ?
O1 C1 C6 C5 -177.1(8) . . . . ?
O1 C1 C6 C24 4.4(13) . . . . ?
O6 C37 C38 C39 177.8(9) . . . . ?
O6 C37 C38 C47 -2.8(14) . . . . ?
O6 C37 C42 C41 -176.8(9) . . . . ?
O6 C37 C42 C60 -3.0(14) . . . . ?
N1 C12 C13 N2 -40.9(10) . . . . ?
N1 C12 C13 C14 144.2(9) . . . . ?
N1 C18 C19 N3 -24.0(11) . . . . ?
N1 C18 C19 C20 159.4(8) . . . . ?
N2 C13 C14 C15 1.7(13) . . . . ?
N3 C19 C20 C21 2.0(14) . . . . ?
N4 C25 C26 N5 -30.1(11) . . . . ?
N4 C25 C26 C27 150.4(9) . . . . ?
N4 C31 C32 N6 -38.1(11) . . . . ?
N4 C31 C32 C33 147.6(9) . . . . ?
N5 C26 C27 C28 1.4(16) . . . . ?
N6 C32 C33 C34 -1.8(14) . . . . ?
N7 C48 C49 N8 22.4(13) . . . . ?
N7 C48 C49 C50 -158.8(11) . . . . ?
N7 C54 C55 N9 32.5(16) . . . . ?
N7 C54 C55 C56 -154.7(13) . . . . ?
N8 C49 C50 C51 -1(2) . . . . ?
N9 C55 C56 C57 -4(3) . . . . ?
N10 C61 C62 N11 39.7(12) . . . . ?
N10 C61 C62 C63 -139.5(9) . . . . ?
N10 C67 C68 N12 28.1(11) . . . . ?
N10 C67 C68 C69 -147.8(9) . . . . ?
N11 C62 C63 C64 3.6(14) . . . . ?
N12 C68 C69 C70 3.4(14) . . . . ?
C1 C2 C3 C4 1.1(14) . . . . ?
C1 C2 C11 N1 64.5(10) . . . . ?
C1 C6 C24 N4 65.3(10) . . . . ?
C2 C1 C6 C5 2.8(13) . . . . ?
C2 C1 C6 C24 -175.6(8) . . . . ?
C2 C3 C4 C5 -2.6(14) . . . . ?
C2 C3 C4 C7 -176.8(9) . . . . ?
C3 C2 C11 N1 -112.2(9) . . . . ?
C3 C4 C5 C6 4.3(14) . . . . ?
C3 C4 C7 C8 -122.8(11) . . . . ?
C3 C4 C7 C9 -0.2(15) . . . . ?
C3 C4 C7 C10 119.8(12) . . . . ?
C4 C5 C6 C1 -4.7(14) . . . . ?
C4 C5 C6 C24 173.8(8) . . . . ?
C5 C4 C7 C8 63.1(12) . . . . ?
C5 C4 C7 C9 -174.2(9) . . . . ?
C5 C4 C7 C10 -54.2(12) . . . . ?
C5 C6 C24 N4 -113.2(9) . . . . ?
C6 C1 C2 C3 -1.1(12) . . . . ?
C6 C1 C2 C11 -177.8(8) . . . . ?
C7 C4 C5 C6 179.0(9) . . . . ?
C11 N1 C12 C13 -90.9(8) . . . . ?
C11 N1 C18 C19 163.7(7) . . . . ?
C11 C2 C3 C4 177.7(9) . . . . ?
C12 N1 C11 C2 54.7(9) . . . . ?
C12 N1 C18 C19 -72.1(9) . . . . ?
C12 C13 C14 C15 176.2(9) . . . . ?
C13 N2 C17 C16 -1.4(13) . . . . ?
C13 C14 C15 C16 -3.9(14) . . . . ?
C14 C15 C16 C17 3.5(15) . . . . ?
C15 C16 C17 N2 -0.9(14) . . . . ?
C17 N2 C13 C12 -174.0(8) . . . . ?
C17 N2 C13 C14 1.0(13) . . . . ?
C18 N1 C11 C2 178.3(7) . . . . ?
C18 N1 C12 C13 145.9(7) . . . . ?
C18 C19 C20 C21 178.5(9) . . . . ?
C19 N3 C23 C22 1.7(14) . . . . ?
C19 C20 C21 C22 0.3(15) . . . . ?
C20 C21 C22 C23 -1.6(15) . . . . ?
C21 C22 C23 N3 0.6(15) . . . . ?
C23 N3 C19 C18 -179.8(8) . . . . ?
C23 N3 C19 C20 -3.0(13) . . . . ?
C24 N4 C25 C26 162.6(7) . . . . ?
C24 N4 C31 C32 -90.3(9) . . . . ?
C25 N4 C24 C6 176.0(7) . . . . ?
C25 N4 C31 C32 143.9(8) . . . . ?
C25 C26 C27 C28 -179.2(10) . . . . ?
C26 N5 C30 C29 -1.3(14) . . . . ?
C26 C27 C28 C29 -2.5(17) . . . . ?
C27 C28 C29 C30 1.9(17) . . . . ?
C28 C29 C30 N5 0.1(16) . . . . ?
C30 N5 C26 C25 -179.0(8) . . . . ?
C30 N5 C26 C27 0.6(14) . . . . ?
C31 N4 C24 C6 49.6(9) . . . . ?
C31 N4 C25 C26 -70.8(9) . . . . ?
C31 C32 C33 C34 172.1(9) . . . . ?
C32 N6 C36 C35 1.9(14) . . . . ?
C32 C33 C34 C35 2.6(15) . . . . ?
C33 C34 C35 C36 -1.2(15) . . . . ?
C34 C35 C36 N6 -1.1(15) . . . . ?
C36 N6 C32 C31 -175.0(8) . . . . ?
C36 N6 C32 C33 -0.4(13) . . . . ?
C37 C38 C39 C40 0.1(16) . . . . ?
C37 C38 C47 N7 -62.9(13) . . . . ?
C37 C42 C60 N10 -64.5(12) . . . . ?
C38 C37 C42 C41 2.7(14) . . . . ?
C38 C37 C42 C60 176.5(9) . . . . ?
C38 C39 C40 C41 0.5(16) . . . . ?
C38 C39 C40 C43A -176.4(14) . . . . ?
C38 C39 C40 C43B -177.3(13) . . . . ?
C39 C38 C47 N7 116.4(10) . . . . ?
C39 C40 C41 C42 0.5(15) . . . . ?
C39 C40 C43A C44A 52(2) . . . . ?
C39 C40 C43A C45A 171.1(14) . . . . ?
C39 C40 C43A C46A -68(3) . . . . ?
C39 C40 C43B C44B 124.9(19) . . . . ?
C39 C40 C43B C45B -121(3) . . . . ?
C39 C40 C43B C46B 5(3) . . . . ?
C40 C41 C42 C37 -2.1(16) . . . . ?
C40 C41 C42 C60 -176.1(9) . . . . ?
C41 C40 C43A C44A -125.4(19) . . . . ?
C41 C40 C43A C45A -6(2) . . . . ?
C41 C40 C43A C46A 115(2) . . . . ?
C41 C40 C43B C44B -53(2) . . . . ?
C41 C40 C43B C45B 62(3) . . . . ?
C41 C40 C43B C46B -173(2) . . . . ?
C41 C42 C60 N10 109.5(10) . . . . ?
C42 C37 C38 C39 -1.7(14) . . . . ?
C42 C37 C38 C47 177.6(9) . . . . ?
C47 N7 C48 C49 -162.5(9) . . . . ?
C47 N7 C54 C55 92.1(12) . . . . ?
C47 C38 C39 C40 -179.3(10) . . . . ?
C48 N7 C47 C38 178.5(9) . . . . ?
C48 N7 C54 C55 -144.3(11) . . . . ?
C48 C49 C50 C51 -179.4(12) . . . . ?
C49 N8 C53 C52 -1.1(16) . . . . ?
C49 C50 C51 C52 2(2) . . . . ?
C50 C51 C52 C53 -2.1(19) . . . . ?
C51 C52 C53 N8 1.9(18) . . . . ?
C53 N8 C49 C48 179.2(9) . . . . ?
C53 N8 C49 C50 0.5(16) . . . . ?
C54 N7 C47 C38 -55.5(12) . . . . ?
C54 N7 C48 C49 73.2(11) . . . . ?
C54 C55 C56 C57 -175.8(18) . . . . ?
C55 N9 C59 C58 -1(2) . . . . ?
C55 C56 C57 C58 1(4) . . . . ?
C56 C57 C58 C59 1(4) . . . . ?
C57 C58 C59 N9 -1(3) . . . . ?
C59 N9 C55 C54 176.6(12) . . . . ?
C59 N9 C55 C56 4(2) . . . . ?
C60 N10 C61 C62 91.9(10) . . . . ?
C60 N10 C67 C68 -164.4(8) . . . . ?
C61 N10 C60 C42 -50.9(11) . . . . ?
C61 N10 C67 C68 70.0(9) . . . . ?
C61 C62 C63 C64 -177.1(10) . . . . ?
C62 N11 C66 C65 4.0(15) . . . . ?
C62 C63 C64 C65 -0.4(15) . . . . ?
C63 C64 C65 C66 -1.2(15) . . . . ?
C64 C65 C66 N11 -0.6(16) . . . . ?
C66 N11 C62 C61 175.3(9) . . . . ?
C66 N11 C62 C63 -5.4(14) . . . . ?
C67 N10 C60 C42 -177.1(8) . . . . ?
C67 N10 C61 C62 -142.4(8) . . . . ?
C67 C68 C69 C70 179.0(9) . . . . ?
C68 N12 C72 C71 0.7(13) . . . . ?
C68 C69 C70 C71 -3.6(14) . . . . ?
C69 C70 C71 C72 2.3(13) . . . . ?
C70 C71 C72 N12 -0.9(13) . . . . ?
C72 N12 C68 C67 -178.0(8) . . . . ?
C72 N12 C68 C69 -1.9(13) . . . . ?
C43A C40 C41 C42 177.9(12) . . . . ?
C43B C40 C41 C42 177.9(15) . . . . ?
O7 S1 C48A F1A -59.0(12) . . . . ?
O7 S1 C48A F2A 61.3(15) . . . . ?
O7 S1 C48A F3A -175.4(12) . . . . ?
O8 S1 C48A F1A 179.5(10) . . . . ?
O8 S1 C48A F2A -60.2(15) . . . . ?
O8 S1 C48A F3A 63.1(13) . . . . ?
O9 S1 C48A F1A 59.3(12) . . . . ?
O9 S1 C48A F2A 179.5(14) . . . . ?
O9 S1 C48A F3A -57.2(14) . . . . ?
O10A S2A C49A F4A -54.4(18) . . . . ?
O10A S2A C49A F5A -175.5(18) . . . . ?
O10A S2A C49A F6A 64.7(17) . . . . ?
O11A S2A C49A F4A 68.6(18) . . . . ?
O11A S2A C49A F5A -52(2) . . . . ?
O11A S2A C49A F6A -172.3(16) . . . . ?
O12A S2A C49A F4A -176.4(17) . . . . ?
O12A S2A C49A F5A 63(2) . . . . ?
O12A S2A C49A F6A -57.2(18) . . . . ?
O10B S2B C43 F4B -55(2) . . . . ?
O10B S2B C43 F5B -178(2) . . . . ?
O10B S2B C43 F6B 70(2) . . . . ?
O11B S2B C43 F4B 63(2) . . . . ?
O11B S2B C43 F5B -61(2) . . . . ?
O11B S2B C43 F6B -173(2) . . . . ?
O12B S2B C43 F4B -175(2) . . . . ?
O12B S2B C43 F5B 61(2) . . . . ?
O12B S2B C43 F6B -51(2) . . . . ?
O7A S1A C48B F1B -60(4) . . . . ?
O7A S1A C48B F2B 61(4) . . . . ?
O7A S1A C48B F3B -177(4) . . . . ?
O8A S1A C48B F1B 177(3) . . . . ?
O8A S1A C48B F2B -61(4) . . . . ?
O8A S1A C48B F3B 61(3) . . . . ?
O9A S1A C48B F1B 59(4) . . . . ?
O9A S1A C48B F2B -179(4) . . . . ?
O9A S1A C48B F3B -57(4) . . . . ?

_smtbx_masks_special_details     ?
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 0.316 -0.020 0.432 428.6 130.2 '3 THF'
2 0.184 0.020 0.932 428.6 130.7 '3 THF'
3 -0.184 0.520 0.568 428.6 131.6 '3 THF'
4 -0.316 0.480 0.068 428.6 130.8 '3 THF'

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.122
_oxdiff_exptl_absorpt_empirical_full_min 0.523
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.92(4)
2 0.08(4)

####################################################################### 
# 
# 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_hl524
_database_code_depnum_ccdc_archive 'CCDC 2348002'
loop_
_audit_author_name
_audit_author_address
'Joshua Buss'
;University of Michigan
United States of America
;
_audit_update_record             
;
2024-06-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT084_hl524               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: The high wR2 value is a result of sub-optimal crystal quality. 
Several samples were prepared under varying growth conditions, but more 
suitable single crystals were not obtained. Five distinct crytallization
conditions provided sub-par crystallites that were either twinned, weakly 
diffracting, or both. The present dataset, which represents the best quality 
sample we were able to obtain, in conjunction with the solution spectroscopy 
and mass spectrometry data supports the structural assignment presented and 
is discussed judiciously in the manuscript.
;
_vrf_PLAT341_hl524               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0161 Ang.  
RESPONSE: This low bond precison is a result of sub-optimal crystal quality. 
The present dataset, which represents the best quality sample we were able 
to obtain, in conjunction with the solution spectroscopy and mass spectrometry
data supports the structural assignment presented and is discussed judiciously 
in the manuscript.
;
# end Validation Reply Form

_audit_creation_date             2024-06-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C74 H82 N12 Ni4 O10, 2(C F3 O3 S), [+ solvents]'
_chemical_formula_sum            'C76 H82 F6 N12 Ni4 O16 S2'
_chemical_formula_weight         1832.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C37 H45 F3 N6 Ni2 O8 S1'
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'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.1401(9)
_cell_length_b                   32.5762(9)
_cell_length_c                   17.5728(6)
_cell_angle_alpha                90
_cell_angle_beta                 111.887(5)
_cell_angle_gamma                90
_cell_volume                     8573.5(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17266
_cell_measurement_temperature    85
_cell_measurement_theta_max      66.5910
_cell_measurement_theta_min      2.7240
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.137
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.038
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1640
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            117295
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.645
_diffrn_reflns_theta_min         2.713
_diffrn_ambient_temperature      85
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   1.00    1.00    --  -20.00   0.00-180.00  180
  2  ω    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  3  ω    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  4  ω    -25.00  43.00   1.00    1.00    --  -20.00  36.00 120.00   68
  5  ω    -45.00   0.00   1.00    1.00    --  -20.00  72.00-180.00   45
  6  ω   -173.00-128.00   1.00   20.00    --  -92.00 -36.00 120.00   45
  7  ω   -133.00 -88.00   1.00   20.00    --  -92.00 -36.00 -60.00   45
  8  ω   -104.00 -59.00   1.00   20.00    --  -92.00  36.00  60.00   45
  9  ω   -122.00 -77.00   1.00   20.00    --  -92.00 -72.00  60.00   45
 10  ω   -174.00 -78.00   1.00   20.00    --  -92.00 -72.00-120.00   96
 11  ω    -93.00 -35.00   1.00   20.00    --  -92.00  36.00-120.00   58
 12  ω   -176.00 -77.00   1.00   20.00    --  -92.00 -72.00 -60.00   99
 13  ω   -147.00 -75.00   1.00   20.00    --  -92.00 -72.00-180.00   72
 14  ω   -176.00 -77.00   1.00   20.00    --  -92.00 -72.00 120.00   99
 15  ω   -177.00-116.00   1.00   20.00    --  -92.00 -36.00  60.00   61
 16  ω    -87.00  -9.00   1.00   20.00    --  -92.00  36.00 -60.00   78
 17  ω   -102.00 -14.00   1.00   20.00    --  -92.00  36.00   0.00   88
 18  ω   -102.00 -21.00   1.00   20.00    --  -92.00  72.00 120.00   81
 19  ω   -175.00-104.00   1.00   20.00    --  -92.00 -36.00   0.00   71
 20  ω   -104.00 -52.00   1.00   20.00    --  -92.00  72.00  60.00   52
 21  ω   -109.00 -14.00   1.00   20.00    --  -92.00  72.00-120.00   95
 22  ω   -105.00 -24.00   1.00   20.00    --  -92.00  36.00-120.00   81
 23  ω   -105.00  -2.00   1.00   20.00    --  -92.00  36.00-180.00  103
 24  ω   -106.00  -2.00   1.00   20.00    --  -92.00  72.00 -60.00  104
 25  ω   -106.00  -2.00   1.00   20.00    --  -92.00  72.00 -60.00  104
 26  ω   -107.00 -29.00   1.00   20.00    --  -92.00  72.00   0.00   78
 27  ω   -117.00 -72.00   1.00   20.00    --  -92.00  72.00 180.00   45
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0946573000
_diffrn_orient_matrix_UB_12      -0.0178358000
_diffrn_orient_matrix_UB_13      -0.0408539000
_diffrn_orient_matrix_UB_21      0.0149987000
_diffrn_orient_matrix_UB_22      -0.0265446000
_diffrn_orient_matrix_UB_23      0.0765467000
_diffrn_orient_matrix_UB_31      -0.0373243000
_diffrn_orient_matrix_UB_32      0.0348315000
_diffrn_orient_matrix_UB_33      0.0374178000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11245
_reflns_number_total             15886
_reflns_odcompleteness_completeness 98.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.52
_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 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection       
'DTREK_VERSION=d*TREK version 9.9.9.4 W9RSSI -- Aug 22 2012'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.272
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         15886
_refine_ls_number_restraints     503
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.1345
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1748P)²+74.3771P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3526
_refine_ls_wR_factor_ref         0.3756
_refine_special_details          ?
_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,H) groups
2. Restrained distances
 C76B-F4B = C76B-F5B = C76B-F6B
 1.33 with sigma of 0.02
 C76B-S2B
 1.82 with sigma of 0.02
 C75B-F1B = C75B-F2B = C75B-F3B
 1.33 with sigma of 0.02
 S2B-O14B = S2B-O16B = S2B-O15B
 1.44 with sigma of 0.02
 C76B-O14B
 2.58 with sigma of 0.04
 C76B-O16B
 2.56 with sigma of 0.04
 C76B-O15B
 2.57 with sigma of 0.04
 C75B-F1B \\sim C75A-F1A
 with sigma of 0.02
 C75B-F2B \\sim C75A-F2A
 with sigma of 0.02
 C75B-F3B \\sim C75A-F3A
 with sigma of 0.02
 C9A-C7 \\sim C8B-C7 \\sim C8A-C7 \\sim C7-C10B \\sim C7-C10A \\sim C9B-C7
 with sigma of 0.02
 S1-O11B \\sim S1A-O11A
 with sigma of 0.02
 F1B-F2B \\sim F1A-F2A
 with sigma of 0.04
 F1B-F3B \\sim F1A-F3A
 with sigma of 0.04
 C8A-C9A \\sim C8A-C10A \\sim C9A-C10A
 with sigma of 0.02
 F2B-F3B \\sim F2A-F3A
 with sigma of 0.04
 C8B-C9B \\sim C8B-C10B \\sim C9B-C10B
 with sigma of 0.02
 C75B-F1B \\sim C75B-F2B \\sim C75B-F3B
 with sigma of 0.02
 F1B-F2B \\sim F2B-F3B \\sim F3B-F1B
 with sigma of 0.04
 F3B-C75B \\sim F1B-C75B \\sim F2B-C75B \\sim F1A-C75A \\sim F2A-C75A \\sim
F3A-C75A
 with sigma of 0.02
 S1A-C75A \\sim S1-C75B
 with sigma of 0.02
 S1A-O12A \\sim S1A-O13A \\sim S1A-O11A \\sim S1-O11B \\sim S1-O13B \\sim
S1-O12B
 with sigma of 0.02
 C76B-F4B \\sim C76B-F5B \\sim C76B-F6B
 with sigma of 0.02
 F4B-F5B \\sim F5B-F6B \\sim F6B-F4B
 with sigma of 0.04
 S2B-F4B \\sim S2B-F5B \\sim S2B-F6B
 with sigma of 0.04
 S2B-O14B \\sim S2B-O16B \\sim S2B-O15B
 with sigma of 0.02
 O14B-O16B \\sim O16B-O15B \\sim O14B-O15B
 with sigma of 0.04
 C76B-O14B \\sim C76B-O16B \\sim C76B-O15B
 with sigma of 0.04
 C76B-F4B \\sim C76A-F5A
 with sigma of 0.02
 C76B-F5B \\sim C76A-F6A
 with sigma of 0.02
 C76B-F6B \\sim C76A-F4A
 with sigma of 0.02
 C76B-S2B \\sim C76A-S2A
 with sigma of 0.02
 S2B-O14B \\sim S2A-O16A
 with sigma of 0.02
 S2B-O16B \\sim S2A-O15A
 with sigma of 0.02
 S2B-O15B \\sim S2A-O14A
 with sigma of 0.02
 C76B-O14B \\sim C76A-O16A
 with sigma of 0.04
 C76B-O16B \\sim C76A-O15A
 with sigma of 0.04
 C76B-O15B \\sim C76A-O14A
 with sigma of 0.04
 F4B-F5B \\sim F5A-F6A
 with sigma of 0.04
 F4B-F6B \\sim F5A-F4A
 with sigma of 0.04
 F4B-S2B \\sim F5A-S2A
 with sigma of 0.04
 F5B-F6B \\sim F6A-F4A
 with sigma of 0.04
 F5B-S2B \\sim F6A-S2A
 with sigma of 0.04
 F6B-S2B \\sim F4A-S2A
 with sigma of 0.04
 O14B-O16B \\sim O16A-O15A
 with sigma of 0.04
 O14B-O15B \\sim O16A-O14A
 with sigma of 0.04
 O16B-O15B \\sim O15A-O14A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S1 \\sim F1B \\sim F2B \\sim F3B \\sim O11B \\sim O12B \\sim O13B \\sim C75B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
S2B \\sim F4B \\sim F5B \\sim F6B \\sim O14B \\sim O15B \\sim O16B \\sim C76B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 S1, F1B, F2B, F3B, O11B, O12B, O13B, C75B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1A, F1A, F2A, F3A, O11A, O12A, O13A, C75A, S1, F1B, F2B, F3B, O11B, O12B,
 O13B, C75B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2B, F4B, F5B, F6B, O14B, O15B, O16B, C76B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2A, S2B, F4A, F4B, F5A, F5B, F6A, F6B, O14A, O14B, O15A, O15B, O16A, O16B,
 C76A, C76B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7, C8A, C9A, C10A, C8B, C9B, C10B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=
 Sof(C10B)=Sof(H10F)=Sof(H10G)=Sof(H10H)=1-FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(H10E)=FVAR(1)
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O11A)=Sof(O12A)=Sof(O13A)=Sof(C75A)=1-
 FVAR(2)
 Sof(S1)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O11B)=Sof(O12B)=Sof(O13B)=Sof(C75B)=
 FVAR(2)
 Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O14A)=Sof(O15A)=Sof(O16A)=Sof(C76A)=1-
 FVAR(3)
 Sof(S2B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O14B)=Sof(O15B)=Sof(O16B)=Sof(C76B)=
 FVAR(3)
6.a Rotating group:
 O9(H9A,H9B), O10(H10A,H10B)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C25(H25A,
 H25B), C31(H31A,H31B), C49(H49A,H49B), C50(H50A,H50B), C56(H56A,H56B),
 C62(H62A,H62B), C63(H63A,H63B), C69(H69A,H69B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21),
 C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
  C35(H35), C36(H36), C41(H41), C43(H43), C52(H52), C53(H53), C54(H54),
 C55(H55), C58(H58), C59(H59), C60(H60), C61(H61), C65(H65), C66(H66), C67(H67),
  C68(H68), C71(H71), C72(H72), C73(H73), C74(H74)
6.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C8A(H8AA,H8AB,
 H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10C,H10D,H10E), C8B(H8BA,H8BB,H8BC),
 C9B(H9BA,H9BB,H9BC), C10B(H10F,H10G,H10H)
;
_atom_sites_solution_hydrogens   mixed
_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 0.65389(11) 0.38895(5) 0.50310(8) 0.0447(4) Uani 1 1 d . . . . .
Ni2 Ni 0.59875(10) 0.28853(4) 0.44305(8) 0.0414(4) Uani 1 1 d . . . . .
Ni3 Ni 0.49578(12) 0.41595(5) 0.20519(8) 0.0516(4) Uani 1 1 d . . . . .
Ni4 Ni 0.32050(11) 0.35121(5) 0.24734(8) 0.0462(4) Uani 1 1 d . . . . .
O1 O 0.6710(4) 0.32867(18) 0.5269(3) 0.0441(13) Uani 1 1 d . . . . .
O2 O 0.6293(4) 0.38670(19) 0.3807(3) 0.0465(14) Uani 1 1 d . . . . .
O3 O 0.6312(4) 0.31952(18) 0.3544(3) 0.0450(14) Uani 1 1 d . . . . .
O4 O 0.5585(5) 0.36261(18) 0.2542(3) 0.0469(14) Uani 1 1 d . . . . .
O5 O 0.5155(4) 0.38118(19) 0.4734(3) 0.0468(14) Uani 1 1 d . . . . .
O6 O 0.4822(4) 0.32104(18) 0.4059(3) 0.0413(13) Uani 1 1 d . . . . .
O7 O 0.3973(4) 0.37620(19) 0.3579(3) 0.0476(14) Uani 1 1 d . . . . .
O8 O 0.3662(5) 0.3915(2) 0.1782(4) 0.0526(16) Uani 1 1 d . . . . .
O9 O 0.4901(5) 0.4352(2) 0.3164(3) 0.0537(16) Uani 1 1 d . . . . .
H9A H 0.535736 0.426469 0.355944 0.081 Uiso 1 1 d R U . . .
H9B H 0.446136 0.423705 0.323547 0.081 Uiso 1 1 d R U . . .
O10 O 0.4207(4) 0.31248(18) 0.2449(3) 0.0439(13) Uani 1 1 d . . . . .
H10A H 0.450615 0.303797 0.293212 0.066 Uiso 1 1 d R U . . .
H10B H 0.458501 0.325946 0.231428 0.066 Uiso 1 1 d R U . . .
N1 N 0.6866(6) 0.4013(3) 0.6282(5) 0.0526(19) Uani 1 1 d . . . . .
N2 N 0.6382(6) 0.4527(3) 0.5035(4) 0.0507(19) Uani 1 1 d . . . . .
N3 N 0.7905(6) 0.3934(2) 0.5364(4) 0.0519(19) Uani 1 1 d . . . . .
N4 N 0.7062(5) 0.2471(2) 0.4750(4) 0.0464(17) Uani 1 1 d . . . . .
N5 N 0.5748(5) 0.2580(2) 0.5352(4) 0.0441(16) Uani 1 1 d . . . . .
N6 N 0.5416(5) 0.2394(2) 0.3620(4) 0.0424(16) Uani 1 1 d . . . . .
N7 N 0.4470(7) 0.4730(3) 0.1531(5) 0.058(2) Uani 1 1 d . . . . .
N8 N 0.4812(6) 0.4022(3) 0.0860(5) 0.055(2) Uani 1 1 d . . . . .
N9 N 0.6135(6) 0.4498(3) 0.2347(5) 0.062(2) Uani 1 1 d . . . . .
N10 N 0.2309(5) 0.3228(2) 0.1402(4) 0.0493(18) Uani 1 1 d . . . . .
N11 N 0.2741(5) 0.3020(3) 0.2971(5) 0.0497(18) Uani 1 1 d . . . . .
N12 N 0.2155(6) 0.3903(3) 0.2270(5) 0.057(2) Uani 1 1 d . . . . .
C1 C 0.7371(7) 0.3156(3) 0.5959(5) 0.052(2) Uani 1 1 d . . . . .
C2 C 0.7452(7) 0.3311(3) 0.6746(5) 0.052(2) Uani 1 1 d . . . . .
C3 C 0.8140(8) 0.3171(4) 0.7455(6) 0.065(3) Uani 1 1 d . . . . .
H3 H 0.819769 0.328810 0.796768 0.078 Uiso 1 1 calc R U . . .
C4 C 0.8723(8) 0.2877(4) 0.7440(6) 0.061(3) Uani 1 1 d . . . . .
C5 C 0.8669(7) 0.2735(3) 0.6670(6) 0.060(3) Uani 1 1 d . . . . .
H5 H 0.910214 0.254494 0.664045 0.072 Uiso 1 1 calc R U . . .
C6 C 0.8005(6) 0.2863(3) 0.5953(5) 0.048(2) Uani 1 1 d . . . . .
C7 C 0.9491(7) 0.2737(3) 0.8221(6) 0.069(2) Uani 1 1 d D . . . .
C11 C 0.6785(8) 0.3636(3) 0.6746(5) 0.058(3) Uani 1 1 d . . . . .
H11A H 0.617320 0.352359 0.649127 0.069 Uiso 1 1 calc R U . . .
H11B H 0.688403 0.371286 0.731824 0.069 Uiso 1 1 calc R U . . .
C12 C 0.6223(9) 0.4335(3) 0.6302(6) 0.063(3) Uani 1 1 d . . . . .
H12A H 0.640704 0.445284 0.685981 0.076 Uiso 1 1 calc R U . . .
H12B H 0.561945 0.421495 0.615464 0.076 Uiso 1 1 calc R U . . .
C13 C 0.6206(7) 0.4666(3) 0.5697(6) 0.057(2) Uani 1 1 d . . . . .
C14 C 0.6056(9) 0.5071(4) 0.5803(7) 0.073(3) Uani 1 1 d . . . . .
H14 H 0.591062 0.515415 0.625580 0.088 Uiso 1 1 calc R U . . .
C15 C 0.6116(8) 0.5358(4) 0.5249(7) 0.070(3) Uani 1 1 d . . . . .
H15 H 0.602297 0.564126 0.531870 0.084 Uiso 1 1 calc R U . . .
C16 C 0.6314(8) 0.5225(4) 0.4597(6) 0.068(3) Uani 1 1 d . . . . .
H16 H 0.635879 0.541658 0.420663 0.082 Uiso 1 1 calc R U . . .
C17 C 0.6449(8) 0.4813(3) 0.4506(6) 0.058(3) Uani 1 1 d . . . . .
H17 H 0.659436 0.472719 0.405424 0.070 Uiso 1 1 calc R U . . .
C18 C 0.7810(7) 0.4161(3) 0.6630(5) 0.052(2) Uani 1 1 d . . . . .
H18A H 0.807886 0.408430 0.721630 0.063 Uiso 1 1 calc R U . . .
H18B H 0.781531 0.446415 0.659386 0.063 Uiso 1 1 calc R U . . .
C19 C 0.8371(7) 0.3983(3) 0.6183(5) 0.054(2) Uani 1 1 d . . . . .
C20 C 0.9252(7) 0.3897(4) 0.6544(6) 0.061(3) Uani 1 1 d . . . . .
H20 H 0.954550 0.393262 0.711917 0.073 Uiso 1 1 calc R U . . .
C21 C 0.9735(9) 0.3755(4) 0.6082(7) 0.072(3) Uani 1 1 d . . . . .
H21 H 1.035303 0.369176 0.632795 0.087 Uiso 1 1 calc R U . . .
C22 C 0.9261(7) 0.3711(4) 0.5234(7) 0.066(3) Uani 1 1 d . . . . .
H22 H 0.955594 0.361953 0.488769 0.079 Uiso 1 1 calc R U . . .
C23 C 0.8377(7) 0.3802(3) 0.4916(6) 0.056(2) Uani 1 1 d . . . . .
H23 H 0.806892 0.377167 0.434128 0.067 Uiso 1 1 calc R U . . .
C24 C 0.7928(6) 0.2692(3) 0.5133(5) 0.047(2) Uani 1 1 d . . . . .
H24A H 0.796261 0.291843 0.477033 0.057 Uiso 1 1 calc R U . . .
H24B H 0.842882 0.250101 0.520591 0.057 Uiso 1 1 calc R U . . .
C25 C 0.6946(7) 0.2153(3) 0.5314(6) 0.049(2) Uani 1 1 d . . . . .
H25A H 0.753912 0.207528 0.572041 0.058 Uiso 1 1 calc R U . . .
H25B H 0.667138 0.190495 0.499482 0.058 Uiso 1 1 calc R U . . .
C26 C 0.6370(7) 0.2305(3) 0.5757(5) 0.050(2) Uani 1 1 d . . . . .
C27 C 0.6434(8) 0.2151(3) 0.6507(5) 0.055(2) Uani 1 1 d . . . . .
H27 H 0.688521 0.195641 0.677793 0.066 Uiso 1 1 calc R U . . .
C28 C 0.5863(9) 0.2273(3) 0.6866(6) 0.064(3) Uani 1 1 d . . . . .
H28 H 0.592023 0.217525 0.739185 0.077 Uiso 1 1 calc R U . . .
C29 C 0.5174(8) 0.2555(3) 0.6424(5) 0.053(2) Uani 1 1 d . . . . .
H29 H 0.473669 0.263680 0.663440 0.064 Uiso 1 1 calc R U . . .
C30 C 0.5159(7) 0.2704(3) 0.5688(5) 0.047(2) Uani 1 1 d . . . . .
H30 H 0.471806 0.290070 0.540441 0.056 Uiso 1 1 calc R U . . .
C31 C 0.6984(7) 0.2276(3) 0.3952(6) 0.055(2) Uani 1 1 d . . . . .
H31A H 0.714102 0.247644 0.360399 0.065 Uiso 1 1 calc R U . . .
H31B H 0.739460 0.203871 0.405256 0.065 Uiso 1 1 calc R U . . .
C32 C 0.6039(7) 0.2137(3) 0.3533(5) 0.047(2) Uani 1 1 d . . . . .
C33 C 0.5810(7) 0.1768(3) 0.3130(6) 0.052(2) Uani 1 1 d . . . . .
H33 H 0.626300 0.158962 0.310199 0.063 Uiso 1 1 calc R U . . .
C34 C 0.4926(7) 0.1655(3) 0.2767(6) 0.052(2) Uani 1 1 d . . . . .
H34 H 0.476153 0.140607 0.246802 0.062 Uiso 1 1 calc R U . . .
C35 C 0.4289(7) 0.1910(3) 0.2847(5) 0.049(2) Uani 1 1 d . . . . .
H35 H 0.367328 0.184148 0.260958 0.059 Uiso 1 1 calc R U . . .
C36 C 0.4569(6) 0.2275(3) 0.3286(5) 0.0427(19) Uani 1 1 d . . . . .
H36 H 0.412646 0.244818 0.335080 0.051 Uiso 1 1 calc R U . . .
C37 C 0.4678(6) 0.3593(3) 0.4141(4) 0.0407(19) Uani 1 1 d . . . . .
C38 C 0.6083(7) 0.3556(3) 0.3318(5) 0.045(2) Uani 1 1 d . . . . .
C39 C 0.3042(7) 0.4051(3) 0.1074(5) 0.052(2) Uani 1 1 d . . . . .
C40 C 0.2926(8) 0.4469(3) 0.0891(6) 0.059(3) Uani 1 1 d . . . . .
C41 C 0.2303(8) 0.4602(3) 0.0135(6) 0.061(3) Uani 1 1 d . . . . .
H41 H 0.223020 0.488785 0.002595 0.073 Uiso 1 1 calc R U . . .
C42 C 0.1793(7) 0.4330(3) -0.0454(6) 0.053(2) Uani 1 1 d . . . . .
C43 C 0.1892(6) 0.3913(3) -0.0255(6) 0.051(2) Uani 1 1 d . . . . .
H43 H 0.153837 0.372020 -0.064691 0.062 Uiso 1 1 calc R U . . .
C44 C 0.2489(7) 0.3771(3) 0.0493(6) 0.053(2) Uani 1 1 d . . . . .
C45 C 0.1125(8) 0.4476(3) -0.1287(6) 0.057(2) Uani 1 1 d . . . . .
C46 C 0.1312(7) 0.4244(4) -0.1987(6) 0.056(2) Uani 1 1 d . . . . .
H46A H 0.194142 0.427739 -0.191094 0.084 Uiso 1 1 calc R U . . .
H46B H 0.093362 0.435792 -0.251930 0.084 Uiso 1 1 calc R U . . .
H46C H 0.117824 0.395174 -0.196764 0.084 Uiso 1 1 calc R U . . .
C47 C 0.0170(8) 0.4398(4) -0.1353(7) 0.063(3) Uani 1 1 d . . . . .
H47A H 0.006425 0.410209 -0.135446 0.095 Uiso 1 1 calc R U . . .
H47B H -0.024763 0.451926 -0.186205 0.095 Uiso 1 1 calc R U . . .
H47C H 0.007780 0.452393 -0.088324 0.095 Uiso 1 1 calc R U . . .
C48 C 0.1254(9) 0.4933(3) -0.1425(6) 0.070(3) Uani 1 1 d . . . . .
H48A H 0.108502 0.509737 -0.103898 0.106 Uiso 1 1 calc R U . . .
H48B H 0.087784 0.500804 -0.198784 0.106 Uiso 1 1 calc R U . . .
H48C H 0.188176 0.498390 -0.133541 0.106 Uiso 1 1 calc R U . . .
C49 C 0.3556(8) 0.4776(3) 0.1491(6) 0.063(3) Uani 1 1 d . . . . .
H49A H 0.334684 0.505852 0.131514 0.076 Uiso 1 1 calc R U . . .
H49B H 0.354206 0.473262 0.204369 0.076 Uiso 1 1 calc R U . . .
C50 C 0.4534(10) 0.4750(4) 0.0711(6) 0.071(3) Uani 1 1 d . . . . .
H50A H 0.511380 0.487252 0.076409 0.085 Uiso 1 1 calc R U . . .
H50B H 0.405330 0.492842 0.034673 0.085 Uiso 1 1 calc R U . . .
C51 C 0.4454(8) 0.4329(3) 0.0330(6) 0.061(3) Uani 1 1 d . . . . .
C52 C 0.4065(8) 0.4260(4) -0.0512(6) 0.061(3) Uani 1 1 d . . . . .
H52 H 0.381215 0.448133 -0.087776 0.073 Uiso 1 1 calc R U . . .
C53 C 0.4052(8) 0.3869(3) -0.0808(5) 0.062(3) Uani 1 1 d . . . . .
H53 H 0.379102 0.381645 -0.138038 0.074 Uiso 1 1 calc R U . . .
C54 C 0.4422(8) 0.3554(4) -0.0262(6) 0.064(3) Uani 1 1 d . . . . .
H54 H 0.441166 0.327988 -0.045024 0.077 Uiso 1 1 calc R U . . .
C55 C 0.4809(7) 0.3645(3) 0.0565(5) 0.056(2) Uani 1 1 d . . . . .
H55 H 0.508493 0.343023 0.093871 0.067 Uiso 1 1 calc R U . . .
C56 C 0.5065(9) 0.5040(3) 0.2082(6) 0.071(3) Uani 1 1 d . . . . .
H56A H 0.490089 0.507967 0.256641 0.085 Uiso 1 1 calc R U . . .
H56B H 0.499262 0.530556 0.179092 0.085 Uiso 1 1 calc R U . . .
C57 C 0.6018(8) 0.4902(4) 0.2354(6) 0.064(3) Uani 1 1 d . . . . .
C58 C 0.6740(11) 0.5175(4) 0.2650(7) 0.083(4) Uani 1 1 d . . . . .
H58 H 0.665076 0.546329 0.265260 0.100 Uiso 1 1 calc R U . . .
C59 C 0.7582(10) 0.5008(6) 0.2936(8) 0.092(5) Uani 1 1 d . . . . .
H59 H 0.808775 0.518178 0.316277 0.110 Uiso 1 1 calc R U . . .
C60 C 0.7699(10) 0.4600(5) 0.2897(7) 0.081(4) Uani 1 1 d . . . . .
H60 H 0.828535 0.448954 0.307175 0.097 Uiso 1 1 calc R U . . .
C61 C 0.6978(7) 0.4346(4) 0.2608(6) 0.067(3) Uani 1 1 d . . . . .
H61 H 0.706649 0.405849 0.258884 0.080 Uiso 1 1 calc R U . . .
C62 C 0.2558(7) 0.3320(3) 0.0691(5) 0.051(2) Uani 1 1 d . . . . .
H62A H 0.216060 0.316600 0.020692 0.062 Uiso 1 1 calc R U . . .
H62B H 0.317779 0.322768 0.081090 0.062 Uiso 1 1 calc R U . . .
C63 C 0.2358(7) 0.2789(3) 0.1567(6) 0.052(2) Uani 1 1 d . . . . .
H63A H 0.288576 0.267271 0.148677 0.063 Uiso 1 1 calc R U . . .
H63B H 0.181868 0.265288 0.117663 0.063 Uiso 1 1 calc R U . . .
C64 C 0.2426(7) 0.2705(3) 0.2441(5) 0.048(2) Uani 1 1 d . . . . .
C65 C 0.2212(7) 0.2331(4) 0.2687(6) 0.057(2) Uani 1 1 d . . . . .
H65 H 0.197015 0.211744 0.230014 0.069 Uiso 1 1 calc R U . . .
C66 C 0.2357(8) 0.2272(4) 0.3521(7) 0.062(3) Uani 1 1 d . . . . .
H66 H 0.223283 0.201487 0.371134 0.074 Uiso 1 1 calc R U . . .
C67 C 0.2679(7) 0.2591(4) 0.4043(6) 0.063(3) Uani 1 1 d . . . . .
H67 H 0.278208 0.255729 0.460864 0.075 Uiso 1 1 calc R U . . .
C68 C 0.2857(6) 0.2962(4) 0.3765(6) 0.056(2) Uani 1 1 d . . . . .
H68 H 0.306576 0.318365 0.414011 0.067 Uiso 1 1 calc R U . . .
C69 C 0.1396(7) 0.3389(3) 0.1263(6) 0.056(2) Uani 1 1 d . . . . .
H69A H 0.110973 0.321188 0.155248 0.068 Uiso 1 1 calc R U . . .
H69B H 0.102597 0.338042 0.067020 0.068 Uiso 1 1 calc R U . . .
C70 C 0.1441(7) 0.3821(4) 0.1569(7) 0.067(3) Uani 1 1 d . . . . .
C71 C 0.0819(10) 0.4123(4) 0.1187(8) 0.091(5) Uani 1 1 d . . . . .
H71 H 0.033524 0.405905 0.069299 0.109 Uiso 1 1 calc R U . . .
C72 C 0.0882(11) 0.4503(5) 0.1497(10) 0.099(5) Uani 1 1 d . . . . .
H72 H 0.044112 0.470405 0.123507 0.119 Uiso 1 1 calc R U . . .
C73 C 0.1612(10) 0.4598(5) 0.2219(10) 0.091(4) Uani 1 1 d . . . . .
H73 H 0.170199 0.486823 0.243891 0.109 Uiso 1 1 calc R U . . .
C74 C 0.2206(9) 0.4277(4) 0.2601(8) 0.082(4) Uani 1 1 d . . . . .
H74 H 0.266487 0.432763 0.311969 0.099 Uiso 1 1 calc R U . . .
C8A C 0.9134(10) 0.2573(6) 0.8830(9) 0.090(5) Uani 0.724(17) 1 d D . P A 1
H8AA H 0.876330 0.278251 0.894900 0.135 Uiso 0.724(17) 1 calc R U P A 1
H8AB H 0.963145 0.250020 0.933583 0.135 Uiso 0.724(17) 1 calc R U P A 1
H8AC H 0.877185 0.232850 0.860412 0.135 Uiso 0.724(17) 1 calc R U P A 1
C9A C 1.0057(11) 0.2381(5) 0.8033(9) 0.079(4) Uani 0.724(17) 1 d D . P A 1
H9AA H 0.965374 0.216435 0.771552 0.118 Uiso 0.724(17) 1 calc R U P A 1
H9AB H 1.047114 0.226585 0.855094 0.118 Uiso 0.724(17) 1 calc R U P A 1
H9AC H 1.039527 0.249107 0.771821 0.118 Uiso 0.724(17) 1 calc R U P A 1
C10A C 1.0155(9) 0.3087(5) 0.8561(9) 0.073(4) Uani 0.724(17) 1 d D . P A 1
H10C H 1.039816 0.316982 0.814976 0.110 Uiso 0.724(17) 1 calc R U P A 1
H10D H 1.064160 0.299464 0.905824 0.110 Uiso 0.724(17) 1 calc R U P A 1
H10E H 0.985095 0.332111 0.869261 0.110 Uiso 0.724(17) 1 calc R U P A 1
C8B C 0.918(2) 0.2312(8) 0.839(2) 0.070(7) Uani 0.276(17) 1 d D . P A 2
H8BA H 0.858277 0.233377 0.840604 0.104 Uiso 0.276(17) 1 calc R U P A 2
H8BB H 0.959808 0.220916 0.891866 0.104 Uiso 0.276(17) 1 calc R U P A 2
H8BC H 0.916767 0.212133 0.795381 0.104 Uiso 0.276(17) 1 calc R U P A 2
C9B C 1.0436(17) 0.2713(13) 0.826(3) 0.090(10) Uani 0.276(17) 1 d D . P A 2
H9BA H 1.047567 0.250476 0.787116 0.135 Uiso 0.276(17) 1 calc R U P A 2
H9BB H 1.083325 0.263693 0.881605 0.135 Uiso 0.276(17) 1 calc R U P A 2
H9BC H 1.061660 0.297996 0.811666 0.135 Uiso 0.276(17) 1 calc R U P A 2
C10B C 0.950(2) 0.3007(11) 0.8969(17) 0.075(8) Uani 0.276(17) 1 d D . P A 2
H10F H 0.970965 0.328402 0.891607 0.112 Uiso 0.276(17) 1 calc R U P A 2
H10G H 0.990673 0.288241 0.948040 0.112 Uiso 0.276(17) 1 calc R U P A 2
H10H H 0.889874 0.302071 0.897524 0.112 Uiso 0.276(17) 1 calc R U P A 2
S2A S 0.2308(12) 0.3497(5) 0.5912(9) 0.109(6) Uani 0.274(9) 1 d D . P B 2
S2B S 0.2319(3) 0.37937(12) 0.6367(2) 0.0532(11) Uani 0.726(9) 1 d D U P B 1
F4A F 0.140(3) 0.3588(12) 0.4366(16) 0.161(12) Uani 0.274(9) 1 d D . P B 2
F4B F 0.2642(13) 0.3712(4) 0.5045(8) 0.151(5) Uani 0.726(9) 1 d D U P B 1
F5A F 0.237(2) 0.4050(11) 0.488(2) 0.150(11) Uani 0.274(9) 1 d D . P B 2
F5B F 0.1567(11) 0.3358(5) 0.5091(10) 0.163(5) Uani 0.726(9) 1 d D U P B 1
F6A F 0.116(2) 0.4040(11) 0.511(2) 0.148(11) Uani 0.274(9) 1 d D . P B 2
F6B F 0.2883(13) 0.3166(5) 0.5761(9) 0.121(5) Uani 0.726(9) 1 d D U P B 1
O14A O 0.158(2) 0.3254(10) 0.594(3) 0.131(12) Uani 0.274(9) 1 d D . P B 2
O14B O 0.3249(7) 0.3903(4) 0.6783(10) 0.099(4) Uani 0.726(9) 1 d D U P B 1
O15A O 0.268(3) 0.3777(11) 0.6574(18) 0.120(14) Uani 0.274(9) 1 d D . P B 2
O15B O 0.2045(10) 0.3515(4) 0.6849(9) 0.100(4) Uani 0.726(9) 1 d D U P B 1
O16A O 0.296(3) 0.3263(10) 0.571(3) 0.095(11) Uani 0.274(9) 1 d D . P B 2
O16B O 0.1727(7) 0.4126(3) 0.6012(6) 0.067(3) Uani 0.726(9) 1 d D U P B 1
C76A C 0.1786(18) 0.3811(8) 0.5019(16) 0.121(9) Uani 0.274(9) 1 d D . P B 2
C76B C 0.2366(10) 0.3491(4) 0.5529(8) 0.106(4) Uani 0.726(9) 1 d D U P B 1
S1A S 0.7092(7) 0.0881(3) 0.4290(6) 0.045(3) Uani 0.201(8) 1 d D . P C 2
F1A F 0.876(2) 0.0765(12) 0.4992(15) 0.053(6) Uani 0.201(8) 1 d D . P C 2
F2A F 0.8414(19) 0.1060(7) 0.3849(16) 0.061(5) Uani 0.201(8) 1 d D . P C 2
F3A F 0.8186(17) 0.0414(7) 0.3882(16) 0.056(5) Uani 0.201(8) 1 d D . P C 2
O11A O 0.6461(19) 0.0834(8) 0.3465(13) 0.046(6) Uani 0.201(8) 1 d D . P C 2
O12A O 0.729(3) 0.1296(6) 0.460(2) 0.060(7) Uani 0.201(8) 1 d D . P C 2
O13A O 0.698(3) 0.0604(12) 0.490(2) 0.048(7) Uani 0.201(8) 1 d D . P C 2
C75A C 0.8157(19) 0.0766(7) 0.4238(14) 0.049(5) Uani 0.201(8) 1 d D . P C 2
S1 S 0.7867(4) 0.09343(13) 0.4380(3) 0.1012(19) Uani 0.799(8) 1 d D U P C 1
F1B F 0.7622(16) 0.1099(5) 0.5759(11) 0.197(6) Uani 0.799(8) 1 d D U P C 1
F2B F 0.6979(13) 0.0555(4) 0.5146(11) 0.133(5) Uani 0.799(8) 1 d D U P C 1
F3B F 0.6477(13) 0.1147(5) 0.4709(13) 0.187(6) Uani 0.799(8) 1 d D U P C 1
O11B O 0.7287(13) 0.0766(5) 0.3613(8) 0.131(5) Uani 0.799(8) 1 d D U P C 1
O12B O 0.8627(14) 0.0695(6) 0.4890(13) 0.128(6) Uani 0.799(8) 1 d D U P C 1
O13B O 0.7997(13) 0.1365(3) 0.4307(12) 0.136(5) Uani 0.799(8) 1 d D U P C 1
C75B C 0.7222(13) 0.0930(4) 0.5024(12) 0.134(4) Uani 0.799(8) 1 d D U P C 1


_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 2.005(6) . ?
Ni1 O2 2.037(6) . ?
Ni1 O5 2.111(7) . ?
Ni1 N1 2.100(7) . ?
Ni1 N2 2.094(8) . ?
Ni1 N3 2.064(9) . ?
Ni2 O1 1.990(6) . ?
Ni2 O3 2.081(6) . ?
Ni2 O6 2.042(6) . ?
Ni2 N4 2.102(8) . ?
Ni2 N5 2.057(7) . ?
Ni2 N6 2.111(8) . ?
Ni3 O4 2.033(6) . ?
Ni3 O8 2.119(7) . ?
Ni3 O9 2.088(6) . ?
Ni3 N7 2.093(9) . ?
Ni3 N8 2.067(8) . ?
Ni3 N9 2.089(9) . ?
Ni4 O7 2.044(6) . ?
Ni4 O8 2.102(7) . ?
Ni4 O10 2.064(6) . ?
Ni4 N10 2.113(7) . ?
Ni4 N11 2.094(8) . ?
Ni4 N12 2.042(9) . ?
O1 C1 1.351(11) . ?
O2 C38 1.289(10) . ?
O3 C38 1.253(11) . ?
O4 C38 1.318(11) . ?
O5 C37 1.261(10) . ?
O6 C37 1.284(11) . ?
O7 C37 1.318(11) . ?
O8 C39 1.349(11) . ?
O9 H9A 0.8517 . ?
O9 H9B 0.8515 . ?
O10 H10A 0.8540 . ?
O10 H10B 0.8538 . ?
N1 C11 1.504(13) . ?
N1 C12 1.486(14) . ?
N1 C18 1.495(13) . ?
N2 C13 1.371(12) . ?
N2 C17 1.348(13) . ?
N3 C19 1.363(12) . ?
N3 C23 1.352(13) . ?
N4 C24 1.492(11) . ?
N4 C25 1.493(12) . ?
N4 C31 1.501(12) . ?
N5 C26 1.336(13) . ?
N5 C30 1.354(12) . ?
N6 C32 1.359(12) . ?
N6 C36 1.330(12) . ?
N7 C49 1.457(16) . ?
N7 C50 1.485(13) . ?
N7 C56 1.477(13) . ?
N8 C51 1.341(13) . ?
N8 C55 1.331(14) . ?
N9 C57 1.329(15) . ?
N9 C61 1.356(15) . ?
N10 C62 1.479(12) . ?
N10 C63 1.456(13) . ?
N10 C69 1.495(13) . ?
N11 C64 1.350(12) . ?
N11 C68 1.349(12) . ?
N12 C70 1.363(14) . ?
N12 C74 1.339(14) . ?
C1 C2 1.432(12) . ?
C1 C6 1.403(15) . ?
C2 C3 1.400(15) . ?
C2 C11 1.510(16) . ?
C3 H3 0.9500 . ?
C3 C4 1.351(18) . ?
C4 C5 1.402(16) . ?
C4 C7 1.535(14) . ?
C5 H5 0.9500 . ?
C5 C6 1.378(14) . ?
C6 C24 1.505(13) . ?
C7 C8A 1.491(13) . ?
C7 C9A 1.587(15) . ?
C7 C10A 1.525(14) . ?
C7 C8B 1.540(18) . ?
C7 C9B 1.505(18) . ?
C7 C10B 1.574(18) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.507(16) . ?
C13 C14 1.367(15) . ?
C14 H14 0.9500 . ?
C14 C15 1.379(19) . ?
C15 H15 0.9500 . ?
C15 C16 1.371(17) . ?
C16 H16 0.9500 . ?
C16 C17 1.378(15) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.517(15) . ?
C19 C20 1.353(15) . ?
C20 H20 0.9500 . ?
C20 C21 1.398(17) . ?
C21 H21 0.9500 . ?
C21 C22 1.405(16) . ?
C22 H22 0.9500 . ?
C22 C23 1.358(15) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.501(14) . ?
C26 C27 1.378(12) . ?
C27 H27 0.9500 . ?
C27 C28 1.354(16) . ?
C28 H28 0.9500 . ?
C28 C29 1.426(17) . ?
C29 H29 0.9500 . ?
C29 C30 1.372(12) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.494(15) . ?
C32 C33 1.375(14) . ?
C33 H33 0.9500 . ?
C33 C34 1.378(15) . ?
C34 H34 0.9500 . ?
C34 C35 1.369(14) . ?
C35 H35 0.9500 . ?
C35 C36 1.396(13) . ?
C36 H36 0.9500 . ?
C39 C40 1.394(14) . ?
C39 C44 1.411(13) . ?
C40 C41 1.402(14) . ?
C40 C49 1.532(14) . ?
C41 H41 0.9500 . ?
C41 C42 1.377(14) . ?
C42 C43 1.395(14) . ?
C42 C45 1.536(13) . ?
C43 H43 0.9500 . ?
C43 C44 1.389(13) . ?
C44 C62 1.503(14) . ?
C45 C46 1.565(14) . ?
C45 C47 1.525(16) . ?
C45 C48 1.532(15) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.510(16) . ?
C51 C52 1.394(13) . ?
C52 H52 0.9500 . ?
C52 C53 1.372(16) . ?
C53 H53 0.9500 . ?
C53 C54 1.381(16) . ?
C54 H54 0.9500 . ?
C54 C55 1.384(14) . ?
C55 H55 0.9500 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.500(19) . ?
C57 C58 1.405(17) . ?
C58 H58 0.9500 . ?
C58 C59 1.37(2) . ?
C59 H59 0.9500 . ?
C59 C60 1.35(2) . ?
C60 H60 0.9500 . ?
C60 C61 1.363(17) . ?
C61 H61 0.9500 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.522(13) . ?
C64 C65 1.379(15) . ?
C65 H65 0.9500 . ?
C65 C66 1.408(15) . ?
C66 H66 0.9500 . ?
C66 C67 1.356(17) . ?
C67 H67 0.9500 . ?
C67 C68 1.375(16) . ?
C68 H68 0.9500 . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C69 C70 1.499(16) . ?
C70 C71 1.387(17) . ?
C71 H71 0.9500 . ?
C71 C72 1.341(19) . ?
C72 H72 0.9500 . ?
C72 C73 1.41(2) . ?
C73 H73 0.9500 . ?
C73 C74 1.410(19) . ?
C74 H74 0.9500 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C10A H10C 0.9800 . ?
C10A H10D 0.9800 . ?
C10A H10E 0.9800 . ?
C8B H8BA 0.9800 . ?
C8B H8BB 0.9800 . ?
C8B H8BC 0.9800 . ?
C9B H9BA 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?
C10B H10F 0.9800 . ?
C10B H10G 0.9800 . ?
C10B H10H 0.9800 . ?
S2A O14A 1.436(15) . ?
S2A O15A 1.422(16) . ?
S2A O16A 1.442(15) . ?
S2A C76A 1.80(2) . ?
S2B O14B 1.448(10) . ?
S2B O15B 1.421(9) . ?
S2B O16B 1.425(9) . ?
S2B C76B 1.797(13) . ?
F4A C76A 1.304(16) . ?
F4B C76B 1.313(12) . ?
F5A C76A 1.305(16) . ?
F5B C76B 1.305(12) . ?
F6A C76A 1.305(16) . ?
F6B C76B 1.315(12) . ?
S1A O11A 1.435(16) . ?
S1A O12A 1.449(16) . ?
S1A O13A 1.462(17) . ?
S1A C75A 1.80(3) . ?
F1A C75A 1.318(17) . ?
F2A C75A 1.329(17) . ?
F3A C75A 1.315(17) . ?
S1 O11B 1.433(12) . ?
S1 O12B 1.447(14) . ?
S1 O13B 1.433(11) . ?
S1 C75B 1.80(2) . ?
F1B C75B 1.330(13) . ?
F2B C75B 1.325(13) . ?
F3B C75B 1.326(13) . ?

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 O2 98.2(2) . . ?
O1 Ni1 O5 89.1(3) . . ?
O1 Ni1 N1 90.4(3) . . ?
O1 Ni1 N2 168.1(3) . . ?
O1 Ni1 N3 87.7(3) . . ?
O2 Ni1 O5 87.9(2) . . ?
O2 Ni1 N1 170.5(3) . . ?
O2 Ni1 N2 93.6(3) . . ?
O2 Ni1 N3 93.9(3) . . ?
N1 Ni1 O5 96.4(3) . . ?
N2 Ni1 O5 90.1(3) . . ?
N2 Ni1 N1 77.9(3) . . ?
N3 Ni1 O5 176.5(3) . . ?
N3 Ni1 N1 82.3(3) . . ?
N3 Ni1 N2 92.8(3) . . ?
O1 Ni2 O3 89.7(2) . . ?
O1 Ni2 O6 96.4(2) . . ?
O1 Ni2 N4 91.5(3) . . ?
O1 Ni2 N5 88.0(3) . . ?
O1 Ni2 N6 170.1(3) . . ?
O3 Ni2 N4 95.6(3) . . ?
O3 Ni2 N6 91.8(2) . . ?
O6 Ni2 O3 88.2(2) . . ?
O6 Ni2 N4 171.2(3) . . ?
O6 Ni2 N5 94.7(3) . . ?
O6 Ni2 N6 93.4(3) . . ?
N4 Ni2 N6 78.6(3) . . ?
N5 Ni2 O3 176.5(3) . . ?
N5 Ni2 N4 81.8(3) . . ?
N5 Ni2 N6 90.1(3) . . ?
O4 Ni3 O8 93.9(3) . . ?
O4 Ni3 O9 92.8(2) . . ?
O4 Ni3 N7 172.5(3) . . ?
O4 Ni3 N8 95.5(3) . . ?
O4 Ni3 N9 94.8(3) . . ?
O9 Ni3 O8 86.5(3) . . ?
O9 Ni3 N7 90.1(3) . . ?
O9 Ni3 N9 87.8(3) . . ?
N7 Ni3 O8 93.2(3) . . ?
N8 Ni3 O8 87.8(3) . . ?
N8 Ni3 O9 170.2(3) . . ?
N8 Ni3 N7 82.4(3) . . ?
N8 Ni3 N9 96.6(3) . . ?
N9 Ni3 O8 169.9(4) . . ?
N9 Ni3 N7 78.4(4) . . ?
O7 Ni4 O8 94.7(3) . . ?
O7 Ni4 O10 93.5(2) . . ?
O7 Ni4 N10 173.0(3) . . ?
O7 Ni4 N11 95.3(3) . . ?
O8 Ni4 N10 91.7(3) . . ?
O10 Ni4 O8 85.6(3) . . ?
O10 Ni4 N10 89.7(3) . . ?
O10 Ni4 N11 86.9(3) . . ?
N11 Ni4 O8 167.8(3) . . ?
N11 Ni4 N10 78.7(3) . . ?
N12 Ni4 O7 95.0(3) . . ?
N12 Ni4 O8 87.5(3) . . ?
N12 Ni4 O10 169.4(3) . . ?
N12 Ni4 N10 82.5(3) . . ?
N12 Ni4 N11 98.5(3) . . ?
Ni2 O1 Ni1 119.5(3) . . ?
C1 O1 Ni1 119.8(6) . . ?
C1 O1 Ni2 120.4(6) . . ?
C38 O2 Ni1 129.2(5) . . ?
C38 O3 Ni2 124.5(5) . . ?
C38 O4 Ni3 126.9(5) . . ?
C37 O5 Ni1 122.4(5) . . ?
C37 O6 Ni2 130.6(5) . . ?
C37 O7 Ni4 126.4(5) . . ?
Ni4 O8 Ni3 129.4(3) . . ?
C39 O8 Ni3 114.5(6) . . ?
C39 O8 Ni4 116.0(6) . . ?
Ni3 O9 H9A 109.6 . . ?
Ni3 O9 H9B 109.5 . . ?
H9A O9 H9B 104.3 . . ?
Ni4 O10 H10A 109.8 . . ?
Ni4 O10 H10B 109.8 . . ?
H10A O10 H10B 104.3 . . ?
C11 N1 Ni1 111.9(6) . . ?
C12 N1 Ni1 104.7(6) . . ?
C12 N1 C11 111.2(8) . . ?
C12 N1 C18 112.1(8) . . ?
C18 N1 Ni1 108.0(5) . . ?
C18 N1 C11 108.9(8) . . ?
C13 N2 Ni1 113.1(7) . . ?
C17 N2 Ni1 129.9(6) . . ?
C17 N2 C13 116.9(9) . . ?
C19 N3 Ni1 114.7(7) . . ?
C23 N3 Ni1 125.9(6) . . ?
C23 N3 C19 116.3(9) . . ?
C24 N4 Ni2 110.6(6) . . ?
C24 N4 C25 111.3(7) . . ?
C24 N4 C31 111.4(7) . . ?
C25 N4 Ni2 109.1(6) . . ?
C25 N4 C31 109.9(7) . . ?
C31 N4 Ni2 104.4(6) . . ?
C26 N5 Ni2 114.7(6) . . ?
C26 N5 C30 118.6(8) . . ?
C30 N5 Ni2 124.7(6) . . ?
C32 N6 Ni2 112.8(6) . . ?
C36 N6 Ni2 129.6(6) . . ?
C36 N6 C32 116.9(8) . . ?
C49 N7 Ni3 108.7(6) . . ?
C49 N7 C50 112.6(9) . . ?
C49 N7 C56 111.2(9) . . ?
C50 N7 Ni3 108.1(7) . . ?
C56 N7 Ni3 105.9(6) . . ?
C56 N7 C50 110.1(9) . . ?
C51 N8 Ni3 113.5(7) . . ?
C55 N8 Ni3 125.2(6) . . ?
C55 N8 C51 118.5(8) . . ?
C57 N9 Ni3 113.9(8) . . ?
C57 N9 C61 119.1(10) . . ?
C61 N9 Ni3 126.6(8) . . ?
C62 N10 Ni4 110.6(6) . . ?
C62 N10 C69 110.7(8) . . ?
C63 N10 Ni4 106.5(5) . . ?
C63 N10 C62 110.9(7) . . ?
C63 N10 C69 110.7(8) . . ?
C69 N10 Ni4 107.3(5) . . ?
C64 N11 Ni4 113.2(6) . . ?
C68 N11 Ni4 127.2(7) . . ?
C68 N11 C64 118.7(9) . . ?
C70 N12 Ni4 113.7(7) . . ?
C74 N12 Ni4 125.3(8) . . ?
C74 N12 C70 117.7(10) . . ?
O1 C1 C2 120.8(9) . . ?
O1 C1 C6 122.9(8) . . ?
C6 C1 C2 116.3(8) . . ?
C1 C2 C11 116.1(8) . . ?
C3 C2 C1 120.1(10) . . ?
C3 C2 C11 123.8(9) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 C2 122.7(10) . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C5 117.3(9) . . ?
C3 C4 C7 121.9(10) . . ?
C5 C4 C7 120.3(11) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 C4 122.0(11) . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C24 117.3(8) . . ?
C5 C6 C1 121.3(9) . . ?
C5 C6 C24 121.4(9) . . ?
C4 C7 C9A 111.5(10) . . ?
C4 C7 C8B 103.2(16) . . ?
C4 C7 C10B 109.6(16) . . ?
C8A C7 C4 110.4(9) . . ?
C8A C7 C9A 107.0(9) . . ?
C8A C7 C10A 113.0(9) . . ?
C10A C7 C4 110.1(9) . . ?
C10A C7 C9A 104.7(9) . . ?
C8B C7 C10B 104.1(14) . . ?
C9B C7 C4 122(2) . . ?
C9B C7 C8B 109.8(15) . . ?
C9B C7 C10B 107.2(15) . . ?
N1 C11 C2 111.4(8) . . ?
N1 C11 H11A 109.3 . . ?
N1 C11 H11B 109.3 . . ?
C2 C11 H11A 109.3 . . ?
C2 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
N1 C12 H12A 110.0 . . ?
N1 C12 H12B 110.0 . . ?
N1 C12 C13 108.5(8) . . ?
H12A C12 H12B 108.4 . . ?
C13 C12 H12A 110.0 . . ?
C13 C12 H12B 110.0 . . ?
N2 C13 C12 114.1(9) . . ?
C14 C13 N2 122.4(11) . . ?
C14 C13 C12 123.5(9) . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.8(11) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 120.8 . . ?
C16 C15 C14 118.3(10) . . ?
C16 C15 H15 120.8 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.1(12) . . ?
C17 C16 H16 120.0 . . ?
N2 C17 C16 122.4(10) . . ?
N2 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
N1 C18 H18A 109.1 . . ?
N1 C18 H18B 109.1 . . ?
N1 C18 C19 112.3(7) . . ?
H18A C18 H18B 107.9 . . ?
C19 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
N3 C19 C18 113.0(9) . . ?
C20 C19 N3 122.7(9) . . ?
C20 C19 C18 124.2(8) . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.8(10) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 121.7 . . ?
C20 C21 C22 116.6(11) . . ?
C22 C21 H21 121.7 . . ?
C21 C22 H22 120.4 . . ?
C23 C22 C21 119.2(11) . . ?
C23 C22 H22 120.4 . . ?
N3 C23 C22 124.3(9) . . ?
N3 C23 H23 117.9 . . ?
C22 C23 H23 117.9 . . ?
N4 C24 C6 109.9(7) . . ?
N4 C24 H24A 109.7 . . ?
N4 C24 H24B 109.7 . . ?
C6 C24 H24A 109.7 . . ?
C6 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
N4 C25 H25A 109.3 . . ?
N4 C25 H25B 109.3 . . ?
N4 C25 C26 111.8(8) . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
N5 C26 C25 115.7(8) . . ?
N5 C26 C27 121.7(10) . . ?
C27 C26 C25 122.4(9) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 C26 121.2(10) . . ?
C28 C27 H27 119.4 . . ?
C27 C28 H28 121.2 . . ?
C27 C28 C29 117.6(8) . . ?
C29 C28 H28 121.2 . . ?
C28 C29 H29 120.8 . . ?
C30 C29 C28 118.5(10) . . ?
C30 C29 H29 120.8 . . ?
N5 C30 C29 122.4(10) . . ?
N5 C30 H30 118.8 . . ?
C29 C30 H30 118.8 . . ?
N4 C31 H31A 110.2 . . ?
N4 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
C32 C31 N4 107.6(7) . . ?
C32 C31 H31A 110.2 . . ?
C32 C31 H31B 110.2 . . ?
N6 C32 C31 114.9(8) . . ?
N6 C32 C33 121.9(9) . . ?
C33 C32 C31 123.1(9) . . ?
C32 C33 H33 119.8 . . ?
C32 C33 C34 120.3(9) . . ?
C34 C33 H33 119.8 . . ?
C33 C34 H34 120.7 . . ?
C35 C34 C33 118.6(9) . . ?
C35 C34 H34 120.7 . . ?
C34 C35 H35 120.9 . . ?
C34 C35 C36 118.2(10) . . ?
C36 C35 H35 120.9 . . ?
N6 C36 C35 124.1(9) . . ?
N6 C36 H36 118.0 . . ?
C35 C36 H36 118.0 . . ?
O5 C37 O6 124.1(8) . . ?
O5 C37 O7 118.2(8) . . ?
O6 C37 O7 117.7(7) . . ?
O2 C38 O4 117.5(8) . . ?
O3 C38 O2 123.5(8) . . ?
O3 C38 O4 118.9(7) . . ?
O8 C39 C40 121.5(8) . . ?
O8 C39 C44 120.4(8) . . ?
C40 C39 C44 118.0(9) . . ?
C39 C40 C41 120.4(9) . . ?
C39 C40 C49 118.7(9) . . ?
C41 C40 C49 120.5(9) . . ?
C40 C41 H41 119.0 . . ?
C42 C41 C40 122.0(9) . . ?
C42 C41 H41 119.0 . . ?
C41 C42 C43 117.2(9) . . ?
C41 C42 C45 121.8(9) . . ?
C43 C42 C45 121.0(8) . . ?
C42 C43 H43 118.8 . . ?
C44 C43 C42 122.4(9) . . ?
C44 C43 H43 118.8 . . ?
C39 C44 C62 119.5(8) . . ?
C43 C44 C39 119.8(9) . . ?
C43 C44 C62 120.7(8) . . ?
C42 C45 C46 109.1(9) . . ?
C47 C45 C42 110.5(8) . . ?
C47 C45 C46 110.3(8) . . ?
C47 C45 C48 110.0(10) . . ?
C48 C45 C42 111.3(9) . . ?
C48 C45 C46 105.5(8) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N7 C49 C40 111.6(9) . . ?
N7 C49 H49A 109.3 . . ?
N7 C49 H49B 109.3 . . ?
C40 C49 H49A 109.3 . . ?
C40 C49 H49B 109.3 . . ?
H49A C49 H49B 108.0 . . ?
N7 C50 H50A 109.3 . . ?
N7 C50 H50B 109.3 . . ?
N7 C50 C51 111.5(8) . . ?
H50A C50 H50B 108.0 . . ?
C51 C50 H50A 109.3 . . ?
C51 C50 H50B 109.3 . . ?
N8 C51 C50 115.1(8) . . ?
N8 C51 C52 121.7(10) . . ?
C52 C51 C50 123.1(10) . . ?
C51 C52 H52 120.4 . . ?
C53 C52 C51 119.2(10) . . ?
C53 C52 H52 120.4 . . ?
C52 C53 H53 120.5 . . ?
C52 C53 C54 119.1(9) . . ?
C54 C53 H53 120.5 . . ?
C53 C54 H54 120.7 . . ?
C53 C54 C55 118.6(10) . . ?
C55 C54 H54 120.7 . . ?
N8 C55 C54 122.8(10) . . ?
N8 C55 H55 118.6 . . ?
C54 C55 H55 118.6 . . ?
N7 C56 H56A 109.6 . . ?
N7 C56 H56B 109.6 . . ?
N7 C56 C57 110.1(10) . . ?
H56A C56 H56B 108.2 . . ?
C57 C56 H56A 109.6 . . ?
C57 C56 H56B 109.6 . . ?
N9 C57 C56 115.3(9) . . ?
N9 C57 C58 122.0(12) . . ?
C58 C57 C56 122.6(12) . . ?
C57 C58 H58 121.4 . . ?
C59 C58 C57 117.1(14) . . ?
C59 C58 H58 121.4 . . ?
C58 C59 H59 119.6 . . ?
C60 C59 C58 120.7(13) . . ?
C60 C59 H59 119.6 . . ?
C59 C60 H60 119.9 . . ?
C59 C60 C61 120.1(15) . . ?
C61 C60 H60 119.9 . . ?
N9 C61 C60 120.9(14) . . ?
N9 C61 H61 119.5 . . ?
C60 C61 H61 119.5 . . ?
N10 C62 C44 111.9(8) . . ?
N10 C62 H62A 109.2 . . ?
N10 C62 H62B 109.2 . . ?
C44 C62 H62A 109.2 . . ?
C44 C62 H62B 109.2 . . ?
H62A C62 H62B 107.9 . . ?
N10 C63 H63A 109.5 . . ?
N10 C63 H63B 109.5 . . ?
N10 C63 C64 110.9(7) . . ?
H63A C63 H63B 108.1 . . ?
C64 C63 H63A 109.5 . . ?
C64 C63 H63B 109.5 . . ?
N11 C64 C63 115.3(8) . . ?
N11 C64 C65 121.8(8) . . ?
C65 C64 C63 122.9(9) . . ?
C64 C65 H65 120.5 . . ?
C64 C65 C66 119.0(10) . . ?
C66 C65 H65 120.5 . . ?
C65 C66 H66 120.9 . . ?
C67 C66 C65 118.2(10) . . ?
C67 C66 H66 120.9 . . ?
C66 C67 H67 119.6 . . ?
C66 C67 C68 120.8(10) . . ?
C68 C67 H67 119.6 . . ?
N11 C68 C67 121.5(10) . . ?
N11 C68 H68 119.2 . . ?
C67 C68 H68 119.2 . . ?
N10 C69 H69A 109.4 . . ?
N10 C69 H69B 109.4 . . ?
N10 C69 C70 111.0(8) . . ?
H69A C69 H69B 108.0 . . ?
C70 C69 H69A 109.4 . . ?
C70 C69 H69B 109.4 . . ?
N12 C70 C69 114.8(9) . . ?
N12 C70 C71 120.9(11) . . ?
C71 C70 C69 124.3(10) . . ?
C70 C71 H71 119.1 . . ?
C72 C71 C70 121.8(12) . . ?
C72 C71 H71 119.1 . . ?
C71 C72 H72 120.6 . . ?
C71 C72 C73 118.7(13) . . ?
C73 C72 H72 120.6 . . ?
C72 C73 H73 121.4 . . ?
C72 C73 C74 117.3(12) . . ?
C74 C73 H73 121.4 . . ?
N12 C74 C73 123.2(11) . . ?
N12 C74 H74 118.4 . . ?
C73 C74 H74 118.4 . . ?
C7 C8A H8AA 109.5 . . ?
C7 C8A H8AB 109.5 . . ?
C7 C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C7 C9A H9AA 109.5 . . ?
C7 C9A H9AB 109.5 . . ?
C7 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C7 C10A H10C 109.5 . . ?
C7 C10A H10D 109.5 . . ?
C7 C10A H10E 109.5 . . ?
H10C C10A H10D 109.5 . . ?
H10C C10A H10E 109.5 . . ?
H10D C10A H10E 109.5 . . ?
C7 C8B H8BA 109.5 . . ?
C7 C8B H8BB 109.5 . . ?
C7 C8B H8BC 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
C7 C9B H9BA 109.5 . . ?
C7 C9B H9BB 109.5 . . ?
C7 C9B H9BC 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
C7 C10B H10F 109.5 . . ?
C7 C10B H10G 109.5 . . ?
C7 C10B H10H 109.5 . . ?
H10F C10B H10G 109.5 . . ?
H10F C10B H10H 109.5 . . ?
H10G C10B H10H 109.5 . . ?
O14A S2A O16A 113.5(17) . . ?
O14A S2A C76A 102.9(15) . . ?
O15A S2A O14A 115.0(19) . . ?
O15A S2A O16A 114.8(19) . . ?
O15A S2A C76A 105.3(16) . . ?
O16A S2A C76A 103.4(16) . . ?
O14B S2B C76B 101.3(8) . . ?
O15B S2B O14B 110.6(9) . . ?
O15B S2B O16B 116.2(7) . . ?
O15B S2B C76B 104.8(7) . . ?
O16B S2B O14B 115.7(7) . . ?
O16B S2B C76B 106.5(6) . . ?
F4A C76A S2A 111.3(19) . . ?
F4A C76A F5A 108(2) . . ?
F4A C76A F6A 107(2) . . ?
F5A C76A S2A 111.3(18) . . ?
F5A C76A F6A 108(2) . . ?
F6A C76A S2A 110.6(18) . . ?
F4B C76B S2B 111.1(10) . . ?
F4B C76B F6B 108.2(13) . . ?
F5B C76B S2B 109.4(10) . . ?
F5B C76B F4B 107.5(14) . . ?
F5B C76B F6B 106.8(14) . . ?
F6B C76B S2B 113.8(10) . . ?
O11A S1A O12A 117.1(19) . . ?
O11A S1A O13A 116(2) . . ?
O11A S1A C75A 104.9(16) . . ?
O12A S1A O13A 112(3) . . ?
O12A S1A C75A 97.7(19) . . ?
O13A S1A C75A 107.0(18) . . ?
F1A C75A S1A 108(2) . . ?
F1A C75A F2A 105(2) . . ?
F2A C75A S1A 111(2) . . ?
F3A C75A S1A 114(2) . . ?
F3A C75A F1A 109(2) . . ?
F3A C75A F2A 108(2) . . ?
O11B S1 O12B 118.8(13) . . ?
O11B S1 C75B 105.1(11) . . ?
O12B S1 C75B 99.3(13) . . ?
O13B S1 O11B 110.9(10) . . ?
O13B S1 O12B 117.7(12) . . ?
O13B S1 C75B 101.7(11) . . ?
F1B C75B S1 115.0(16) . . ?
F2B C75B S1 112.6(14) . . ?
F2B C75B F1B 106.9(16) . . ?
F2B C75B F3B 106.5(16) . . ?
F3B C75B S1 112.3(15) . . ?
F3B C75B F1B 102.8(17) . . ?

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 C1 C2 53.4(11) . . . . ?
Ni1 O1 C1 C6 -127.0(8) . . . . ?
Ni1 O2 C38 O3 -28.5(13) . . . . ?
Ni1 O2 C38 O4 150.2(6) . . . . ?
Ni1 O5 C37 O6 57.5(10) . . . . ?
Ni1 O5 C37 O7 -124.5(7) . . . . ?
Ni1 N1 C11 C2 64.7(9) . . . . ?
Ni1 N1 C12 C13 -47.9(9) . . . . ?
Ni1 N1 C18 C19 -29.4(9) . . . . ?
Ni1 N2 C13 C12 3.7(11) . . . . ?
Ni1 N2 C13 C14 -178.1(9) . . . . ?
Ni1 N2 C17 C16 179.3(8) . . . . ?
Ni1 N3 C19 C18 -22.9(11) . . . . ?
Ni1 N3 C19 C20 159.8(9) . . . . ?
Ni1 N3 C23 C22 -157.7(9) . . . . ?
Ni2 O1 C1 C2 -133.1(8) . . . . ?
Ni2 O1 C1 C6 46.5(11) . . . . ?
Ni2 O3 C38 O2 59.0(12) . . . . ?
Ni2 O3 C38 O4 -119.7(7) . . . . ?
Ni2 O6 C37 O5 -30.6(11) . . . . ?
Ni2 O6 C37 O7 151.4(6) . . . . ?
Ni2 N4 C24 C6 67.6(8) . . . . ?
Ni2 N4 C25 C26 -23.7(9) . . . . ?
Ni2 N4 C31 C32 -49.3(8) . . . . ?
Ni2 N5 C26 C25 -20.9(10) . . . . ?
Ni2 N5 C26 C27 163.4(7) . . . . ?
Ni2 N5 C30 C29 -163.3(7) . . . . ?
Ni2 N6 C32 C31 -6.0(9) . . . . ?
Ni2 N6 C32 C33 170.4(7) . . . . ?
Ni2 N6 C36 C35 -170.8(6) . . . . ?
Ni3 O4 C38 O2 -9.4(12) . . . . ?
Ni3 O4 C38 O3 169.4(6) . . . . ?
Ni3 O8 C39 C40 -50.3(12) . . . . ?
Ni3 O8 C39 C44 129.6(9) . . . . ?
Ni3 N7 C49 C40 -66.5(9) . . . . ?
Ni3 N7 C50 C51 29.3(12) . . . . ?
Ni3 N7 C56 C57 41.7(9) . . . . ?
Ni3 N8 C51 C50 21.2(13) . . . . ?
Ni3 N8 C51 C52 -160.9(9) . . . . ?
Ni3 N8 C55 C54 157.5(9) . . . . ?
Ni3 N9 C57 C56 -4.9(11) . . . . ?
Ni3 N9 C57 C58 170.8(8) . . . . ?
Ni3 N9 C61 C60 -170.2(8) . . . . ?
Ni4 O7 C37 O5 169.5(5) . . . . ?
Ni4 O7 C37 O6 -12.3(11) . . . . ?
Ni4 O8 C39 C40 127.7(9) . . . . ?
Ni4 O8 C39 C44 -52.5(11) . . . . ?
Ni4 N10 C62 C44 -63.6(9) . . . . ?
Ni4 N10 C63 C64 39.7(9) . . . . ?
Ni4 N10 C69 C70 31.2(10) . . . . ?
Ni4 N11 C64 C63 -7.4(10) . . . . ?
Ni4 N11 C64 C65 170.4(8) . . . . ?
Ni4 N11 C68 C67 -166.8(8) . . . . ?
Ni4 N12 C70 C69 22.8(13) . . . . ?
Ni4 N12 C70 C71 -157.3(12) . . . . ?
Ni4 N12 C74 C73 152.0(13) . . . . ?
O1 C1 C2 C3 179.8(9) . . . . ?
O1 C1 C2 C11 -2.3(13) . . . . ?
O1 C1 C6 C5 -179.7(9) . . . . ?
O1 C1 C6 C24 -0.1(14) . . . . ?
O8 C39 C40 C41 177.2(10) . . . . ?
O8 C39 C40 C49 3.4(16) . . . . ?
O8 C39 C44 C43 -175.9(9) . . . . ?
O8 C39 C44 C62 3.7(15) . . . . ?
N1 C12 C13 N2 30.2(12) . . . . ?
N1 C12 C13 C14 -148.0(10) . . . . ?
N1 C18 C19 N3 35.4(12) . . . . ?
N1 C18 C19 C20 -147.4(10) . . . . ?
N2 C13 C14 C15 -2.8(17) . . . . ?
N3 C19 C20 C21 0.8(17) . . . . ?
N4 C25 C26 N5 30.2(11) . . . . ?
N4 C25 C26 C27 -154.2(9) . . . . ?
N4 C31 C32 N6 37.7(11) . . . . ?
N4 C31 C32 C33 -138.6(9) . . . . ?
N5 C26 C27 C28 0.0(15) . . . . ?
N6 C32 C33 C34 2.9(13) . . . . ?
N7 C50 C51 N8 -34.5(15) . . . . ?
N7 C50 C51 C52 147.5(12) . . . . ?
N7 C56 C57 N9 -25.4(12) . . . . ?
N7 C56 C57 C58 158.9(10) . . . . ?
N8 C51 C52 C53 -0.3(18) . . . . ?
N9 C57 C58 C59 0.0(17) . . . . ?
N10 C63 C64 N11 -22.5(12) . . . . ?
N10 C63 C64 C65 159.7(9) . . . . ?
N10 C69 C70 N12 -36.9(14) . . . . ?
N10 C69 C70 C71 143.2(13) . . . . ?
N11 C64 C65 C66 -2.3(15) . . . . ?
N12 C70 C71 C72 -1(2) . . . . ?
C1 C2 C3 C4 -2.9(16) . . . . ?
C1 C2 C11 N1 -61.5(11) . . . . ?
C1 C6 C24 N4 -62.4(11) . . . . ?
C2 C1 C6 C5 -0.1(14) . . . . ?
C2 C1 C6 C24 179.5(8) . . . . ?
C2 C3 C4 C5 5.2(16) . . . . ?
C2 C3 C4 C7 178.0(9) . . . . ?
C3 C2 C11 N1 116.4(10) . . . . ?
C3 C4 C5 C6 -5.1(16) . . . . ?
C3 C4 C7 C8A 59.6(14) . . . . ?
C3 C4 C7 C9A 178.4(11) . . . . ?
C3 C4 C7 C10A -65.9(13) . . . . ?
C3 C4 C7 C8B 106.6(17) . . . . ?
C3 C4 C7 C9B -129.9(19) . . . . ?
C3 C4 C7 C10B -3.9(19) . . . . ?
C4 C5 C6 C1 2.6(15) . . . . ?
C4 C5 C6 C24 -176.9(9) . . . . ?
C5 C4 C7 C8A -127.8(12) . . . . ?
C5 C4 C7 C9A -9.0(13) . . . . ?
C5 C4 C7 C10A 106.7(12) . . . . ?
C5 C4 C7 C8B -80.8(17) . . . . ?
C5 C4 C7 C9B 43(2) . . . . ?
C5 C4 C7 C10B 168.7(16) . . . . ?
C5 C6 C24 N4 117.2(10) . . . . ?
C6 C1 C2 C3 0.2(14) . . . . ?
C6 C1 C2 C11 178.2(9) . . . . ?
C7 C4 C5 C6 -178.0(9) . . . . ?
C11 N1 C12 C13 -168.9(8) . . . . ?
C11 N1 C18 C19 92.3(9) . . . . ?
C11 C2 C3 C4 179.3(10) . . . . ?
C12 N1 C11 C2 -178.6(8) . . . . ?
C12 N1 C18 C19 -144.3(8) . . . . ?
C12 C13 C14 C15 175.3(11) . . . . ?
C13 N2 C17 C16 -2.6(15) . . . . ?
C13 C14 C15 C16 1.0(18) . . . . ?
C14 C15 C16 C17 -0.1(17) . . . . ?
C15 C16 C17 N2 0.9(17) . . . . ?
C17 N2 C13 C12 -174.7(9) . . . . ?
C17 N2 C13 C14 3.5(15) . . . . ?
C18 N1 C11 C2 -54.6(9) . . . . ?
C18 N1 C12 C13 68.9(10) . . . . ?
C18 C19 C20 C21 -176.2(11) . . . . ?
C19 N3 C23 C22 1.4(15) . . . . ?
C19 C20 C21 C22 0.4(18) . . . . ?
C20 C21 C22 C23 -0.7(18) . . . . ?
C21 C22 C23 N3 -0.2(18) . . . . ?
C23 N3 C19 C18 175.7(9) . . . . ?
C23 N3 C19 C20 -1.7(15) . . . . ?
C24 N4 C25 C26 98.6(9) . . . . ?
C24 N4 C31 C32 -168.7(8) . . . . ?
C25 N4 C24 C6 -53.8(10) . . . . ?
C25 N4 C31 C32 67.5(10) . . . . ?
C25 C26 C27 C28 -175.3(10) . . . . ?
C26 N5 C30 C29 -0.5(13) . . . . ?
C26 C27 C28 C29 2.3(16) . . . . ?
C27 C28 C29 C30 -3.7(15) . . . . ?
C28 C29 C30 N5 2.9(14) . . . . ?
C30 N5 C26 C25 174.6(8) . . . . ?
C30 N5 C26 C27 -1.0(13) . . . . ?
C31 N4 C24 C6 -176.8(8) . . . . ?
C31 N4 C25 C26 -137.6(8) . . . . ?
C31 C32 C33 C34 179.0(9) . . . . ?
C32 N6 C36 C35 -1.2(11) . . . . ?
C32 C33 C34 C35 -2.7(13) . . . . ?
C33 C34 C35 C36 0.6(12) . . . . ?
C34 C35 C36 N6 1.4(12) . . . . ?
C36 N6 C32 C31 -177.3(7) . . . . ?
C36 N6 C32 C33 -0.9(12) . . . . ?
C39 C40 C41 C42 -0.7(18) . . . . ?
C39 C40 C49 N7 65.9(13) . . . . ?
C39 C44 C62 N10 63.1(13) . . . . ?
C40 C39 C44 C43 4.0(16) . . . . ?
C40 C39 C44 C62 -176.4(10) . . . . ?
C40 C41 C42 C43 2.7(17) . . . . ?
C40 C41 C42 C45 -178.7(11) . . . . ?
C41 C40 C49 N7 -107.9(12) . . . . ?
C41 C42 C43 C44 -1.3(16) . . . . ?
C41 C42 C45 C46 127.8(11) . . . . ?
C41 C42 C45 C47 -110.8(12) . . . . ?
C41 C42 C45 C48 11.7(15) . . . . ?
C42 C43 C44 C39 -2.1(16) . . . . ?
C42 C43 C44 C62 178.4(9) . . . . ?
C43 C42 C45 C46 -53.7(13) . . . . ?
C43 C42 C45 C47 67.7(13) . . . . ?
C43 C42 C45 C48 -169.7(10) . . . . ?
C43 C44 C62 N10 -117.4(10) . . . . ?
C44 C39 C40 C41 -2.7(17) . . . . ?
C44 C39 C40 C49 -176.5(10) . . . . ?
C45 C42 C43 C44 -179.9(10) . . . . ?
C49 N7 C50 C51 -90.8(12) . . . . ?
C49 N7 C56 C57 159.6(8) . . . . ?
C49 C40 C41 C42 173.0(11) . . . . ?
C50 N7 C49 C40 53.3(11) . . . . ?
C50 N7 C56 C57 -74.9(11) . . . . ?
C50 C51 C52 C53 177.5(12) . . . . ?
C51 N8 C55 C54 -2.6(16) . . . . ?
C51 C52 C53 C54 0.2(18) . . . . ?
C52 C53 C54 C55 -1.2(18) . . . . ?
C53 C54 C55 N8 2.4(17) . . . . ?
C55 N8 C51 C50 -176.5(10) . . . . ?
C55 N8 C51 C52 1.5(17) . . . . ?
C56 N7 C49 C40 177.4(8) . . . . ?
C56 N7 C50 C51 144.5(11) . . . . ?
C56 C57 C58 C59 175.4(11) . . . . ?
C57 N9 C61 C60 2.0(14) . . . . ?
C57 C58 C59 C60 2.7(19) . . . . ?
C58 C59 C60 C61 -3.1(19) . . . . ?
C59 C60 C61 N9 0.7(17) . . . . ?
C61 N9 C57 C56 -178.0(9) . . . . ?
C61 N9 C57 C58 -2.3(15) . . . . ?
C62 N10 C63 C64 160.2(8) . . . . ?
C62 N10 C69 C70 -89.5(10) . . . . ?
C63 N10 C62 C44 178.5(8) . . . . ?
C63 N10 C69 C70 147.0(9) . . . . ?
C63 C64 C65 C66 175.4(9) . . . . ?
C64 N11 C68 C67 1.4(14) . . . . ?
C64 C65 C66 C67 1.9(16) . . . . ?
C65 C66 C67 C68 0.1(16) . . . . ?
C66 C67 C68 N11 -1.8(16) . . . . ?
C68 N11 C64 C63 -177.2(8) . . . . ?
C68 N11 C64 C65 0.6(14) . . . . ?
C69 N10 C62 C44 55.2(10) . . . . ?
C69 N10 C63 C64 -76.6(9) . . . . ?
C69 C70 C71 C72 178.5(15) . . . . ?
C70 N12 C74 C73 -7(2) . . . . ?
C70 C71 C72 C73 2(3) . . . . ?
C71 C72 C73 C74 -4(3) . . . . ?
C72 C73 C74 N12 7(3) . . . . ?
C74 N12 C70 C69 -176.2(11) . . . . ?
C74 N12 C70 C71 3.7(19) . . . . ?
O14A S2A C76A F4A -58(3) . . . . ?
O14A S2A C76A F5A -179(3) . . . . ?
O14A S2A C76A F6A 61(3) . . . . ?
O14B S2B C76B F4B -62.9(13) . . . . ?
O14B S2B C76B F5B 178.7(12) . . . . ?
O14B S2B C76B F6B 59.4(15) . . . . ?
O15A S2A C76A F4A -179(3) . . . . ?
O15A S2A C76A F5A 61(3) . . . . ?
O15A S2A C76A F6A -60(3) . . . . ?
O15B S2B C76B F4B -177.9(12) . . . . ?
O15B S2B C76B F5B 63.6(13) . . . . ?
O15B S2B C76B F6B -55.6(15) . . . . ?
O16A S2A C76A F4A 61(3) . . . . ?
O16A S2A C76A F5A -60(3) . . . . ?
O16A S2A C76A F6A 179(3) . . . . ?
O16B S2B C76B F4B 58.4(13) . . . . ?
O16B S2B C76B F5B -60.0(12) . . . . ?
O16B S2B C76B F6B -179.3(13) . . . . ?
O11A S1A C75A F1A -174(2) . . . . ?
O11A S1A C75A F2A 71(2) . . . . ?
O11A S1A C75A F3A -52(2) . . . . ?
O12A S1A C75A F1A 65(2) . . . . ?
O12A S1A C75A F2A -50(2) . . . . ?
O12A S1A C75A F3A -173(2) . . . . ?
O13A S1A C75A F1A -50(3) . . . . ?
O13A S1A C75A F2A -166(3) . . . . ?
O13A S1A C75A F3A 72(3) . . . . ?
O11B S1 C75B F1B -176.1(14) . . . . ?
O11B S1 C75B F2B 61.2(16) . . . . ?
O11B S1 C75B F3B -59.0(15) . . . . ?
O12B S1 C75B F1B 60.6(16) . . . . ?
O12B S1 C75B F2B -62.2(16) . . . . ?
O12B S1 C75B F3B 177.6(15) . . . . ?
O13B S1 C75B F1B -60.4(15) . . . . ?
O13B S1 C75B F2B 176.9(14) . . . . ?
O13B S1 C75B F3B 56.6(15) . . . . ?

_smtbx_masks_special_details     ?
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 0.000 506.1 111.6 '11 H2O'
2 0.000 0.500 0.500 506.1 111.6 '11 H2O'
3 0.456 0.130 0.105 10.2 3.1 '1 ?'
4 0.456 0.370 0.605 10.2 3.1 '1 ?'
5 0.544 0.630 0.395 10.2 3.0 '1 ?'
6 0.544 0.870 0.895 10.2 3.1 '1 ?'

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.048
_oxdiff_exptl_absorpt_empirical_full_min 0.528
