# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ni4a
_database_code_depnum_ccdc_archive 'CCDC 2026736'
loop_
_audit_author_name
_audit_author_address
'Di Sun'
;Shandong university
China
;
_audit_update_record             
;
2020-09-01 deposited with the CCDC.	2021-02-24 downloaded from the CCDC.
;
_audit_creation_date             2020-01-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C62 H70 N12 Ni4 O12, 2(N O3), 2(C2 H3 N)'
_chemical_formula_sum            'C66 H76 N16 Ni4 O18'
_chemical_formula_weight         1616.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         NiCHON
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.7045(4)
_cell_length_b                   25.3661(6)
_cell_length_c                   17.6478(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.667(2)
_cell_angle_gamma                90
_cell_volume                     7474.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15462
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      76.6360
_cell_measurement_theta_min      3.6590
_shelx_estimated_absorpt_T_max   0.965
_shelx_estimated_absorpt_T_min   0.916
_exptl_absorpt_coefficient_mu    1.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41900
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.592
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     95.00 177.00   1.00    5.27    --  107.75  19.00 150.00   82
  2  ω    136.00 178.00   1.00    5.27    --  107.75  37.00  90.00   42
  3  ω    138.00 178.00   1.00    5.27    --  107.75  37.00 -30.00   40
  4  ω    109.00 135.00   1.00    5.27    --  107.75  37.00  90.00   26
  5  ω     85.00 111.00   1.00    5.27    --  107.75  77.00  -3.00   26
  6  ω     95.00 135.00   1.00    5.27    --  107.75  37.00 -30.00   40
  7  ω     76.00 131.00   1.00    5.27    --  107.75 -77.00-129.00   55
  8  ω     39.00 108.00   1.00    5.27    --  107.75 -99.00-150.00   69
  9  ω     38.00 103.00   1.00    5.27    --  107.75 -99.00-180.00   65
 10  ω      8.00  68.00   1.00    1.32    --   48.32 -77.00-129.00   60
 11  ω     41.00  71.00   1.00    1.32    --   48.32  77.00  -3.00   30
 12  ω    -71.00  24.00   1.00    1.32    --  -48.32  77.00  -3.00   95
 13  ω    -53.00 -27.00   1.00    5.27    --  -86.25  77.00  -3.00   26
 14  ω   -103.00 -26.00   1.00    1.32    --  -48.32 -77.00-129.00   77
 15  ω   -139.00 -63.00   1.00    5.27    --  -86.25 -77.00-129.00   76
 16  ω   -158.00 -83.00   1.00    5.27    --  -86.25 -99.00   0.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0022189000
_diffrn_orient_matrix_UB_12      -0.0200903000
_diffrn_orient_matrix_UB_13      -0.0823779000
_diffrn_orient_matrix_UB_21      -0.0539399000
_diffrn_orient_matrix_UB_22      0.0467966000
_diffrn_orient_matrix_UB_23      -0.0238051000
_diffrn_orient_matrix_UB_31      0.0748209000
_diffrn_orient_matrix_UB_32      0.0331232000
_diffrn_orient_matrix_UB_33      -0.0164208000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9896
_reflns_number_total             13102
_reflns_odcompleteness_completeness 98.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.442
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         13102
_refine_ls_number_restraints     175
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0999
_refine_ls_restrained_S_all      1.183
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2700
_refine_ls_wR_factor_ref         0.2942
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 N1-O16
 2.6 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O5-H5
 0.87 with sigma of 0.01
 C59-H12
 1.909789 with sigma of 0.02
 Ni3-H12
 2.790437 with sigma of 0.02
 C60-H5
 1.893626 with sigma of 0.02
 Ni1-H5
 2.836745 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3A \\sim C2A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C65 \\sim N13 \\sim C64: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O16 \\sim O17 \\sim N16 \\sim O18: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
N16A \\sim O18A \\sim O17A \\sim O16A: within 2A with sigma of 0.004 and sigma
for terminal atoms of 0.008
C3 \\sim C2 \\sim N1 \\sim N2 \\sim C4 \\sim C1: within 2A with sigma of 0.004
and sigma for terminal atoms of 0.008
N2A \\sim C4A \\sim C1A \\sim N1A \\sim C2A \\sim C3A: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(N16A) \\sim Ueq, Uanis(O18A) \\sim Ueq, Uanis(O17A) \\sim Ueq,
Uanis(O16A) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.2
4. Others
 Fixed Sof: N1(0.4) H1(0.4) N1A(0.6) H1A(0.6) C1(0.4) H1B(0.4) C1A(0.6)
 H1AA(0.6) C2(0.4) C2A(0.6) C3(0.4) H3A(0.4) H3B(0.4) H3C(0.4) C3A(0.6)
 H3AA(0.6) H3AB(0.6) H3AC(0.6) H5AA(0.4) H5AB(0.4) H5AC(0.4) H5BD(0.6)
 H5BE(0.6) H5BF(0.6) O16(0.5) O17(0.5) O18(0.5) N16(0.5) O18A(0.5) O17A(0.5)
 O16A(0.5) N16A(0.5) C4(0.4) N2(0.4) N2A(0.6) C4A(0.6)
5.a Ternary CH refined with riding coordinates:
 C58(H58), C59(H59), C60(H60), C61(H61)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N1A(H1A), N12(H12A), C1(H1B), C1A(H1AA), C8(H8), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37), C40(H40), C45(H45), C50(H50), C55(H55)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C5(H5AA,H5AB,H5AC), C5(H5BD,H5BE,H5BF),
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C),
  C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C57(H57A,H57B,H57C), C64(H64A,H64B,H64C), C63(H63A,
 H63B,H63C)
;
_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 0.17802(5) 0.40467(3) 0.37324(4) 0.0306(3) Uani 1 1 d D . . . .
Ni2 Ni 0.14964(5) 0.32976(3) 0.20267(4) 0.0271(2) Uani 1 1 d . . . . .
Ni3 Ni 0.26677(6) 0.40818(4) 0.13046(4) 0.0360(3) Uani 1 1 d D . . . .
Ni4 Ni 0.30854(5) 0.33491(3) 0.30377(4) 0.0265(2) Uani 1 1 d . . . . .
O1 O 0.3286(2) 0.32252(14) 0.41443(17) 0.0317(8) Uani 1 1 d . . . . .
O2 O 0.2339(2) 0.37303(14) 0.46717(18) 0.0345(8) Uani 1 1 d . . . . .
O3 O 0.1305(2) 0.31351(14) 0.09220(18) 0.0339(8) Uani 1 1 d . . . . .
O4 O 0.2178(2) 0.36895(15) 0.03877(18) 0.0362(8) Uani 1 1 d . . . . .
O5 O 0.0689(2) 0.36908(14) 0.40467(18) 0.0333(8) Uani 1 1 d D . . . .
H5 H 0.046(2) 0.3675(14) 0.4487(14) 0.050 Uiso 1 1 d DR . . . .
O6 O 0.1174(2) 0.44346(15) 0.28900(19) 0.0383(9) Uani 1 1 d . . . . .
O7 O 0.1839(2) 0.33431(13) 0.31532(17) 0.0260(7) Uani 1 1 d . . . . .
O8 O 0.1537(2) 0.41131(13) 0.17774(18) 0.0347(8) Uani 1 1 d . . . . .
O9 O 0.2909(2) 0.41561(13) 0.32535(18) 0.0320(7) Uani 1 1 d . . . . .
O10 O 0.2732(2) 0.33800(13) 0.19084(17) 0.0285(7) Uani 1 1 d . . . . .
O11 O 0.3229(3) 0.45035(16) 0.2142(2) 0.0472(10) Uani 1 1 d . . . . .
O12 O 0.3779(3) 0.38080(17) 0.0976(2) 0.0436(10) Uani 1 1 d D . . . .
H12 H 0.404(3) 0.3827(17) 0.0553(19) 0.065 Uiso 1 1 d DR . . . .
N1 N 0.3144(8) 0.4596(5) -0.0143(7) 0.055(2) Uani 0.4 1 d D U P A 1
H1 H 0.3161 0.4276 -0.0337 0.066 Uiso 0.4 1 calc R . P A 1
N1A N 0.2390(6) 0.4659(3) -0.0123(4) 0.0428(14) Uani 0.6 1 d . U P B 2
H1A H 0.2350 0.4340 -0.0316 0.051 Uiso 0.6 1 calc R . P B 2
N3 N 0.4529(3) 0.34164(19) 0.1980(2) 0.0350(10) Uani 1 1 d . . . . .
N4 N 0.4274(3) 0.35069(18) 0.2712(2) 0.0340(9) Uani 1 1 d . . . . .
N5 N 0.3270(3) 0.25787(16) 0.2737(2) 0.0279(8) Uani 1 1 d . . . . .
N6 N 0.3367(3) 0.25576(17) 0.1967(2) 0.0295(9) Uani 1 1 d . . . . .
N7 N 0.1448(2) 0.25077(16) 0.23344(19) 0.0265(8) Uani 1 1 d . . . . .
N8 N 0.1357(3) 0.24806(16) 0.3098(2) 0.0276(8) Uani 1 1 d . . . . .
N9 N 0.0311(3) 0.33876(17) 0.2329(2) 0.0315(9) Uani 1 1 d . . . . .
N10 N 0.0044(3) 0.32411(17) 0.3036(2) 0.0317(9) Uani 1 1 d . . . . .
N11 N 0.1629(3) 0.47164(18) 0.4388(2) 0.0370(10) Uani 1 1 d . . . . .
N12 N 0.1284(3) 0.4648(2) 0.5069(2) 0.0426(11) Uani 1 1 d . . . . .
H12A H 0.1211 0.4338 0.5280 0.051 Uiso 1 1 calc R . . . .
C1 C 0.3214(12) 0.5443(7) -0.0036(9) 0.056(2) Uani 0.4 1 d . U P A 1
H1B H 0.3275 0.5809 -0.0138 0.068 Uiso 0.4 1 calc R . P A 1
C1A C 0.2401(7) 0.5509(4) -0.0040(5) 0.0466(16) Uani 0.6 1 d . U P B 2
H1AA H 0.2379 0.5875 -0.0153 0.056 Uiso 0.6 1 calc R . P B 2
C2 C 0.3383(12) 0.5015(7) -0.0513(9) 0.057(2) Uani 0.4 1 d . U P A 1
C2A C 0.2287(7) 0.5105(4) -0.0534(5) 0.0496(15) Uani 0.6 1 d . U P B 2
C3 C 0.3769(14) 0.4999(8) -0.1328(10) 0.068(4) Uani 0.4 1 d . U P A 1
H3A H 0.4340 0.5086 -0.1280 0.103 Uiso 0.4 1 calc GR . P A 1
H3B H 0.3499 0.5256 -0.1662 0.103 Uiso 0.4 1 calc GR . P A 1
H3C H 0.3706 0.4645 -0.1544 0.103 Uiso 0.4 1 calc GR . P A 1
C3A C 0.1991(11) 0.5081(6) -0.1384(6) 0.077(3) Uani 0.6 1 d . U P B 2
H3AA H 0.2092 0.4729 -0.1588 0.115 Uiso 0.6 1 calc GR . P B 2
H3AB H 0.2280 0.5344 -0.1678 0.115 Uiso 0.6 1 calc GR . P B 2
H3AC H 0.1416 0.5156 -0.1418 0.115 Uiso 0.6 1 calc GR . P B 2
C5 C 0.2702(5) 0.5542(3) 0.1381(4) 0.0583(17) Uani 1 1 d . . . . .
H5AA H 0.3132 0.5505 0.1767 0.087 Uiso 0.4 1 calc GR . P C 1
H5AB H 0.2201 0.5404 0.1580 0.087 Uiso 0.4 1 calc GR . P C 1
H5AC H 0.2633 0.5915 0.1251 0.087 Uiso 0.4 1 calc GR . P C 1
H5BD H 0.3279 0.5591 0.1468 0.087 Uiso 0.6 1 calc GR . P D 2
H5BE H 0.2486 0.5332 0.1794 0.087 Uiso 0.6 1 calc GR . P D 2
H5BF H 0.2436 0.5886 0.1363 0.087 Uiso 0.6 1 calc GR . P D 2
C6 C 0.0658(5) 0.5126(3) 0.6125(4) 0.067(2) Uani 1 1 d . . . . .
H6A H 0.0535 0.4768 0.6294 0.101 Uiso 1 1 calc GR . . . .
H6B H 0.0160 0.5327 0.6062 0.101 Uiso 1 1 calc GR . . . .
H6C H 0.1010 0.5299 0.6503 0.101 Uiso 1 1 calc GR . . . .
C7 C 0.1070(4) 0.5101(3) 0.5382(3) 0.0488(15) Uani 1 1 d . . . . .
C8 C 0.1297(5) 0.5499(3) 0.4886(4) 0.0544(16) Uani 1 1 d . . . . .
H8 H 0.1235 0.5869 0.4947 0.065 Uiso 1 1 calc R . . . .
C9 C 0.1639(4) 0.5231(2) 0.4278(3) 0.0431(13) Uani 1 1 d . . . . .
C10 C 0.1985(4) 0.5482(2) 0.3597(3) 0.0493(15) Uani 1 1 d . . . . .
H10A H 0.2475 0.5673 0.3747 0.074 Uiso 1 1 calc GR . . . .
H10B H 0.1596 0.5729 0.3371 0.074 Uiso 1 1 calc GR . . . .
H10C H 0.2112 0.5210 0.3226 0.074 Uiso 1 1 calc GR . . . .
C11 C 0.2952(3) 0.34380(19) 0.4699(3) 0.0299(10) Uani 1 1 d . . . . .
C12 C 0.3335(3) 0.3327(2) 0.5468(2) 0.0295(10) Uani 1 1 d . . . . .
C13 C 0.3061(3) 0.3580(2) 0.6114(3) 0.0372(12) Uani 1 1 d . . . . .
H13 H 0.2620 0.3816 0.6073 0.045 Uiso 1 1 calc R . . . .
C14 C 0.3433(4) 0.3488(3) 0.6819(3) 0.0442(14) Uani 1 1 d . . . . .
H14 H 0.3248 0.3662 0.7257 0.053 Uiso 1 1 calc R . . . .
C15 C 0.4077(3) 0.3140(3) 0.6880(3) 0.0433(14) Uani 1 1 d . . . . .
H15 H 0.4333 0.3080 0.7361 0.052 Uiso 1 1 calc R . . . .
C16 C 0.4348(3) 0.2880(2) 0.6245(3) 0.0398(12) Uani 1 1 d . . . . .
H16 H 0.4779 0.2636 0.6288 0.048 Uiso 1 1 calc R . . . .
C17 C 0.3972(3) 0.2983(2) 0.5539(3) 0.0331(11) Uani 1 1 d . . . . .
H17 H 0.4161 0.2813 0.5100 0.040 Uiso 1 1 calc R . . . .
C18 C 0.1641(3) 0.33359(18) 0.0361(3) 0.0293(10) Uani 1 1 d . . . . .
C19 C 0.1363(3) 0.3143(2) -0.0407(3) 0.0309(11) Uani 1 1 d . . . . .
C20 C 0.1745(4) 0.3306(2) -0.1051(3) 0.0404(13) Uani 1 1 d . . . . .
H20 H 0.2198 0.3532 -0.1005 0.048 Uiso 1 1 calc R . . . .
C21 C 0.1473(5) 0.3143(3) -0.1760(3) 0.0571(18) Uani 1 1 d . . . . .
H21 H 0.1738 0.3257 -0.2200 0.069 Uiso 1 1 calc R . . . .
C22 C 0.0816(4) 0.2814(3) -0.1829(3) 0.0521(16) Uani 1 1 d . . . . .
H22 H 0.0628 0.2705 -0.2317 0.063 Uiso 1 1 calc R . . . .
C23 C 0.0429(4) 0.2643(2) -0.1189(3) 0.0433(13) Uani 1 1 d . . . . .
H23 H -0.0020 0.2414 -0.1233 0.052 Uiso 1 1 calc R . . . .
C24 C 0.0712(3) 0.2813(2) -0.0480(3) 0.0365(12) Uani 1 1 d . . . . .
H24 H 0.0451 0.2698 -0.0039 0.044 Uiso 1 1 calc R . . . .
C25 C 0.3276(4) 0.4485(2) 0.2843(3) 0.0358(11) Uani 1 1 d . . . . .
C26 C 0.3826(4) 0.4873(2) 0.3232(3) 0.0399(12) Uani 1 1 d . . . . .
C27 C 0.4364(4) 0.5157(3) 0.2810(4) 0.0505(15) Uani 1 1 d . . . . .
H27 H 0.4388 0.5100 0.2279 0.061 Uiso 1 1 calc R . . . .
C28 C 0.4870(5) 0.5527(3) 0.3160(5) 0.070(2) Uani 1 1 d . . . . .
H28 H 0.5232 0.5726 0.2868 0.084 Uiso 1 1 calc R . . . .
C29 C 0.4841(5) 0.5603(3) 0.3928(5) 0.067(2) Uani 1 1 d . . . . .
H29 H 0.5189 0.5852 0.4168 0.080 Uiso 1 1 calc R . . . .
C30 C 0.4308(5) 0.5317(3) 0.4357(4) 0.066(2) Uani 1 1 d . . . . .
H30 H 0.4289 0.5375 0.4888 0.079 Uiso 1 1 calc R . . . .
C31 C 0.3803(4) 0.4950(3) 0.4013(4) 0.0506(15) Uani 1 1 d . . . . .
H31 H 0.3444 0.4751 0.4307 0.061 Uiso 1 1 calc R . . . .
C32 C 0.0781(4) 0.4909(2) 0.1802(3) 0.0395(12) Uani 1 1 d . . . . .
C33 C 0.0783(4) 0.4967(3) 0.1017(3) 0.0502(15) Uani 1 1 d . . . . .
H33 H 0.1032 0.4710 0.0711 0.060 Uiso 1 1 calc R . . . .
C34 C 0.0415(5) 0.5408(3) 0.0685(4) 0.066(2) Uani 1 1 d . . . . .
H34 H 0.0415 0.5449 0.0149 0.080 Uiso 1 1 calc R . . . .
C35 C 0.0056(5) 0.5783(3) 0.1118(5) 0.071(2) Uani 1 1 d . . . . .
H35 H -0.0173 0.6088 0.0886 0.085 Uiso 1 1 calc R . . . .
C36 C 0.0025(5) 0.5716(3) 0.1892(5) 0.068(2) Uani 1 1 d . . . . .
H36 H -0.0251 0.5965 0.2191 0.081 Uiso 1 1 calc R . . . .
C37 C 0.0399(4) 0.5284(3) 0.2235(4) 0.0502(15) Uani 1 1 d . . . . .
H37 H 0.0393 0.5245 0.2770 0.060 Uiso 1 1 calc R . . . .
C38 C -0.1215(4) 0.3194(3) 0.3778(4) 0.0591(19) Uani 1 1 d . . . . .
H38A H -0.1126 0.2826 0.3927 0.089 Uiso 1 1 calc GR . . . .
H38B H -0.1789 0.3253 0.3680 0.089 Uiso 1 1 calc GR . . . .
H38C H -0.1025 0.3427 0.4187 0.089 Uiso 1 1 calc GR . . . .
C39 C -0.0766(4) 0.3310(2) 0.3072(3) 0.0404(13) Uani 1 1 d . . . . .
C40 C -0.1024(4) 0.3490(3) 0.2377(3) 0.0430(13) Uani 1 1 d . . . . .
H40 H -0.1559 0.3575 0.2226 0.052 Uiso 1 1 calc R . . . .
C41 C -0.0350(3) 0.3525(2) 0.1932(3) 0.0340(11) Uani 1 1 d . . . . .
C42 C -0.0333(4) 0.3692(3) 0.1122(3) 0.0438(13) Uani 1 1 d . . . . .
H42A H 0.0133 0.3919 0.1047 0.066 Uiso 1 1 calc GR . . . .
H42B H -0.0823 0.3887 0.0989 0.066 Uiso 1 1 calc GR . . . .
H42C H -0.0296 0.3380 0.0797 0.066 Uiso 1 1 calc GR . . . .
C43 C 0.1079(4) 0.1839(2) 0.4134(3) 0.0369(12) Uani 1 1 d . . . . .
H43A H 0.1557 0.1926 0.4443 0.055 Uiso 1 1 calc GR . . . .
H43B H 0.0967 0.1461 0.4172 0.055 Uiso 1 1 calc GR . . . .
H43C H 0.0621 0.2040 0.4316 0.055 Uiso 1 1 calc GR . . . .
C44 C 0.1217(3) 0.19797(19) 0.3324(3) 0.0278(10) Uani 1 1 d . . . . .
C45 C 0.1233(3) 0.1674(2) 0.2684(3) 0.0337(11) Uani 1 1 d . . . . .
H45 H 0.1154 0.1304 0.2654 0.040 Uiso 1 1 calc R . . . .
C46 C 0.1389(3) 0.20167(18) 0.2082(3) 0.0274(10) Uani 1 1 d . . . . .
C47 C 0.1480(3) 0.1879(2) 0.1265(3) 0.0336(11) Uani 1 1 d . . . . .
H47A H 0.0961 0.1766 0.1047 0.050 Uiso 1 1 calc GR . . . .
H47B H 0.1869 0.1593 0.1222 0.050 Uiso 1 1 calc GR . . . .
H47C H 0.1668 0.2189 0.0990 0.050 Uiso 1 1 calc GR . . . .
C48 C 0.3366(3) 0.1965(2) 0.3816(3) 0.0360(11) Uani 1 1 d . . . . .
H48A H 0.3272 0.2287 0.4107 0.054 Uiso 1 1 calc GR . . . .
H48B H 0.3865 0.1799 0.3999 0.054 Uiso 1 1 calc GR . . . .
H48C H 0.2919 0.1720 0.3881 0.054 Uiso 1 1 calc GR . . . .
C49 C 0.3429(3) 0.2099(2) 0.2997(3) 0.0306(10) Uani 1 1 d . . . . .
C50 C 0.3650(4) 0.1774(2) 0.2393(3) 0.0420(13) Uani 1 1 d . . . . .
H50 H 0.3802 0.1414 0.2425 0.050 Uiso 1 1 calc R . . . .
C51 C 0.3603(3) 0.2075(2) 0.1757(3) 0.0339(11) Uani 1 1 d . . . . .
C52 C 0.3760(4) 0.1941(3) 0.0939(3) 0.0488(15) Uani 1 1 d . . . . .
H52A H 0.3250 0.1879 0.0666 0.073 Uiso 1 1 calc GR . . . .
H52B H 0.4091 0.1623 0.0919 0.073 Uiso 1 1 calc GR . . . .
H52C H 0.4041 0.2235 0.0703 0.073 Uiso 1 1 calc GR . . . .
C53 C 0.4944(4) 0.3790(3) 0.3920(3) 0.0448(14) Uani 1 1 d . . . . .
H53A H 0.5181 0.4140 0.4002 0.067 Uiso 1 1 calc GR . . . .
H53B H 0.5261 0.3526 0.4202 0.067 Uiso 1 1 calc GR . . . .
H53C H 0.4394 0.3789 0.4098 0.067 Uiso 1 1 calc GR . . . .
C54 C 0.4938(4) 0.3660(2) 0.3088(3) 0.0390(12) Uani 1 1 d . . . . .
C55 C 0.5591(4) 0.3686(3) 0.2613(3) 0.0453(14) Uani 1 1 d . . . . .
H55 H 0.6124 0.3788 0.2749 0.054 Uiso 1 1 calc R . . . .
C56 C 0.5308(4) 0.3535(3) 0.1916(3) 0.0425(13) Uani 1 1 d . . . . .
C57 C 0.5712(4) 0.3504(3) 0.1172(4) 0.0574(17) Uani 1 1 d . . . . .
H57A H 0.5670 0.3144 0.0973 0.086 Uiso 1 1 calc GR . . . .
H57B H 0.6277 0.3599 0.1243 0.086 Uiso 1 1 calc GR . . . .
H57C H 0.5452 0.3749 0.0812 0.086 Uiso 1 1 calc GR . . . .
C58 C 0.3211(3) 0.3038(2) 0.1518(3) 0.0333(11) Uani 1 1 d . . . . .
H58 H 0.2926 0.2937 0.1034 0.040 Uiso 1 1 calc R . . . .
C59 C 0.4000(4) 0.3317(2) 0.1328(3) 0.0388(13) Uani 1 1 d D . . . .
H59 H 0.4291 0.3097 0.0955 0.047 Uiso 1 1 calc R . . . .
C60 C 0.0571(3) 0.3189(2) 0.3702(3) 0.0325(11) Uani 1 1 d D . . . .
H60 H 0.0310 0.2951 0.4073 0.039 Uiso 1 1 calc R . . . .
C61 C 0.1407(3) 0.29680(19) 0.3537(2) 0.0273(10) Uani 1 1 d . . . . .
H61 H 0.1693 0.2892 0.4031 0.033 Uiso 1 1 calc R . . . .
C66 C 0.1197(3) 0.4453(2) 0.2182(3) 0.0342(11) Uani 1 1 d . . . . .
O13 O 0.0857(3) 0.28774(19) 0.5426(2) 0.0572(12) Uani 1 1 d . . . . .
O14 O 0.0515(3) 0.36947(17) 0.5486(2) 0.0425(9) Uani 1 1 d . . . . .
O15 O 0.0920(5) 0.3288(3) 0.6485(2) 0.092(2) Uani 1 1 d . . . . .
N15 N 0.0768(3) 0.3269(2) 0.5806(3) 0.0492(13) Uani 1 1 d . . . . .
O16 O 0.4162(8) 0.3852(6) -0.0396(9) 0.076(3) Uani 0.5 1 d D U P E 1
O17 O 0.4145(7) 0.3029(6) -0.0331(8) 0.060(3) Uani 0.5 1 d . U P E 1
O18 O 0.4112(9) 0.3486(7) -0.1429(6) 0.085(3) Uani 0.5 1 d . U P E 1
N16 N 0.4037(9) 0.3466(7) -0.0714(9) 0.061(2) Uani 0.5 1 d . U P E 1
N13 N 0.7420(6) 0.4192(5) 0.3108(9) 0.140(4) Uani 1 1 d . U . . .
C64 C 0.6982(8) 0.4980(6) 0.3834(11) 0.141(4) Uani 1 1 d . U . . .
H64A H 0.6754 0.5246 0.3488 0.212 Uiso 1 1 calc GR . . . .
H64B H 0.7447 0.5128 0.4110 0.212 Uiso 1 1 calc GR . . . .
H64C H 0.6578 0.4874 0.4196 0.212 Uiso 1 1 calc GR . . . .
C65 C 0.7211(7) 0.4557(6) 0.3435(11) 0.129(4) Uani 1 1 d . U . . .
N14 N 0.2252(4) 0.6798(4) -0.0610(4) 0.079(2) Uani 1 1 d . . . . .
C62 C 0.2443(4) 0.7032(3) -0.1119(5) 0.0592(18) Uani 1 1 d . . . . .
C63 C 0.2697(5) 0.7309(3) -0.1778(5) 0.0664(19) Uani 1 1 d . . . . .
H63A H 0.2918 0.7057 -0.2138 0.100 Uiso 1 1 calc GR . . . .
H63B H 0.3109 0.7567 -0.1629 0.100 Uiso 1 1 calc GR . . . .
H63C H 0.2238 0.7491 -0.2016 0.100 Uiso 1 1 calc GR . . . .
O18A O 0.3799(9) 0.3166(6) -0.1403(5) 0.081(3) Uani 0.5 1 d . U P F 2
O17A O 0.3835(11) 0.2885(7) -0.0276(9) 0.082(3) Uani 0.5 1 d . U P F 2
O16A O 0.3834(9) 0.3776(7) -0.0488(8) 0.070(3) Uani 0.5 1 d . U P F 2
N16A N 0.3899(10) 0.3235(8) -0.0699(10) 0.069(3) Uani 0.5 1 d . U P F 2
C4 C 0.2935(14) 0.5209(8) 0.0617(11) 0.055(2) Uani 0.4 1 d . U P A 1
N2 N 0.2871(11) 0.4693(8) 0.0559(10) 0.053(2) Uani 0.4 1 d . U P A 1
N2A N 0.2561(6) 0.4759(4) 0.0625(5) 0.0406(16) Uani 0.6 1 d . U P B 2
C4A C 0.2562(8) 0.5276(4) 0.0683(6) 0.0433(16) Uani 0.6 1 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 O2 2.043(3) . ?
Ni1 O5 2.123(4) . ?
Ni1 O6 2.029(4) . ?
Ni1 O7 2.060(3) . ?
Ni1 O9 2.108(4) . ?
Ni1 N11 2.075(4) . ?
Ni2 O3 2.009(3) . ?
Ni2 O7 2.056(3) . ?
Ni2 O8 2.116(3) . ?
Ni2 O10 2.091(3) . ?
Ni2 N7 2.078(4) . ?
Ni2 N9 2.078(5) . ?
Ni3 O4 2.050(3) . ?
Ni3 O8 2.089(4) . ?
Ni3 O10 2.076(3) . ?
Ni3 O11 2.032(4) . ?
Ni3 O12 2.080(5) . ?
Ni3 N2 2.068(18) . ?
Ni3 N2A 2.099(10) . ?
Ni4 O1 1.997(3) . ?
Ni4 O7 2.098(3) . ?
Ni4 O9 2.104(4) . ?
Ni4 O10 2.063(3) . ?
Ni4 N4 2.121(5) . ?
Ni4 N5 2.051(4) . ?
O1 C11 1.263(6) . ?
O2 C11 1.263(6) . ?
O3 C18 1.259(6) . ?
O4 C18 1.268(6) . ?
O5 H5 0.880(10) . ?
O5 C60 1.421(6) . ?
O6 C66 1.252(6) . ?
O7 C61 1.383(6) . ?
O8 C66 1.265(7) . ?
O9 C25 1.274(7) . ?
O10 C58 1.378(6) . ?
O11 C25 1.237(6) . ?
O12 H12 0.879(10) . ?
O12 C59 1.437(7) . ?
N1 H1 0.8800 . ?
N1 C2 1.32(2) . ?
N1 N2 1.36(2) . ?
N1A H1A 0.8800 . ?
N1A C2A 1.352(12) . ?
N1A N2A 1.367(13) . ?
N3 N4 1.391(6) . ?
N3 C56 1.343(8) . ?
N3 C59 1.452(7) . ?
N4 C54 1.334(7) . ?
N5 N6 1.375(5) . ?
N5 C49 1.324(7) . ?
N6 C51 1.343(7) . ?
N6 C58 1.472(7) . ?
N7 N8 1.363(5) . ?
N7 C46 1.325(6) . ?
N8 C44 1.354(6) . ?
N8 C61 1.460(6) . ?
N9 N10 1.388(6) . ?
N9 C41 1.336(7) . ?
N10 C39 1.367(8) . ?
N10 C60 1.454(7) . ?
N11 N12 1.360(6) . ?
N11 C9 1.319(8) . ?
N12 H12A 0.8800 . ?
N12 C7 1.327(8) . ?
C1 H1B 0.9500 . ?
C1 C2 1.41(3) . ?
C1 C4 1.39(2) . ?
C1A H1AA 0.9500 . ?
C1A C2A 1.356(15) . ?
C1A C4A 1.425(13) . ?
C2 C3 1.60(2) . ?
C2A C3A 1.566(15) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C5 H5AA 0.9800 . ?
C5 H5AB 0.9800 . ?
C5 H5AC 0.9800 . ?
C5 H5BD 0.9800 . ?
C5 H5BE 0.9800 . ?
C5 H5BF 0.9800 . ?
C5 C4 1.65(2) . ?
C5 C4A 1.418(13) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 C7 1.500(9) . ?
C7 C8 1.396(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.406(8) . ?
C9 C10 1.491(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.510(6) . ?
C12 C13 1.397(7) . ?
C12 C17 1.379(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.395(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.393(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.404(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.502(6) . ?
C19 C20 1.384(7) . ?
C19 C24 1.375(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.382(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.380(10) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.392(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.498(8) . ?
C26 C27 1.386(9) . ?
C26 C31 1.394(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.396(10) . ?
C28 H28 0.9500 . ?
C28 C29 1.370(12) . ?
C29 H29 0.9500 . ?
C29 C30 1.390(13) . ?
C30 H30 0.9500 . ?
C30 C31 1.386(10) . ?
C31 H31 0.9500 . ?
C32 C33 1.394(8) . ?
C32 C37 1.386(9) . ?
C32 C66 1.498(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.397(9) . ?
C34 H34 0.9500 . ?
C34 C35 1.370(13) . ?
C35 H35 0.9500 . ?
C35 C36 1.379(12) . ?
C36 H36 0.9500 . ?
C36 C37 1.392(9) . ?
C37 H37 0.9500 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C38 C39 1.503(8) . ?
C39 C40 1.367(8) . ?
C40 H40 0.9500 . ?
C40 C41 1.395(8) . ?
C41 C42 1.492(7) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 C44 1.497(6) . ?
C44 C45 1.370(7) . ?
C45 H45 0.9500 . ?
C45 C46 1.402(7) . ?
C46 C47 1.496(7) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 C49 1.493(7) . ?
C49 C50 1.404(7) . ?
C50 H50 0.9500 . ?
C50 C51 1.359(8) . ?
C51 C52 1.512(7) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C53 C54 1.505(7) . ?
C54 C55 1.396(9) . ?
C55 H55 0.9500 . ?
C55 C56 1.360(9) . ?
C56 C57 1.496(8) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58 1.0000 . ?
C58 C59 1.541(8) . ?
C59 H59 1.0000 . ?
C60 H60 1.0000 . ?
C60 C61 1.542(7) . ?
C61 H61 1.0000 . ?
O13 N15 1.210(7) . ?
O14 N15 1.285(7) . ?
O15 N15 1.218(7) . ?
O16 N16 1.14(2) . ?
O17 N16 1.31(2) . ?
O18 N16 1.273(19) . ?
N13 C65 1.150(17) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C64 C65 1.345(19) . ?
N14 C62 1.128(11) . ?
C62 C63 1.434(12) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
O18A N16A 1.26(2) . ?
O17A N16A 1.17(2) . ?
O16A N16A 1.43(2) . ?
C4 N2 1.32(3) . ?
N2A C4A 1.316(14) . ?

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 O5 89.83(15) . . ?
O2 Ni1 O7 92.01(14) . . ?
O2 Ni1 O9 89.06(14) . . ?
O2 Ni1 N11 85.97(16) . . ?
O6 Ni1 O2 172.61(15) . . ?
O6 Ni1 O5 89.06(15) . . ?
O6 Ni1 O7 94.97(14) . . ?
O6 Ni1 O9 94.34(15) . . ?
O6 Ni1 N11 86.84(16) . . ?
O7 Ni1 O5 79.34(13) . . ?
O7 Ni1 O9 81.89(13) . . ?
O7 Ni1 N11 173.79(17) . . ?
O9 Ni1 O5 161.15(14) . . ?
N11 Ni1 O5 94.77(17) . . ?
N11 Ni1 O9 103.92(17) . . ?
O3 Ni2 O7 169.04(15) . . ?
O3 Ni2 O8 90.23(14) . . ?
O3 Ni2 O10 93.05(14) . . ?
O3 Ni2 N7 92.84(14) . . ?
O3 Ni2 N9 98.38(16) . . ?
O7 Ni2 O8 97.84(13) . . ?
O7 Ni2 O10 80.97(13) . . ?
O7 Ni2 N7 79.24(13) . . ?
O7 Ni2 N9 89.21(14) . . ?
O10 Ni2 O8 81.02(15) . . ?
N7 Ni2 O8 176.81(14) . . ?
N7 Ni2 O10 99.69(15) . . ?
N9 Ni2 O8 89.00(16) . . ?
N9 Ni2 O10 164.86(15) . . ?
N9 Ni2 N7 89.68(16) . . ?
O4 Ni3 O8 89.36(15) . . ?
O4 Ni3 O10 90.14(14) . . ?
O4 Ni3 O12 87.52(16) . . ?
O4 Ni3 N2 86.0(5) . . ?
O4 Ni3 N2A 85.5(3) . . ?
O8 Ni3 N2A 97.7(3) . . ?
O10 Ni3 O8 82.04(13) . . ?
O10 Ni3 O12 79.85(14) . . ?
O10 Ni3 N2A 175.6(3) . . ?
O11 Ni3 O4 174.40(16) . . ?
O11 Ni3 O8 95.31(16) . . ?
O11 Ni3 O10 93.56(15) . . ?
O11 Ni3 O12 89.00(18) . . ?
O11 Ni3 N2 89.3(5) . . ?
O11 Ni3 N2A 90.8(3) . . ?
O12 Ni3 O8 161.60(15) . . ?
O12 Ni3 N2A 100.1(3) . . ?
N2 Ni3 O8 113.1(5) . . ?
N2 Ni3 O10 164.3(5) . . ?
N2 Ni3 O12 84.7(5) . . ?
O1 Ni4 O7 92.46(14) . . ?
O1 Ni4 O9 89.80(14) . . ?
O1 Ni4 O10 170.33(15) . . ?
O1 Ni4 N4 99.36(15) . . ?
O1 Ni4 N5 94.63(15) . . ?
O7 Ni4 O9 81.10(14) . . ?
O7 Ni4 N4 165.27(15) . . ?
O9 Ni4 N4 90.13(16) . . ?
O10 Ni4 O7 80.64(13) . . ?
O10 Ni4 O9 95.76(13) . . ?
O10 Ni4 N4 88.55(14) . . ?
N5 Ni4 O7 100.09(15) . . ?
N5 Ni4 O9 175.35(14) . . ?
N5 Ni4 O10 80.06(14) . . ?
N5 Ni4 N4 87.76(17) . . ?
C11 O1 Ni4 128.7(3) . . ?
C11 O2 Ni1 127.8(3) . . ?
C18 O3 Ni2 128.2(3) . . ?
C18 O4 Ni3 129.6(3) . . ?
Ni1 O5 H5 131(2) . . ?
C60 O5 Ni1 112.2(3) . . ?
C60 O5 H5 106.1(17) . . ?
C66 O6 Ni1 136.1(4) . . ?
Ni1 O7 Ni4 95.95(14) . . ?
Ni2 O7 Ni1 120.82(16) . . ?
Ni2 O7 Ni4 98.95(13) . . ?
C61 O7 Ni1 108.7(3) . . ?
C61 O7 Ni2 107.5(3) . . ?
C61 O7 Ni4 125.9(3) . . ?
Ni3 O8 Ni2 94.63(15) . . ?
C66 O8 Ni2 122.1(3) . . ?
C66 O8 Ni3 132.7(3) . . ?
Ni4 O9 Ni1 94.35(14) . . ?
C25 O9 Ni1 139.9(4) . . ?
C25 O9 Ni4 117.5(3) . . ?
Ni3 O10 Ni2 95.76(15) . . ?
Ni4 O10 Ni2 98.93(13) . . ?
Ni4 O10 Ni3 122.51(16) . . ?
C58 O10 Ni2 125.2(3) . . ?
C58 O10 Ni3 107.8(3) . . ?
C58 O10 Ni4 107.8(3) . . ?
C25 O11 Ni3 136.2(4) . . ?
Ni3 O12 H12 134(2) . . ?
C59 O12 Ni3 112.9(3) . . ?
C59 O12 H12 106.6(18) . . ?
C2 N1 H1 122.6 . . ?
C2 N1 N2 114.9(15) . . ?
N2 N1 H1 122.6 . . ?
C2A N1A H1A 123.7 . . ?
C2A N1A N2A 112.5(9) . . ?
N2A N1A H1A 123.7 . . ?
N4 N3 C59 124.7(4) . . ?
C56 N3 N4 111.4(4) . . ?
C56 N3 C59 122.8(4) . . ?
N3 N4 Ni4 122.3(3) . . ?
C54 N4 Ni4 133.8(3) . . ?
C54 N4 N3 103.7(4) . . ?
N6 N5 Ni4 108.4(3) . . ?
C49 N5 Ni4 144.7(3) . . ?
C49 N5 N6 106.1(4) . . ?
N5 N6 C58 118.4(4) . . ?
C51 N6 N5 110.7(4) . . ?
C51 N6 C58 131.0(4) . . ?
N8 N7 Ni2 108.3(3) . . ?
C46 N7 Ni2 145.2(3) . . ?
C46 N7 N8 106.0(4) . . ?
N7 N8 C61 118.4(4) . . ?
C44 N8 N7 111.3(4) . . ?
C44 N8 C61 130.3(4) . . ?
N10 N9 Ni2 122.3(3) . . ?
C41 N9 Ni2 132.3(3) . . ?
C41 N9 N10 105.0(4) . . ?
N9 N10 C60 123.2(4) . . ?
C39 N10 N9 110.6(4) . . ?
C39 N10 C60 123.4(4) . . ?
N12 N11 Ni1 116.8(4) . . ?
C9 N11 Ni1 136.5(4) . . ?
C9 N11 N12 105.3(4) . . ?
N11 N12 H12A 123.7 . . ?
C7 N12 N11 112.6(5) . . ?
C7 N12 H12A 123.7 . . ?
C2 C1 H1B 128.0 . . ?
C4 C1 H1B 128.0 . . ?
C4 C1 C2 104.0(16) . . ?
C2A C1A H1AA 126.8 . . ?
C2A C1A C4A 106.4(9) . . ?
C4A C1A H1AA 126.8 . . ?
N1 C2 C1 105.0(14) . . ?
N1 C2 C3 124.2(17) . . ?
C1 C2 C3 130.7(15) . . ?
N1A C2A C1A 105.9(8) . . ?
N1A C2A C3A 120.8(10) . . ?
C1A C2A C3A 132.8(10) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2A C3A H3AA 109.5 . . ?
C2A C3A H3AB 109.5 . . ?
C2A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
H5AA C5 H5AB 109.5 . . ?
H5AA C5 H5AC 109.5 . . ?
H5AB C5 H5AC 109.5 . . ?
H5BD C5 H5BE 109.5 . . ?
H5BD C5 H5BF 109.5 . . ?
H5BE C5 H5BF 109.5 . . ?
C4 C5 H5AA 109.5 . . ?
C4 C5 H5AB 109.5 . . ?
C4 C5 H5AC 109.5 . . ?
C4A C5 H5BD 109.5 . . ?
C4A C5 H5BE 109.5 . . ?
C4A C5 H5BF 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
N12 C7 C6 122.4(6) . . ?
N12 C7 C8 106.5(5) . . ?
C8 C7 C6 131.1(6) . . ?
C7 C8 H8 127.7 . . ?
C7 C8 C9 104.6(5) . . ?
C9 C8 H8 127.7 . . ?
N11 C9 C8 111.0(5) . . ?
N11 C9 C10 123.3(5) . . ?
C8 C9 C10 125.7(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C11 C12 115.6(4) . . ?
O2 C11 O1 126.7(4) . . ?
O2 C11 C12 117.8(4) . . ?
C13 C12 C11 120.5(5) . . ?
C17 C12 C11 120.3(4) . . ?
C17 C12 C13 119.2(5) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.1(5) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0(5) . . ?
C15 C14 H14 120.0 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.5(5) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 120.6 . . ?
C15 C16 C17 118.7(5) . . ?
C17 C16 H16 120.6 . . ?
C12 C17 C16 121.5(5) . . ?
C12 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
O3 C18 O4 126.0(4) . . ?
O3 C18 C19 116.4(4) . . ?
O4 C18 C19 117.6(4) . . ?
C20 C19 C18 120.3(5) . . ?
C24 C19 C18 120.5(4) . . ?
C24 C19 C20 119.2(5) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.4(6) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.1(6) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.8 . . ?
C21 C22 C23 120.3(5) . . ?
C23 C22 H22 119.8 . . ?
C22 C23 H23 120.7 . . ?
C22 C23 C24 118.7(6) . . ?
C24 C23 H23 120.7 . . ?
C19 C24 C23 121.3(5) . . ?
C19 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
O9 C25 C26 117.9(4) . . ?
O11 C25 O9 125.1(5) . . ?
O11 C25 C26 117.0(5) . . ?
C27 C26 C25 119.6(5) . . ?
C27 C26 C31 119.7(6) . . ?
C31 C26 C25 120.7(6) . . ?
C26 C27 H27 119.8 . . ?
C26 C27 C28 120.4(7) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 120.2 . . ?
C29 C28 C27 119.6(8) . . ?
C29 C28 H28 120.2 . . ?
C28 C29 H29 119.7 . . ?
C28 C29 C30 120.5(6) . . ?
C30 C29 H29 119.7 . . ?
C29 C30 H30 119.9 . . ?
C31 C30 C29 120.2(7) . . ?
C31 C30 H30 119.9 . . ?
C26 C31 H31 120.2 . . ?
C30 C31 C26 119.6(7) . . ?
C30 C31 H31 120.2 . . ?
C33 C32 C66 120.8(6) . . ?
C37 C32 C33 119.4(6) . . ?
C37 C32 C66 119.8(5) . . ?
C32 C33 H33 120.4 . . ?
C32 C33 C34 119.2(7) . . ?
C34 C33 H33 120.4 . . ?
C33 C34 H34 119.4 . . ?
C35 C34 C33 121.1(7) . . ?
C35 C34 H34 119.4 . . ?
C34 C35 H35 120.1 . . ?
C34 C35 C36 119.8(7) . . ?
C36 C35 H35 120.1 . . ?
C35 C36 H36 120.1 . . ?
C35 C36 C37 119.9(8) . . ?
C37 C36 H36 120.1 . . ?
C32 C37 C36 120.6(6) . . ?
C32 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
N10 C39 C38 122.2(5) . . ?
N10 C39 C40 106.7(5) . . ?
C40 C39 C38 131.1(6) . . ?
C39 C40 H40 126.6 . . ?
C39 C40 C41 106.8(5) . . ?
C41 C40 H40 126.6 . . ?
N9 C41 C40 110.8(4) . . ?
N9 C41 C42 122.6(5) . . ?
C40 C41 C42 126.6(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
N8 C44 C43 122.4(4) . . ?
N8 C44 C45 106.3(4) . . ?
C45 C44 C43 131.3(5) . . ?
C44 C45 H45 126.8 . . ?
C44 C45 C46 106.4(4) . . ?
C46 C45 H45 126.8 . . ?
N7 C46 C45 110.0(4) . . ?
N7 C46 C47 122.3(4) . . ?
C45 C46 C47 127.8(4) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
N5 C49 C48 121.7(4) . . ?
N5 C49 C50 109.4(4) . . ?
C50 C49 C48 128.9(5) . . ?
C49 C50 H50 126.6 . . ?
C51 C50 C49 106.7(5) . . ?
C51 C50 H50 126.6 . . ?
N6 C51 C50 107.1(4) . . ?
N6 C51 C52 121.9(5) . . ?
C50 C51 C52 131.0(5) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C54 C53 H53A 109.5 . . ?
C54 C53 H53B 109.5 . . ?
C54 C53 H53C 109.5 . . ?
N4 C54 C53 122.0(5) . . ?
N4 C54 C55 111.6(5) . . ?
C55 C54 C53 126.3(5) . . ?
C54 C55 H55 127.1 . . ?
C56 C55 C54 105.8(5) . . ?
C56 C55 H55 127.1 . . ?
N3 C56 C55 107.5(5) . . ?
N3 C56 C57 121.6(5) . . ?
C55 C56 C57 130.9(6) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O10 C58 N6 110.4(4) . . ?
O10 C58 H58 108.7 . . ?
O10 C58 C59 109.4(4) . . ?
N6 C58 H58 108.7 . . ?
N6 C58 C59 110.9(5) . . ?
C59 C58 H58 108.7 . . ?
O12 C59 N3 109.6(4) . . ?
O12 C59 C58 106.3(5) . . ?
O12 C59 H59 108.8 . . ?
N3 C59 C58 114.3(4) . . ?
N3 C59 H59 108.8 . . ?
C58 C59 H59 108.8 . . ?
O5 C60 N10 109.8(4) . . ?
O5 C60 H60 108.6 . . ?
O5 C60 C61 107.0(4) . . ?
N10 C60 H60 108.6 . . ?
N10 C60 C61 114.3(4) . . ?
C61 C60 H60 108.6 . . ?
O7 C61 N8 110.2(3) . . ?
O7 C61 C60 109.3(4) . . ?
O7 C61 H61 108.5 . . ?
N8 C61 C60 111.7(4) . . ?
N8 C61 H61 108.5 . . ?
C60 C61 H61 108.5 . . ?
O6 C66 O8 124.4(5) . . ?
O6 C66 C32 116.7(5) . . ?
O8 C66 C32 118.9(4) . . ?
O13 N15 O14 119.3(5) . . ?
O13 N15 O15 123.5(6) . . ?
O15 N15 O14 117.2(6) . . ?
O16 N16 O17 116.9(16) . . ?
O16 N16 O18 115.5(17) . . ?
O18 N16 O17 121.9(17) . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C65 C64 H64A 109.5 . . ?
C65 C64 H64B 109.5 . . ?
C65 C64 H64C 109.5 . . ?
N13 C65 C64 178.4(17) . . ?
N14 C62 C63 177.7(9) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
O18A N16A O16A 112.5(17) . . ?
O17A N16A O18A 120.7(18) . . ?
O17A N16A O16A 123.9(16) . . ?
C1 C4 C5 123.5(16) . . ?
N2 C4 C1 112.9(17) . . ?
N2 C4 C5 123.6(14) . . ?
N1 N2 Ni3 120.7(13) . . ?
C4 N2 Ni3 135.2(13) . . ?
C4 N2 N1 102.9(14) . . ?
N1A N2A Ni3 114.4(7) . . ?
C4A N2A Ni3 140.5(7) . . ?
C4A N2A N1A 105.0(8) . . ?
C5 C4A C1A 127.1(9) . . ?
N2A C4A C1A 110.1(9) . . ?
N2A C4A C5 122.8(8) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.989
_oxdiff_exptl_absorpt_empirical_full_min 0.473
####################################################################### 
# 
# 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_Ni5a
_database_code_depnum_ccdc_archive 'CCDC 2026737'
loop_
_audit_author_name
_audit_author_address
'Di Sun'
;Shandong university
China
;
_audit_update_record             
;
2020-09-01 deposited with the CCDC.	2021-02-24 downloaded from the CCDC.
;
_audit_creation_date             2020-01-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C61 H68 N10 Ni5 O19 S6, C H4 O'
_chemical_formula_sum            'C62 H72 N10 Ni5 O20 S6'
_chemical_formula_weight         1763.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   13.897(9)
_cell_length_b                   14.250(9)
_cell_length_c                   21.731(13)
_cell_angle_alpha                106.518(6)
_cell_angle_beta                 95.516(6)
_cell_angle_gamma                96.119(6)
_cell_volume                     4066(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2874
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.520
_cell_measurement_theta_min      2.264
_shelx_estimated_absorpt_T_max   0.973
_shelx_estimated_absorpt_T_min   0.948
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.948
_diffrn_reflns_av_R_equivalents  0.1548
_diffrn_reflns_av_unetI/netI     0.2032
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54058
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.672
_diffrn_ambient_temperature      298.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6425
_reflns_number_total             16589
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         16589
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1910
_refine_ls_R_factor_gt           0.0702
_refine_ls_restrained_S_all      0.924
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0824P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.2162
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{S9, C3AA}
{C9, S2}
{C2AA, S4}
{S1, C4AA}
{C3, S6}
{S3, C5AA}
{C7, S8}
{S7, C6AA}
{S5, C5}
{C0AA, S10}
{S11, C8AA}
{C11, S12}
3. Restrained distances
 O16-H16
 0.85 with sigma of 0.01
 O20-H20
 0.85 with sigma of 0.01
 O15-H15B
 0.9 with sigma of 0.01
 Ni4-H16
 2.547289 with sigma of 0.02
 C60-H20
 1.974458 with sigma of 0.02
 Ni5-H20
 2.70472 with sigma of 0.02
 C61-H16
 1.882298 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O20 \\sim C60: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C9) = Uanis(S2)
Uanis(S1) = Uanis(C4AA)
Uanis(S11) = Uanis(C8AA)
Uanis(S3) = Uanis(C5AA)
Uanis(C2AA) = Uanis(S1)
Uanis(C2AA) = Uanis(S4)
Uanis(S7) = Uanis(C6AA)
Uanis(C3) = Uanis(S3)
Uanis(C3) = Uanis(S6)
Uanis(S11) = Uanis(C11)
Uanis(C11) = Uanis(S12)
Uanis(S9) = Uanis(C9)
Uanis(S9) = Uanis(C3AA)
Uanis(C7) = Uanis(S8)
Uanis(C7) = Uanis(S7)
Uanis(C0AA) = Uanis(S10)
Uanis(S5) = Uanis(C5)
Uanis(S5) = Uanis(C0AA)
5. Others
 Sof(S2)=Sof(C3AA)=Sof(H3AA)=Sof(H25A)=Sof(H26A)=1-FVAR(1)
 Sof(S9)=Sof(C9)=Sof(H9A)=Sof(H25)=Sof(H26)=FVAR(1)
 Sof(S4)=Sof(C4AA)=Sof(H4AA)=Sof(H6B)=Sof(H8B)=1-FVAR(2)
 Sof(S1)=Sof(C2AA)=Sof(H2AA)=Sof(H6A)=Sof(H8A)=FVAR(2)
 Sof(S6)=Sof(C5AA)=Sof(H5AA)=Sof(H13A)=Sof(H14A)=1-FVAR(3)
 Sof(S3)=Sof(C3)=Sof(H3)=Sof(H13)=Sof(H14)=FVAR(3)
 Sof(S8)=Sof(C6AA)=Sof(H6AA)=Sof(H17A)=Sof(H18A)=1-FVAR(4)
 Sof(S7)=Sof(C7)=Sof(H7)=Sof(H17)=Sof(H18)=FVAR(4)
 Sof(S10)=Sof(C5)=Sof(H5)=Sof(H21A)=Sof(H22A)=1-FVAR(5)
 Sof(S5)=Sof(C0AA)=Sof(H0AA)=Sof(H21)=Sof(H22)=FVAR(5)
 Sof(S12)=Sof(C8AA)=Sof(H8AA)=Sof(H29A)=Sof(H30A)=1-FVAR(6)
 Sof(S11)=Sof(C11)=Sof(H11)=Sof(H29)=Sof(H30)=FVAR(6)
6.a Ternary CH refined with riding coordinates:
 C41(H41), C42(H42), C53(H53), C54(H54)
6.b Aromatic/amide H refined with riding coordinates:
 N9(H9), C2AA(H2AA), C3(H3), C3AA(H3AA), C4AA(H4AA), C0AA(H0AA), C5AA(H5AA),
 C6(H6A), C6(H6B), C6AA(H6AA), C7(H7), C5(H5), C8(H8A), C8(H8B), C8AA(H8AA),
 C9(H9A), C11(H11), C13(H13), C13(H13A), C14(H14), C14(H14A), C17(H17),
 C17(H17A), C18(H18), C18(H18A), C21(H21), C21(H21A), C22(H22), C22(H22A),
 C25(H25), C25(H25A), C26(H26), C26(H26A), C29(H29), C29(H29A), C30(H30),
 C30(H30A), C33(H33), C38(H38), C45(H45), C50(H50), C57(H57)
6.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C52(H52A,
 H52B,H52C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C),
 C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
6.d Idealised tetrahedral OH refined as rotating group:
 O19(H19)
;
_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 0.85470(7) 0.47994(7) 0.80523(5) 0.0448(3) Uani 1 1 d . . . . .
Ni2 Ni 0.69050(7) 0.29087(7) 0.69456(5) 0.0422(3) Uani 1 1 d . . . . .
Ni3 Ni 0.90431(7) 0.34700(7) 0.67310(5) 0.0468(3) Uani 1 1 d . . . . .
Ni4 Ni 0.84624(7) 0.58949(7) 0.70076(5) 0.0503(3) Uani 1 1 d D . . . .
Ni5 Ni 0.54217(8) 0.14731(8) 0.76375(5) 0.0605(3) Uani 1 1 d D . . . .
S1 S 0.2467(4) 0.3366(4) 0.6180(3) 0.0818(9) Uani 0.267(5) 1 d . . P A 3
S2 S 0.6716(7) -0.0710(6) 0.9703(4) 0.1368(18) Uani 0.250(7) 1 d . . P B 2
S3 S 0.5604(3) 0.2531(3) 0.44616(18) 0.0966(10) Uani 0.638(5) 1 d . . P C 5
S4 S 0.3157(2) 0.3762(2) 0.56768(16) 0.0818(9) Uani 0.733(5) 1 d . . P A 4
S5 S 1.0869(3) 0.9524(2) 0.92122(17) 0.1142(19) Uani 0.784(11) 1 d . . P D 9
S6 S 0.5530(4) 0.3642(4) 0.4478(2) 0.0966(10) Uani 0.362(5) 1 d . . P C 6
S7 S 0.4438(4) 0.6505(4) 0.7286(2) 0.091(2) Uani 0.453(11) 1 d . . P E 7
S8 S 0.5368(4) 0.7433(3) 0.7674(3) 0.115(3) Uani 0.547(11) 1 d . . P E 8
S9 S 0.7603(4) -0.1195(3) 0.9403(2) 0.1368(18) Uani 0.750(7) 1 d . . P B 1
S10 S 1.0865(7) 0.8871(6) 0.9786(4) 0.135(9) Uani 0.216(11) 1 d . . P D 10
S11 S 0.8696(3) -0.1097(3) 0.5111(2) 0.1325(14) Uani 0.864(7) 1 d . . P F 11
S12 S 0.7540(8) -0.1231(7) 0.5167(5) 0.1325(14) Uani 0.136(7) 1 d . . P F 12
O1 O 0.8248(3) 0.3381(3) 0.7480(2) 0.0401(12) Uani 1 1 d . . . . .
O2 O 0.9262(3) 0.4904(4) 0.7261(2) 0.0449(13) Uani 1 1 d . . . . .
O3 O 0.7645(3) 0.3509(3) 0.6314(2) 0.0422(12) Uani 1 1 d . . . . .
O4 O 0.6611(3) 0.2477(3) 0.7720(2) 0.0431(12) Uani 1 1 d . . . . .
O5 O 0.6258(3) 0.4177(4) 0.7308(2) 0.0480(13) Uani 1 1 d . . . . .
O6 O 0.7340(4) 0.1603(4) 0.6466(2) 0.0520(14) Uani 1 1 d . . . . .
O7 O 0.7527(4) 0.5369(4) 0.7556(2) 0.0466(13) Uani 1 1 d . . . . .
O8 O 0.7699(4) 0.4987(4) 0.6171(2) 0.0517(14) Uani 1 1 d . . . . .
O9 O 0.8881(4) 0.2008(4) 0.6348(3) 0.0570(15) Uani 1 1 d . . . . .
O10 O 0.9071(4) 0.6966(4) 0.7802(3) 0.0594(16) Uani 1 1 d . . . . .
O11 O 0.9718(4) 0.6115(4) 0.6575(3) 0.0596(15) Uani 1 1 d . . . . .
O12 O 0.5625(4) 0.2432(4) 0.6385(3) 0.0556(14) Uani 1 1 d . . . . .
O13 O 0.9163(4) 0.6180(4) 0.8567(2) 0.0566(15) Uani 1 1 d . . . . .
O14 O 0.4641(4) 0.2054(4) 0.7042(3) 0.0645(16) Uani 1 1 d . . . . .
O15 O 0.5905(5) 0.0484(5) 0.6859(3) 0.0696(18) Uani 1 1 d D . . . .
H15A H 0.638(7) 0.024(7) 0.708(5) 0.104 Uiso 1 1 d R . . . .
H15B H 0.617(14) 0.100(9) 0.674(9) 0.33(12) Uiso 1 1 d D . . . .
O16 O 0.7880(5) 0.7010(4) 0.6779(3) 0.0721(18) Uani 1 1 d D . . . .
H16 H 0.808(6) 0.7595(11) 0.702(3) 0.108 Uiso 1 1 d DR . . . .
O17 O 0.6003(5) 0.0786(5) 0.8264(3) 0.0741(18) Uani 1 1 d . . . . .
O18 O 0.7117(6) 0.0009(5) 0.7722(4) 0.100(3) Uani 1 1 d . . . . .
O20 O 0.4168(5) 0.0470(5) 0.7500(4) 0.110(3) Uani 1 1 d D U . . .
H20 H 0.361(2) 0.052(3) 0.731(4) 0.166 Uiso 1 1 d DR . . . .
N1 N 0.9214(4) 0.3141(5) 0.8339(3) 0.0459(16) Uani 1 1 d . . . . .
N2 N 0.9504(4) 0.4130(5) 0.8528(3) 0.0483(16) Uani 1 1 d . . . . .
N3 N 0.7404(4) 0.3566(4) 0.8727(3) 0.0452(16) Uani 1 1 d . . . . .
N4 N 0.9684(5) 0.3853(5) 0.5988(4) 0.0591(19) Uani 1 1 d . . . . .
N5 N 1.0432(5) 0.3576(6) 0.7207(3) 0.0574(18) Uani 1 1 d . . . . .
N6 N 1.0386(5) 0.4668(6) 0.6130(4) 0.0588(19) Uani 1 1 d . . . . .
N7 N 0.7562(5) 0.4492(5) 0.8657(3) 0.0493(17) Uani 1 1 d . . . . .
N8 N 1.0827(5) 0.4534(6) 0.7439(3) 0.0576(19) Uani 1 1 d . . . . .
N9 N 0.5088(5) 0.3462(6) 0.8343(3) 0.068(2) Uani 1 1 d . . . . .
H9 H 0.5440 0.3642 0.8081 0.082 Uiso 1 1 calc R . . . .
N10 N 0.4919(6) 0.2505(6) 0.8365(4) 0.072(2) Uani 1 1 d . . . . .
C2 C 0.4832(7) 0.2402(6) 0.6593(4) 0.053(2) Uani 1 1 d . . . . .
C2AA C 0.3157(2) 0.3762(2) 0.56768(16) 0.0818(9) Uani 0.267(5) 1 d . . P A 3
H2AA H 0.3018 0.4120 0.5390 0.098 Uiso 0.267(5) 1 calc R . P A 3
C3 C 0.5530(4) 0.3642(4) 0.4478(2) 0.0966(10) Uani 0.638(5) 1 d . . P C 5
H3 H 0.5153 0.3863 0.4185 0.116 Uiso 0.638(5) 1 calc R . P C 5
C3AA C 0.7603(4) -0.1195(3) 0.9403(2) 0.1368(18) Uani 0.250(7) 1 d . . P B 2
H3AA H 0.8011 -0.1587 0.9547 0.164 Uiso 0.250(7) 1 calc R . P B 2
C4 C 0.4046(6) 0.2820(5) 0.6316(4) 0.049(2) Uani 1 1 d . . . . .
C4AA C 0.2467(4) 0.3366(4) 0.6180(3) 0.0818(9) Uani 0.733(5) 1 d . . P A 4
H4AA H 0.1829 0.3465 0.6245 0.098 Uiso 0.733(5) 1 calc R . P A 4
C0AA C 1.0865(7) 0.8871(6) 0.9786(4) 0.1142(19) Uani 0.784(11) 1 d . . P D 9
H0AA H 1.1171 0.9084 1.0212 0.137 Uiso 0.784(11) 1 calc R . P D 9
C5AA C 0.5604(3) 0.2531(3) 0.44616(18) 0.0966(10) Uani 0.362(5) 1 d . . P C 6
H5AA H 0.5299 0.1943 0.4163 0.116 Uiso 0.362(5) 1 calc R . P C 6
C6 C 0.3128(6) 0.2818(7) 0.6497(4) 0.073(3) Uani 1 1 d . . . . .
H6A H 0.2929 0.2502 0.6793 0.088 Uiso 0.267(5) 1 calc R . P A 3
H6B H 0.2929 0.2502 0.6793 0.088 Uiso 0.733(5) 1 calc R . P A 4
C6AA C 0.4438(4) 0.6505(4) 0.7286(2) 0.091(2) Uani 0.547(11) 1 d . . P E 8
H6AA H 0.3789 0.6545 0.7157 0.109 Uiso 0.547(11) 1 calc R . P E 8
C7 C 0.5368(4) 0.7433(3) 0.7674(3) 0.091(2) Uani 0.453(11) 1 d . . P E 7
H7 H 0.5370 0.8113 0.7820 0.109 Uiso 0.453(11) 1 calc R . P E 7
C5 C 1.0869(3) 0.9524(2) 0.92122(17) 0.1142(19) Uani 0.216(11) 1 d . . P D 10
H5 H 1.1156 1.0153 0.9229 0.137 Uiso 0.216(11) 1 calc R . P D 10
C8 C 0.4155(6) 0.3308(6) 0.5856(4) 0.063(2) Uani 1 1 d . . . . .
H8A H 0.4724 0.3373 0.5670 0.076 Uiso 0.267(5) 1 calc R . P A 3
H8B H 0.4724 0.3373 0.5670 0.076 Uiso 0.733(5) 1 calc R . P A 4
C8AA C 0.8696(3) -0.1097(3) 0.5111(2) 0.1325(14) Uani 0.136(7) 1 d . . P F 12
H8AA H 0.9086 -0.1528 0.4884 0.159 Uiso 0.136(7) 1 calc R . P F 12
C9 C 0.6716(7) -0.0710(6) 0.9703(4) 0.1368(18) Uani 0.750(7) 1 d . . P B 1
H9A H 0.6462 -0.0775 1.0072 0.164 Uiso 0.750(7) 1 calc R . P B 1
C10 C 0.7384(5) 0.4095(6) 0.6008(4) 0.047(2) Uani 1 1 d . . . . .
C11 C 0.7540(8) -0.1231(7) 0.5167(5) 0.1325(14) Uani 0.864(7) 1 d . . P F 11
H11 H 0.7097 -0.1797 0.4962 0.159 Uiso 0.864(7) 1 calc R . P F 11
C12 C 0.6660(5) 0.3703(6) 0.5418(4) 0.050(2) Uani 1 1 d . . . . .
C13 C 0.6381(6) 0.2719(7) 0.5128(4) 0.069(3) Uani 1 1 d . . . . .
H13 H 0.6596 0.2221 0.5281 0.082 Uiso 0.638(5) 1 calc R . P C 5
H13A H 0.6596 0.2221 0.5281 0.082 Uiso 0.362(5) 1 calc R . P C 6
C14 C 0.6218(6) 0.4272(6) 0.5084(4) 0.059(2) Uani 1 1 d . . . . .
H14 H 0.6326 0.4959 0.5213 0.070 Uiso 0.638(5) 1 calc R . P C 5
H14A H 0.6326 0.4959 0.5213 0.070 Uiso 0.362(5) 1 calc R . P C 6
C15 C 0.6614(6) 0.5059(6) 0.7440(4) 0.047(2) Uani 1 1 d . . . . .
C16 C 0.5942(6) 0.5800(6) 0.7441(4) 0.0457(19) Uani 1 1 d . . . . .
C17 C 0.4964(6) 0.5579(6) 0.7205(4) 0.062(2) Uani 1 1 d . . . . .
H17 H 0.4649 0.4937 0.7015 0.074 Uiso 0.453(11) 1 calc R . P E 7
H17A H 0.4649 0.4937 0.7015 0.074 Uiso 0.547(11) 1 calc R . P E 8
C18 C 0.6224(7) 0.6796(7) 0.7713(4) 0.075(3) Uani 1 1 d . . . . .
H18 H 0.6858 0.7072 0.7903 0.090 Uiso 0.453(11) 1 calc R . P E 7
H18A H 0.6858 0.7072 0.7903 0.090 Uiso 0.547(11) 1 calc R . P E 8
C19 C 0.9325(6) 0.6918(6) 0.8358(4) 0.056(2) Uani 1 1 d . . . . .
C20 C 0.9913(6) 0.7807(6) 0.8803(4) 0.060(2) Uani 1 1 d . . . . .
C21 C 1.0193(8) 0.8639(6) 0.8640(5) 0.086(3) Uani 1 1 d . . . . .
H21 H 1.0011 0.8699 0.8231 0.103 Uiso 0.784(11) 1 calc R . P D 9
H21A H 1.0011 0.8699 0.8231 0.103 Uiso 0.216(11) 1 calc R . P D 10
C22 C 1.0282(8) 0.7932(7) 0.9451(4) 0.084(3) Uani 1 1 d . . . . .
H22 H 1.0158 0.7442 0.9650 0.101 Uiso 0.784(11) 1 calc R . P D 9
H22A H 1.0158 0.7442 0.9650 0.101 Uiso 0.216(11) 1 calc R . P D 10
C23 C 0.6654(8) 0.0223(7) 0.8188(5) 0.072(3) Uani 1 1 d . . . . .
C24 C 0.6862(8) -0.0225(7) 0.8728(5) 0.076(3) Uani 1 1 d . . . . .
C25 C 0.7593(8) -0.0796(7) 0.8753(5) 0.086(3) Uani 1 1 d . . . . .
H25 H 0.8024 -0.0940 0.8448 0.104 Uiso 0.750(7) 1 calc R . P B 1
H25A H 0.8024 -0.0940 0.8448 0.104 Uiso 0.250(7) 1 calc R . P B 2
C26 C 0.6350(10) -0.0099(8) 0.9252(6) 0.114(4) Uani 1 1 d . . . . .
H26 H 0.5856 0.0295 0.9327 0.137 Uiso 0.750(7) 1 calc R . P B 1
H26A H 0.5856 0.0295 0.9327 0.137 Uiso 0.250(7) 1 calc R . P B 2
C27 C 0.8121(7) 0.1410(6) 0.6239(4) 0.053(2) Uani 1 1 d . . . . .
C28 C 0.8127(8) 0.0406(7) 0.5819(4) 0.069(3) Uani 1 1 d . . . . .
C29 C 0.8962(8) 0.0075(7) 0.5595(5) 0.094(3) Uani 1 1 d . . . . .
H29 H 0.9580 0.0445 0.5696 0.113 Uiso 0.864(7) 1 calc R . P F 11
H29A H 0.9580 0.0445 0.5696 0.113 Uiso 0.136(7) 1 calc R . P F 12
C30 C 0.7313(8) -0.0320(7) 0.5591(5) 0.096(3) Uani 1 1 d . . . . .
H30 H 0.6691 -0.0229 0.5699 0.115 Uiso 0.864(7) 1 calc R . P F 11
H30A H 0.6691 -0.0229 0.5699 0.115 Uiso 0.136(7) 1 calc R . P F 12
C31 C 0.3988(12) 0.1674(10) 0.9007(7) 0.189(8) Uani 1 1 d . . . . .
H31A H 0.3975 0.1090 0.8650 0.284 Uiso 1 1 calc GR . . . .
H31B H 0.3341 0.1728 0.9119 0.284 Uiso 1 1 calc GR . . . .
H31C H 0.4410 0.1633 0.9373 0.284 Uiso 1 1 calc GR . . . .
C32 C 0.4356(9) 0.2548(10) 0.8823(6) 0.110(4) Uani 1 1 d . . . . .
C33 C 0.4146(9) 0.3482(10) 0.9077(6) 0.121(5) Uani 1 1 d . . . . .
H33 H 0.3744 0.3681 0.9394 0.145 Uiso 1 1 calc R . . . .
C34 C 0.4645(8) 0.4082(9) 0.8771(5) 0.086(3) Uani 1 1 d . . . . .
C35 C 0.4769(7) 0.5167(8) 0.8862(5) 0.097(3) Uani 1 1 d . . . . .
H35A H 0.5343 0.5480 0.9164 0.145 Uiso 1 1 calc GR . . . .
H35B H 0.4208 0.5434 0.9027 0.145 Uiso 1 1 calc GR . . . .
H35C H 0.4837 0.5286 0.8454 0.145 Uiso 1 1 calc GR . . . .
C36 C 0.9108(7) 0.2422(7) 0.5037(4) 0.078(3) Uani 1 1 d . . . . .
H36A H 0.9250 0.1926 0.5239 0.117 Uiso 1 1 calc GR . . . .
H36B H 0.9219 0.2210 0.4592 0.117 Uiso 1 1 calc GR . . . .
H36C H 0.8438 0.2522 0.5058 0.117 Uiso 1 1 calc GR . . . .
C37 C 0.9748(6) 0.3356(7) 0.5377(5) 0.060(2) Uani 1 1 d . . . . .
C38 C 1.0468(7) 0.3844(8) 0.5132(5) 0.071(3) Uani 1 1 d . . . . .
H38 H 1.0656 0.3637 0.4721 0.085 Uiso 1 1 calc R . . . .
C39 C 1.0836(6) 0.4669(8) 0.5604(5) 0.067(3) Uani 1 1 d . . . . .
C40 C 1.1598(7) 0.5531(7) 0.5629(5) 0.091(3) Uani 1 1 d . . . . .
H40A H 1.1325 0.6137 0.5759 0.136 Uiso 1 1 calc GR . . . .
H40B H 1.1798 0.5445 0.5208 0.136 Uiso 1 1 calc GR . . . .
H40C H 1.2154 0.5555 0.5935 0.136 Uiso 1 1 calc GR . . . .
C41 C 1.0426(6) 0.5498(7) 0.6682(4) 0.059(2) Uani 1 1 d . . . . .
H41 H 1.1076 0.5884 0.6759 0.070 Uiso 1 1 calc R . . . .
C42 C 1.0234(5) 0.5249(6) 0.7294(4) 0.051(2) Uani 1 1 d . . . . .
H42 H 1.0391 0.5861 0.7654 0.062 Uiso 1 1 calc R . . . .
C43 C 1.2289(7) 0.5646(9) 0.8079(6) 0.122(5) Uani 1 1 d . . . . .
H43A H 1.2413 0.5955 0.7750 0.183 Uiso 1 1 calc GR . . . .
H43B H 1.2898 0.5574 0.8297 0.183 Uiso 1 1 calc GR . . . .
H43C H 1.1934 0.6048 0.8385 0.183 Uiso 1 1 calc GR . . . .
C44 C 1.1709(7) 0.4662(9) 0.7778(5) 0.073(3) Uani 1 1 d . . . . .
C45 C 1.1879(7) 0.3743(9) 0.7783(5) 0.084(3) Uani 1 1 d . . . . .
H45 H 1.2426 0.3584 0.7993 0.100 Uiso 1 1 calc R . . . .
C46 C 1.1073(7) 0.3078(8) 0.7410(5) 0.074(3) Uani 1 1 d . . . . .
C47 C 1.0920(7) 0.1985(7) 0.7244(5) 0.086(3) Uani 1 1 d . . . . .
H47A H 1.0258 0.1763 0.7281 0.129 Uiso 1 1 calc GR . . . .
H47B H 1.1357 0.1780 0.7534 0.129 Uiso 1 1 calc GR . . . .
H47C H 1.1046 0.1705 0.6807 0.129 Uiso 1 1 calc GR . . . .
C48 C 1.0759(7) 0.5293(7) 0.9328(5) 0.093(3) Uani 1 1 d . . . . .
H48A H 1.1450 0.5286 0.9334 0.140 Uiso 1 1 calc GR . . . .
H48B H 1.0610 0.5513 0.9764 0.140 Uiso 1 1 calc GR . . . .
H48C H 1.0556 0.5735 0.9096 0.140 Uiso 1 1 calc GR . . . .
C49 C 1.0244(6) 0.4294(7) 0.9007(4) 0.059(2) Uani 1 1 d . . . . .
C50 C 1.0392(7) 0.3409(7) 0.9124(4) 0.068(3) Uani 1 1 d . . . . .
H50 H 1.0857 0.3327 0.9435 0.082 Uiso 1 1 calc R . . . .
C51 C 0.9740(7) 0.2693(7) 0.8708(4) 0.060(2) Uani 1 1 d . . . . .
C52 C 0.9531(7) 0.1602(6) 0.8612(4) 0.081(3) Uani 1 1 d . . . . .
H52A H 0.8858 0.1429 0.8651 0.121 Uiso 1 1 calc GR . . . .
H52B H 0.9939 0.1431 0.8935 0.121 Uiso 1 1 calc GR . . . .
H52C H 0.9664 0.1247 0.8189 0.121 Uiso 1 1 calc GR . . . .
C53 C 0.8332(5) 0.2742(5) 0.7865(3) 0.0421(19) Uani 1 1 d . . . . .
H53 H 0.8403 0.2083 0.7591 0.051 Uiso 1 1 calc R . . . .
C54 C 0.7403(6) 0.2678(5) 0.8184(4) 0.049(2) Uani 1 1 d . . . . .
H54 H 0.7399 0.2116 0.8359 0.059 Uiso 1 1 calc R . . . .
C55 C 0.6906(7) 0.2724(7) 0.9544(4) 0.083(3) Uani 1 1 d . . . . .
H55A H 0.6387 0.2263 0.9256 0.124 Uiso 1 1 calc GR . . . .
H55B H 0.6716 0.2934 0.9970 0.124 Uiso 1 1 calc GR . . . .
H55C H 0.7483 0.2412 0.9559 0.124 Uiso 1 1 calc GR . . . .
C56 C 0.7109(6) 0.3599(7) 0.9305(4) 0.059(2) Uani 1 1 d . . . . .
C57 C 0.7067(6) 0.4577(7) 0.9610(4) 0.063(2) Uani 1 1 d . . . . .
H57 H 0.6877 0.4833 1.0017 0.075 Uiso 1 1 calc R . . . .
C58 C 0.7355(6) 0.5112(6) 0.9208(4) 0.056(2) Uani 1 1 d . . . . .
C59 C 0.7436(7) 0.6203(6) 0.9318(4) 0.071(3) Uani 1 1 d . . . . .
H59A H 0.8112 0.6484 0.9408 0.106 Uiso 1 1 calc GR . . . .
H59B H 0.7106 0.6493 0.9680 0.106 Uiso 1 1 calc GR . . . .
H59C H 0.7141 0.6332 0.8938 0.106 Uiso 1 1 calc GR . . . .
C60 C 0.4197(10) -0.0593(10) 0.7439(8) 0.165(4) Uani 1 1 d D U . . .
H60A H 0.4012 -0.0979 0.6995 0.248 Uiso 1 1 calc GR . . . .
H60B H 0.3751 -0.0802 0.7701 0.248 Uiso 1 1 calc GR . . . .
H60C H 0.4847 -0.0683 0.7582 0.248 Uiso 1 1 calc GR . . . .
C61 C 0.7201(9) 0.7037(8) 0.6268(5) 0.127(5) Uani 1 1 d D . . . .
H61A H 0.7004 0.7683 0.6358 0.190 Uiso 1 1 calc GR . . . .
H61B H 0.6640 0.6554 0.6221 0.190 Uiso 1 1 calc GR . . . .
H61C H 0.7492 0.6893 0.5875 0.190 Uiso 1 1 calc GR . . . .
O19 O 0.8517(7) 0.8907(5) 0.7345(4) 0.103(2) Uani 1 1 d . . . . .
H19 H 0.8115 0.9266 0.7485 0.155 Uiso 1 1 calc GR . . . .
C62 C 0.9049(13) 0.9312(12) 0.6978(8) 0.190(7) Uani 1 1 d . . . . .
H62A H 0.8628 0.9377 0.6620 0.285 Uiso 1 1 calc GR . . . .
H62B H 0.9525 0.8896 0.6818 0.285 Uiso 1 1 calc GR . . . .
H62C H 0.9375 0.9952 0.7234 0.285 Uiso 1 1 calc GR . . . .


_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 2.024(5) . ?
Ni1 O2 2.099(5) . ?
Ni1 O7 2.069(5) . ?
Ni1 O13 2.015(5) . ?
Ni1 N2 2.077(6) . ?
Ni1 N7 2.083(6) . ?
Ni2 O1 2.038(5) . ?
Ni2 O3 2.103(5) . ?
Ni2 O4 2.010(5) . ?
Ni2 O5 2.090(5) . ?
Ni2 O6 2.043(5) . ?
Ni2 O12 1.991(5) . ?
Ni3 O1 2.077(5) . ?
Ni3 O2 2.014(5) . ?
Ni3 O3 2.077(5) . ?
Ni3 O9 1.990(6) . ?
Ni3 N4 2.090(7) . ?
Ni3 N5 2.070(7) . ?
Ni4 O2 2.047(5) . ?
Ni4 O7 2.066(5) . ?
Ni4 O8 2.026(5) . ?
Ni4 O10 1.993(6) . ?
Ni4 O11 2.096(5) . ?
Ni4 O16 2.018(5) . ?
Ni5 O4 2.025(5) . ?
Ni5 O14 2.016(5) . ?
Ni5 O15 2.089(7) . ?
Ni5 O17 2.044(6) . ?
Ni5 O20 2.072(7) . ?
Ni5 N10 2.064(8) . ?
S1 C2AA 1.694(6) . ?
S1 C6 1.506(9) . ?
S2 C3AA 1.582(11) . ?
S2 C26 1.570(12) . ?
S3 C3 1.587(7) . ?
S3 C13 1.659(9) . ?
S4 C4AA 1.694(6) . ?
S4 C8 1.650(9) . ?
S5 C0AA 1.755(8) . ?
S5 C21 1.628(9) . ?
S6 C5AA 1.587(7) . ?
S6 C14 1.535(9) . ?
S7 C7 1.709(7) . ?
S7 C17 1.551(9) . ?
S8 C6AA 1.709(7) . ?
S8 C18 1.581(9) . ?
S9 C9 1.582(11) . ?
S9 C25 1.665(10) . ?
S10 C5 1.755(8) . ?
S10 C22 1.443(11) . ?
S11 C11 1.617(11) . ?
S11 C29 1.682(10) . ?
S12 C8AA 1.617(11) . ?
S12 C30 1.447(12) . ?
O1 C53 1.407(7) . ?
O2 C42 1.376(8) . ?
O3 C10 1.267(8) . ?
O4 C54 1.367(8) . ?
O5 C15 1.242(9) . ?
O6 C27 1.260(9) . ?
O7 C15 1.273(9) . ?
O8 C10 1.236(8) . ?
O9 C27 1.242(9) . ?
O10 C19 1.247(9) . ?
O11 C41 1.431(9) . ?
O12 C2 1.233(9) . ?
O13 C19 1.267(9) . ?
O14 C2 1.251(9) . ?
O16 C61 1.398(10) . ?
O17 C23 1.264(11) . ?
O18 C23 1.236(11) . ?
O20 C60 1.488(14) . ?
N1 N2 1.355(8) . ?
N1 C51 1.365(9) . ?
N1 C53 1.471(9) . ?
N2 C49 1.341(9) . ?
N3 N7 1.368(8) . ?
N3 C54 1.465(9) . ?
N3 C56 1.348(9) . ?
N4 N6 1.376(9) . ?
N4 C37 1.333(10) . ?
N5 N8 1.347(9) . ?
N5 C46 1.315(10) . ?
N6 C39 1.354(10) . ?
N6 C41 1.416(10) . ?
N7 C58 1.348(9) . ?
N8 C42 1.459(9) . ?
N8 C44 1.333(10) . ?
N9 N10 1.373(9) . ?
N9 C34 1.335(11) . ?
N10 C32 1.316(11) . ?
C2 C4 1.458(10) . ?
C2AA C8 1.650(9) . ?
C3 C14 1.535(9) . ?
C3AA C25 1.665(10) . ?
C4 C6 1.371(11) . ?
C4 C8 1.380(10) . ?
C4AA C6 1.506(9) . ?
C0AA C22 1.443(11) . ?
C5AA C13 1.659(9) . ?
C6AA C17 1.551(9) . ?
C7 C18 1.581(9) . ?
C5 C21 1.628(9) . ?
C8AA C29 1.682(10) . ?
C9 C26 1.570(12) . ?
C10 C12 1.480(10) . ?
C11 C30 1.447(12) . ?
C12 C13 1.360(11) . ?
C12 C14 1.384(10) . ?
C15 C16 1.483(10) . ?
C16 C17 1.376(10) . ?
C16 C18 1.371(10) . ?
C19 C20 1.462(11) . ?
C20 C21 1.361(11) . ?
C20 C22 1.405(11) . ?
C23 C24 1.505(12) . ?
C24 C25 1.374(12) . ?
C24 C26 1.378(14) . ?
C27 C28 1.463(12) . ?
C28 C29 1.379(12) . ?
C28 C30 1.395(13) . ?
C31 C32 1.469(14) . ?
C32 C33 1.362(14) . ?
C33 C34 1.392(14) . ?
C34 C35 1.491(13) . ?
C36 C37 1.473(12) . ?
C37 C38 1.390(11) . ?
C38 C39 1.335(12) . ?
C39 C40 1.520(12) . ?
C41 C42 1.510(10) . ?
C43 C44 1.477(13) . ?
C44 C45 1.359(12) . ?
C45 C46 1.403(13) . ?
C46 C47 1.482(12) . ?
C48 C49 1.466(11) . ?
C49 C50 1.388(11) . ?
C50 C51 1.341(11) . ?
C51 C52 1.501(11) . ?
C53 C54 1.528(10) . ?
C55 C56 1.491(10) . ?
C56 C57 1.373(11) . ?
C57 C58 1.374(10) . ?
C58 C59 1.493(11) . ?
O19 C62 1.341(16) . ?

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 79.68(19) . . ?
O1 Ni1 O7 97.17(19) . . ?
O1 Ni1 N2 79.2(2) . . ?
O1 Ni1 N7 90.1(2) . . ?
O7 Ni1 O2 79.18(19) . . ?
O7 Ni1 N2 175.8(2) . . ?
O7 Ni1 N7 92.4(2) . . ?
O13 Ni1 O1 166.5(2) . . ?
O13 Ni1 O2 90.7(2) . . ?
O13 Ni1 O7 90.2(2) . . ?
O13 Ni1 N2 93.8(2) . . ?
O13 Ni1 N7 100.9(2) . . ?
N2 Ni1 O2 102.0(2) . . ?
N2 Ni1 N7 85.6(2) . . ?
N7 Ni1 O2 165.7(2) . . ?
O1 Ni2 O3 79.66(18) . . ?
O1 Ni2 O5 98.54(19) . . ?
O1 Ni2 O6 91.0(2) . . ?
O4 Ni2 O1 82.27(19) . . ?
O4 Ni2 O3 161.93(19) . . ?
O4 Ni2 O5 89.31(19) . . ?
O4 Ni2 O6 94.6(2) . . ?
O5 Ni2 O3 93.38(19) . . ?
O6 Ni2 O3 85.7(2) . . ?
O6 Ni2 O5 170.1(2) . . ?
O12 Ni2 O1 177.2(2) . . ?
O12 Ni2 O3 98.0(2) . . ?
O12 Ni2 O4 100.1(2) . . ?
O12 Ni2 O5 83.1(2) . . ?
O12 Ni2 O6 87.3(2) . . ?
O1 Ni3 N4 166.6(2) . . ?
O2 Ni3 O1 80.44(18) . . ?
O2 Ni3 O3 94.81(18) . . ?
O2 Ni3 N4 89.7(3) . . ?
O2 Ni3 N5 79.4(2) . . ?
O3 Ni3 O1 79.38(18) . . ?
O3 Ni3 N4 92.5(2) . . ?
O9 Ni3 O1 92.9(2) . . ?
O9 Ni3 O2 170.4(2) . . ?
O9 Ni3 O3 90.7(2) . . ?
O9 Ni3 N4 97.9(3) . . ?
O9 Ni3 N5 94.9(3) . . ?
N5 Ni3 O1 98.7(2) . . ?
N5 Ni3 O3 174.1(3) . . ?
N5 Ni3 N4 88.4(3) . . ?
O2 Ni4 O7 80.45(18) . . ?
O2 Ni4 O11 79.44(19) . . ?
O7 Ni4 O11 159.78(19) . . ?
O8 Ni4 O2 98.8(2) . . ?
O8 Ni4 O7 91.9(2) . . ?
O8 Ni4 O11 93.3(2) . . ?
O10 Ni4 O2 91.3(2) . . ?
O10 Ni4 O7 89.1(2) . . ?
O10 Ni4 O8 169.9(2) . . ?
O10 Ni4 O11 89.2(2) . . ?
O10 Ni4 O16 83.1(2) . . ?
O16 Ni4 O2 170.9(2) . . ?
O16 Ni4 O7 106.6(2) . . ?
O16 Ni4 O8 86.9(2) . . ?
O16 Ni4 O11 93.2(2) . . ?
O4 Ni5 O15 90.6(2) . . ?
O4 Ni5 O17 97.1(2) . . ?
O4 Ni5 O20 176.2(2) . . ?
O4 Ni5 N10 88.3(3) . . ?
O14 Ni5 O4 91.5(2) . . ?
O14 Ni5 O15 91.9(3) . . ?
O14 Ni5 O17 170.9(2) . . ?
O14 Ni5 O20 84.8(2) . . ?
O14 Ni5 N10 84.4(3) . . ?
O17 Ni5 O15 91.0(3) . . ?
O17 Ni5 O20 86.6(2) . . ?
O17 Ni5 N10 92.9(3) . . ?
O20 Ni5 O15 88.4(3) . . ?
N10 Ni5 O15 176.1(3) . . ?
N10 Ni5 O20 92.4(3) . . ?
C6 S1 C2AA 103.8(5) . . ?
C26 S2 C3AA 106.0(8) . . ?
C3 S3 C13 100.0(4) . . ?
C8 S4 C4AA 97.6(4) . . ?
C21 S5 C0AA 94.8(4) . . ?
C14 S6 C5AA 104.9(5) . . ?
C17 S7 C7 101.4(4) . . ?
C18 S8 C6AA 99.5(5) . . ?
C9 S9 C25 99.4(5) . . ?
C22 S10 C5 104.6(6) . . ?
C11 S11 C29 97.1(5) . . ?
C30 S12 C8AA 108.4(8) . . ?
Ni1 O1 Ni2 118.6(2) . . ?
Ni1 O1 Ni3 99.99(19) . . ?
Ni2 O1 Ni3 98.05(18) . . ?
C53 O1 Ni1 109.3(4) . . ?
C53 O1 Ni2 104.7(4) . . ?
C53 O1 Ni3 127.2(4) . . ?
Ni3 O2 Ni1 99.61(19) . . ?
Ni3 O2 Ni4 120.7(2) . . ?
Ni4 O2 Ni1 96.7(2) . . ?
C42 O2 Ni1 125.4(4) . . ?
C42 O2 Ni3 107.5(5) . . ?
C42 O2 Ni4 107.8(4) . . ?
Ni3 O3 Ni2 96.06(18) . . ?
C10 O3 Ni2 129.7(5) . . ?
C10 O3 Ni3 127.4(5) . . ?
Ni2 O4 Ni5 119.4(2) . . ?
C54 O4 Ni2 112.6(4) . . ?
C54 O4 Ni5 125.0(4) . . ?
C15 O5 Ni2 129.0(5) . . ?
C27 O6 Ni2 131.6(5) . . ?
Ni4 O7 Ni1 97.1(2) . . ?
C15 O7 Ni1 125.0(5) . . ?
C15 O7 Ni4 131.1(5) . . ?
C10 O8 Ni4 131.2(5) . . ?
C27 O9 Ni3 128.1(6) . . ?
C19 O10 Ni4 129.5(5) . . ?
C41 O11 Ni4 112.5(4) . . ?
C2 O12 Ni2 123.9(5) . . ?
C19 O13 Ni1 127.2(5) . . ?
C2 O14 Ni5 134.3(6) . . ?
C61 O16 Ni4 132.8(6) . . ?
C23 O17 Ni5 128.7(6) . . ?
C60 O20 Ni5 122.5(7) . . ?
N2 N1 C51 111.1(6) . . ?
N2 N1 C53 118.2(5) . . ?
C51 N1 C53 130.0(7) . . ?
N1 N2 Ni1 109.5(4) . . ?
C49 N2 Ni1 144.6(6) . . ?
C49 N2 N1 105.3(6) . . ?
N7 N3 C54 121.5(6) . . ?
C56 N3 N7 111.1(6) . . ?
C56 N3 C54 126.6(7) . . ?
N6 N4 Ni3 120.2(5) . . ?
C37 N4 Ni3 133.2(6) . . ?
C37 N4 N6 104.5(7) . . ?
N8 N5 Ni3 109.4(5) . . ?
C46 N5 Ni3 144.7(7) . . ?
C46 N5 N8 105.8(8) . . ?
N4 N6 C41 122.7(7) . . ?
C39 N6 N4 110.3(8) . . ?
C39 N6 C41 124.8(8) . . ?
N3 N7 Ni1 120.2(5) . . ?
C58 N7 Ni1 127.5(6) . . ?
C58 N7 N3 105.7(6) . . ?
N5 N8 C42 116.4(6) . . ?
C44 N8 N5 112.7(7) . . ?
C44 N8 C42 130.9(8) . . ?
C34 N9 N10 112.8(8) . . ?
N9 N10 Ni5 115.0(5) . . ?
C32 N10 Ni5 139.9(8) . . ?
C32 N10 N9 104.3(8) . . ?
O12 C2 O14 125.1(8) . . ?
O12 C2 C4 118.9(8) . . ?
O14 C2 C4 116.0(8) . . ?
C8 C2AA S1 97.6(4) . . ?
C14 C3 S3 104.9(5) . . ?
S2 C3AA C25 99.4(5) . . ?
C6 C4 C2 124.6(7) . . ?
C6 C4 C8 111.7(8) . . ?
C8 C4 C2 123.6(8) . . ?
C6 C4AA S4 103.8(5) . . ?
C22 C0AA S5 104.6(6) . . ?
S6 C5AA C13 100.0(4) . . ?
C4 C6 S1 114.8(7) . . ?
C4 C6 C4AA 114.8(7) . . ?
C17 C6AA S8 101.4(4) . . ?
C18 C7 S7 99.5(5) . . ?
C21 C5 S10 94.8(4) . . ?
C4 C8 S4 112.0(7) . . ?
C4 C8 C2AA 112.0(7) . . ?
S12 C8AA C29 97.1(5) . . ?
C26 C9 S9 106.0(8) . . ?
O3 C10 C12 119.0(7) . . ?
O8 C10 O3 123.9(7) . . ?
O8 C10 C12 117.1(7) . . ?
C30 C11 S11 108.4(8) . . ?
C13 C12 C10 122.7(7) . . ?
C13 C12 C14 112.1(8) . . ?
C14 C12 C10 125.2(8) . . ?
C12 C13 S3 110.5(7) . . ?
C12 C13 C5AA 110.5(7) . . ?
C12 C14 S6 112.5(7) . . ?
C12 C14 C3 112.5(7) . . ?
O5 C15 O7 124.2(7) . . ?
O5 C15 C16 118.3(7) . . ?
O7 C15 C16 117.5(7) . . ?
C17 C16 C15 124.9(8) . . ?
C18 C16 C15 122.9(8) . . ?
C18 C16 C17 112.1(7) . . ?
C16 C17 S7 113.5(7) . . ?
C16 C17 C6AA 113.5(7) . . ?
C16 C18 S8 113.5(7) . . ?
C16 C18 C7 113.5(7) . . ?
O10 C19 O13 127.4(8) . . ?
O10 C19 C20 115.6(8) . . ?
O13 C19 C20 117.0(8) . . ?
C21 C20 C19 124.0(8) . . ?
C21 C20 C22 109.9(8) . . ?
C22 C20 C19 126.1(8) . . ?
C20 C21 S5 115.2(7) . . ?
C20 C21 C5 115.2(7) . . ?
C20 C22 S10 115.5(8) . . ?
C20 C22 C0AA 115.5(8) . . ?
O17 C23 C24 115.1(10) . . ?
O18 C23 O17 126.6(9) . . ?
O18 C23 C24 118.3(10) . . ?
C25 C24 C23 123.3(11) . . ?
C25 C24 C26 112.9(10) . . ?
C26 C24 C23 123.8(10) . . ?
C24 C25 S9 110.8(9) . . ?
C24 C25 C3AA 110.8(9) . . ?
C24 C26 S2 110.7(10) . . ?
C24 C26 C9 110.7(10) . . ?
O6 C27 C28 117.1(9) . . ?
O9 C27 O6 124.7(8) . . ?
O9 C27 C28 118.1(9) . . ?
C29 C28 C27 122.6(10) . . ?
C29 C28 C30 111.9(9) . . ?
C30 C28 C27 125.5(9) . . ?
C28 C29 S11 109.8(8) . . ?
C28 C29 C8AA 109.8(8) . . ?
C28 C30 S12 112.8(10) . . ?
C28 C30 C11 112.8(10) . . ?
N10 C32 C31 122.7(12) . . ?
N10 C32 C33 111.4(10) . . ?
C33 C32 C31 125.9(11) . . ?
C32 C33 C34 107.2(10) . . ?
N9 C34 C33 104.3(10) . . ?
N9 C34 C35 122.4(10) . . ?
C33 C34 C35 133.3(11) . . ?
N4 C37 C36 121.7(8) . . ?
N4 C37 C38 110.9(9) . . ?
C38 C37 C36 127.4(10) . . ?
C39 C38 C37 106.3(9) . . ?
N6 C39 C40 120.1(10) . . ?
C38 C39 N6 107.9(9) . . ?
C38 C39 C40 132.0(9) . . ?
O11 C41 C42 106.3(7) . . ?
N6 C41 O11 110.8(7) . . ?
N6 C41 C42 114.7(7) . . ?
O2 C42 N8 109.4(6) . . ?
O2 C42 C41 110.4(6) . . ?
N8 C42 C41 113.6(7) . . ?
N8 C44 C43 122.7(9) . . ?
N8 C44 C45 105.4(9) . . ?
C45 C44 C43 131.8(9) . . ?
C44 C45 C46 106.9(9) . . ?
N5 C46 C45 109.2(9) . . ?
N5 C46 C47 122.6(10) . . ?
C45 C46 C47 128.3(9) . . ?
N2 C49 C48 121.0(7) . . ?
N2 C49 C50 109.7(8) . . ?
C50 C49 C48 129.3(8) . . ?
C51 C50 C49 107.4(8) . . ?
N1 C51 C52 121.4(8) . . ?
C50 C51 N1 106.4(8) . . ?
C50 C51 C52 132.1(7) . . ?
O1 C53 N1 107.4(6) . . ?
O1 C53 C54 108.6(6) . . ?
N1 C53 C54 112.8(6) . . ?
O4 C54 N3 114.2(6) . . ?
O4 C54 C53 108.9(6) . . ?
N3 C54 C53 111.0(6) . . ?
N3 C56 C55 124.8(8) . . ?
N3 C56 C57 106.0(7) . . ?
C57 C56 C55 129.2(8) . . ?
C56 C57 C58 107.8(8) . . ?
N7 C58 C57 109.3(8) . . ?
N7 C58 C59 122.1(7) . . ?
C57 C58 C59 128.5(8) . . ?

_platon_squeeze_details          TITL
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 1.000 0.500 617 171 ' '


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ni6b
_database_code_depnum_ccdc_archive 'CCDC 2026738'
loop_
_audit_author_name
_audit_author_address
'Di Sun'
;Shandong university
China
;
_audit_update_record             
;
2020-09-01 deposited with the CCDC.	2021-02-24 downloaded from the CCDC.
;
_audit_creation_date             2020-01-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C82 H94 N14 Ni6 O24, 4(C2 H3 N)'
_chemical_formula_sum            'C90 H106 N18 Ni6 O24'
_chemical_formula_weight         2176.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         NiCHON
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   32.6272(4)
_cell_length_b                   13.8653(2)
_cell_length_c                   23.2676(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.7600(10)
_cell_angle_gamma                90
_cell_volume                     9966.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13269
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3520
_cell_measurement_theta_min      3.9730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4528
_exptl_crystal_recrystallization_method 173(K)
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25662
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.494
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00  27.00   1.00    0.20    --  -48.32  19.00-150.00   81
  2  ω    -56.00 -13.00   1.00    0.80    --  -86.25  95.00-103.00   43
  3  ω    -79.00  17.00   1.00    0.20    --  -48.32  95.00-103.00   96
  4  ω    102.00 133.00   1.00    0.80    --  107.75  95.00-103.00   31
  5  ω     37.00 120.00   1.00    0.80    --  107.75 -37.00   0.00   83
  6  ω     35.00 121.00   1.00    0.80    --  107.75 -19.00 -30.00   86
  7  ω     36.00 118.00   1.00    0.80    --  107.75 -37.00 150.00   82
  8  ω     35.00 120.00   1.00    0.80    --  107.75 -57.00 150.00   85
  9  ω     44.00 103.00   1.00    0.80    --  107.75 -95.00 146.00   59
 10  ω   -143.00-118.00   1.00    0.80    --  -86.25 -95.00 146.00   25
 11  ω   -111.00 -71.00   1.00    0.20    --  -48.32-125.00 -60.00   40
 12  ω   -157.00-107.00   1.00    0.80    --  -86.25 -99.00 -90.00   50
 13  ω     53.00  78.00   1.00    0.20    --   48.32 -95.00 146.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0193929000
_diffrn_orient_matrix_UB_12      0.0962130000
_diffrn_orient_matrix_UB_13      0.0295927000
_diffrn_orient_matrix_UB_21      -0.0005053000
_diffrn_orient_matrix_UB_22      0.0384385000
_diffrn_orient_matrix_UB_23      -0.0623688000
_diffrn_orient_matrix_UB_31      -0.0459228000
_diffrn_orient_matrix_UB_32      0.0401378000
_diffrn_orient_matrix_UB_33      -0.0112133000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7441
_reflns_number_total             8753
_reflns_odcompleteness_completeness 98.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8753
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0438
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0636P)²+17.5482P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1278
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C30(H30), C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C9(H9), C17(H17), C34(H34), C12(H12), C10(H10), C18(H18), C11(H11),
 C6(H6), C3(H3A), C19(H19), C39(H39), C20(H20), C1(H1), C2(H2), C27(H27)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C32(H32A,H32B,H32C), C7(H7A,H7B,H7C), C14(H14A,H14B,
 H14C), C41(H41A,H41B,H41C), C37(H37A,H37B,H37C), C25(H25A,H25B,H25C), C29(H29A,
 H29B,H29C), C22(H22A,H22B,H22C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
;
_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 0.51419(2) 0.68437(3) 0.19160(2) 0.02245(12) Uani 1 1 d . . . . .
Ni2 Ni 0.56680(2) 0.81670(3) 0.32444(2) 0.02566(13) Uani 1 1 d . . . . .
Ni3 Ni 0.67920(2) 0.80562(3) 0.36932(2) 0.03129(13) Uani 1 1 d . . . . .
O4 O 0.49855(5) 0.83129(12) 0.17986(7) 0.0231(3) Uani 1 1 d . . . . .
O10 O 0.54201(5) 0.68858(11) 0.28382(7) 0.0224(3) Uani 1 1 d . . . . .
O11 O 0.62169(5) 0.76071(13) 0.31521(7) 0.0256(4) Uani 1 1 d . . . . .
O5 O 0.48102(5) 0.66011(13) 0.10301(8) 0.0279(4) Uani 1 1 d . . . . .
O6 O 0.42221(5) 0.75140(12) 0.09171(7) 0.0263(4) Uani 1 1 d . . . . .
O3 O 0.55719(5) 0.89600(13) 0.24648(7) 0.0273(4) Uani 1 1 d . . . . .
O2 O 0.59056(6) 0.93705(13) 0.37136(8) 0.0300(4) Uani 1 1 d . . . . .
O7 O 0.72147(6) 0.68294(16) 0.37704(9) 0.0414(5) Uani 1 1 d . . . . .
O1W O 0.66463(7) 0.7441(2) 0.44122(10) 0.0462(6) Uani 1 1 d . . . . .
O1 O 0.66163(7) 0.93674(17) 0.38785(11) 0.0480(6) Uani 1 1 d . . . . .
N5 N 0.57508(7) 0.70701(16) 0.18162(9) 0.0259(4) Uani 1 1 d . . . . .
O9 O 0.74359(7) 0.80983(18) 0.43184(9) 0.0460(5) Uani 1 1 d . . . . .
N2 N 0.56296(7) 0.53448(16) 0.26638(10) 0.0300(5) Uani 1 1 d . . . . .
N1 N 0.53166(7) 0.53954(16) 0.21158(10) 0.0305(5) Uani 1 1 d . . . . .
N6 N 0.61169(7) 0.67033(16) 0.22469(9) 0.0282(5) Uani 1 1 d . . . . .
N4 N 0.69211(7) 0.85862(18) 0.29414(11) 0.0351(5) Uani 1 1 d . . . . .
O8 O 0.78686(7) 0.6861(2) 0.44145(10) 0.0566(7) Uani 1 1 d . . . . .
N3 N 0.65675(7) 0.88845(18) 0.24843(11) 0.0363(5) Uani 1 1 d . . . . .
H3 H 0.6301 0.8847 0.2496 0.044 Uiso 1 1 calc R . . . .
N7 N 0.75153(8) 0.7254(2) 0.41758(10) 0.0436(6) Uani 1 1 d . . . . .
C16 C 0.52580(7) 0.89979(17) 0.19848(10) 0.0227(5) Uani 1 1 d . . . . .
C15 C 0.52023(8) 0.98761(18) 0.15926(11) 0.0261(5) Uani 1 1 d . . . . .
C30 C 0.57607(8) 0.62339(18) 0.30058(11) 0.0260(5) Uani 1 1 d . . . . .
H30 H 0.5832 0.6088 0.3448 0.031 Uiso 1 1 calc R . . . .
C8 C 0.44559(8) 0.69707(17) 0.07157(11) 0.0249(5) Uani 1 1 d . . . . .
C35 C 0.58596(9) 0.7168(2) 0.13106(11) 0.0303(5) Uani 1 1 d . . . . .
C31 C 0.61612(8) 0.66945(19) 0.28994(11) 0.0274(5) Uani 1 1 d . . . . .
H31 H 0.6421 0.6298 0.3118 0.033 Uiso 1 1 calc R . . . .
C13 C 0.54090(9) 1.0758(2) 0.18144(12) 0.0332(6) Uani 1 1 d . . . . .
C9 C 0.49501(8) 0.97940(19) 0.09844(11) 0.0303(5) Uani 1 1 d . . . . .
H9 H 0.4808 0.9202 0.0840 0.036 Uiso 1 1 calc R . . . .
C24 C 0.62763(9) 0.9725(2) 0.39229(12) 0.0323(6) Uani 1 1 d . . . . .
C23 C 0.63132(9) 1.0684(2) 0.42442(12) 0.0343(6) Uani 1 1 d . . . . .
C33 C 0.64406(9) 0.6579(2) 0.20056(12) 0.0335(6) Uani 1 1 d . . . . .
C4 C 0.42844(8) 0.6712(2) 0.00530(12) 0.0326(6) Uani 1 1 d . . . . .
C17 C 0.59514(10) 1.1274(2) 0.40840(12) 0.0369(6) Uani 1 1 d . . . . .
H17 H 0.5693 1.1055 0.3790 0.044 Uiso 1 1 calc R . . . .
C34 C 0.62830(9) 0.6871(2) 0.14105(12) 0.0360(6) Uani 1 1 d . . . . .
H34 H 0.6434 0.6869 0.1123 0.043 Uiso 1 1 calc R . . . .
C36 C 0.55473(9) 0.7537(2) 0.07299(12) 0.0360(6) Uani 1 1 d . . . . .
H36A H 0.5380 0.6998 0.0497 0.054 Uiso 1 1 calc GR . . . .
H36B H 0.5707 0.7855 0.0491 0.054 Uiso 1 1 calc GR . . . .
H36C H 0.5350 0.8002 0.0821 0.054 Uiso 1 1 calc GR . . . .
C5 C 0.40345(9) 0.7343(2) -0.03943(12) 0.0369(6) Uani 1 1 d . . . . .
C12 C 0.53573(10) 1.1513(2) 0.13973(13) 0.0365(6) Uani 1 1 d . . . . .
H12 H 0.5496 1.2112 0.1534 0.044 Uiso 1 1 calc R . . . .
C40 C 0.72570(10) 0.8776(2) 0.27519(15) 0.0427(7) Uani 1 1 d . . . . .
C10 C 0.49036(10) 1.0561(2) 0.05866(12) 0.0376(6) Uani 1 1 d . . . . .
H10 H 0.4730 1.0496 0.0174 0.045 Uiso 1 1 calc R . . . .
C32 C 0.68749(9) 0.6173(3) 0.23524(13) 0.0440(7) Uani 1 1 d . . . . .
H32A H 0.7024 0.6614 0.2682 0.066 Uiso 1 1 calc GR . . . .
H32B H 0.7047 0.6094 0.2079 0.066 Uiso 1 1 calc GR . . . .
H32C H 0.6838 0.5545 0.2522 0.066 Uiso 1 1 calc GR . . . .
C18 C 0.59583(12) 1.2173(2) 0.43417(14) 0.0439(7) Uani 1 1 d . . . . .
H18 H 0.5708 1.2571 0.4221 0.053 Uiso 1 1 calc R . . . .
C11 C 0.51118(10) 1.1418(2) 0.07948(13) 0.0377(6) Uani 1 1 d . . . . .
H11 H 0.5086 1.1943 0.0523 0.045 Uiso 1 1 calc R . . . .
C21 C 0.66936(10) 1.0990(3) 0.46934(15) 0.0463(7) Uani 1 1 d . . . . .
C6 C 0.38635(10) 0.6994(3) -0.09840(13) 0.0464(8) Uani 1 1 d . . . . .
H6 H 0.3688 0.7410 -0.1289 0.056 Uiso 1 1 calc R . . . .
C38 C 0.66701(10) 0.9245(2) 0.20100(14) 0.0445(7) Uani 1 1 d . . . . .
C43 C 0.69214(11) 0.4664(3) 0.54910(16) 0.0507(8) Uani 1 1 d . . . . .
C28 C 0.57771(14) 0.4445(2) 0.28016(14) 0.0598(11) Uani 1 1 d . . . . .
C7 C 0.39613(10) 0.8389(2) -0.02837(13) 0.0429(7) Uani 1 1 d . . . . .
H7A H 0.4121 0.8553 0.0139 0.064 Uiso 1 1 calc GR . . . .
H7B H 0.3652 0.8502 -0.0362 0.064 Uiso 1 1 calc GR . . . .
H7C H 0.4064 0.8792 -0.0556 0.064 Uiso 1 1 calc GR . . . .
C3 C 0.43700(11) 0.5789(3) -0.01127(15) 0.0501(8) Uani 1 1 d . . . . .
H3A H 0.4551 0.5371 0.0186 0.060 Uiso 1 1 calc R . . . .
C19 C 0.63307(11) 1.2489(2) 0.47746(14) 0.0461(7) Uani 1 1 d . . . . .
H19 H 0.6340 1.3112 0.4950 0.055 Uiso 1 1 calc R . . . .
N8 N 0.70385(11) 0.4090(3) 0.58531(17) 0.0662(9) Uani 1 1 d . . . . .
C39 C 0.71131(11) 0.9193(3) 0.21714(16) 0.0513(8) Uani 1 1 d . . . . .
H39 H 0.7287 0.9398 0.1937 0.062 Uiso 1 1 calc R . . . .
C14 C 0.56698(13) 1.0930(2) 0.24644(14) 0.0540(9) Uani 1 1 d . . . . .
H14A H 0.5500 1.0743 0.2726 0.081 Uiso 1 1 calc GR . . . .
H14B H 0.5745 1.1616 0.2524 0.081 Uiso 1 1 calc GR . . . .
H14C H 0.5935 1.0545 0.2569 0.081 Uiso 1 1 calc GR . . . .
C26 C 0.52562(14) 0.4499(2) 0.19074(14) 0.0549(9) Uani 1 1 d . . . . .
C20 C 0.66870(12) 1.1905(3) 0.49518(16) 0.0517(8) Uani 1 1 d . . . . .
H20 H 0.6939 1.2124 0.5260 0.062 Uiso 1 1 calc R . . . .
C41 C 0.77112(10) 0.8551(3) 0.31314(16) 0.0518(8) Uani 1 1 d . . . . .
H41A H 0.7776 0.8873 0.3526 0.078 Uiso 1 1 calc GR . . . .
H41B H 0.7911 0.8781 0.2925 0.078 Uiso 1 1 calc GR . . . .
H41C H 0.7744 0.7853 0.3193 0.078 Uiso 1 1 calc GR . . . .
C37 C 0.63364(12) 0.9613(3) 0.14538(16) 0.0595(10) Uani 1 1 d . . . . .
H37A H 0.6060 0.9291 0.1405 0.089 Uiso 1 1 calc GR . . . .
H37B H 0.6427 0.9480 0.1099 0.089 Uiso 1 1 calc GR . . . .
H37C H 0.6302 1.0310 0.1491 0.089 Uiso 1 1 calc GR . . . .
C1 C 0.39371(12) 0.6080(3) -0.11414(15) 0.0612(10) Uani 1 1 d . . . . .
H1 H 0.3811 0.5865 -0.1548 0.073 Uiso 1 1 calc R . . . .
C25 C 0.49207(15) 0.4250(3) 0.13201(16) 0.0684(12) Uani 1 1 d . . . . .
H25A H 0.4740 0.4816 0.1163 0.103 Uiso 1 1 calc GR . . . .
H25B H 0.4740 0.3724 0.1385 0.103 Uiso 1 1 calc GR . . . .
H25C H 0.5062 0.4045 0.1027 0.103 Uiso 1 1 calc GR . . . .
C2 C 0.41960(14) 0.5468(3) -0.07054(18) 0.0704(12) Uani 1 1 d . . . . .
H2 H 0.4254 0.4833 -0.0811 0.084 Uiso 1 1 calc R . . . .
C29 C 0.61397(17) 0.4208(3) 0.33801(16) 0.0776(15) Uani 1 1 d . . . . .
H29A H 0.6409 0.4507 0.3367 0.116 Uiso 1 1 calc GR . . . .
H29B H 0.6177 0.3507 0.3417 0.116 Uiso 1 1 calc GR . . . .
H29C H 0.6067 0.4458 0.3730 0.116 Uiso 1 1 calc GR . . . .
C22 C 0.71008(12) 1.0395(3) 0.4913(2) 0.0699(12) Uani 1 1 d . . . . .
H22A H 0.7039 0.9789 0.5086 0.105 Uiso 1 1 calc GR . . . .
H22B H 0.7323 1.0755 0.5225 0.105 Uiso 1 1 calc GR . . . .
H22C H 0.7206 1.0255 0.4572 0.105 Uiso 1 1 calc GR . . . .
C27 C 0.55446(19) 0.3886(3) 0.23311(17) 0.0880(18) Uani 1 1 d . . . . .
H27 H 0.5571 0.3209 0.2294 0.106 Uiso 1 1 calc R . . . .
C42 C 0.67740(14) 0.5408(4) 0.5045(2) 0.0785(13) Uani 1 1 d . . . . .
H42A H 0.6723 0.5136 0.4640 0.118 Uiso 1 1 calc GR . . . .
H42B H 0.6994 0.5915 0.5119 0.118 Uiso 1 1 calc GR . . . .
H42C H 0.6504 0.5682 0.5072 0.118 Uiso 1 1 calc GR . . . .
C45 C 0.82508(15) 0.2959(5) 0.7148(2) 0.0806(14) Uani 1 1 d . . . . .
C44 C 0.80234(15) 0.3723(4) 0.6792(3) 0.0882(15) Uani 1 1 d . . . . .
H44A H 0.7749 0.3483 0.6512 0.132 Uiso 1 1 calc GR . . . .
H44B H 0.8197 0.4000 0.6559 0.132 Uiso 1 1 calc GR . . . .
H44C H 0.7965 0.4219 0.7055 0.132 Uiso 1 1 calc GR . . . .
N9 N 0.84307(18) 0.2319(6) 0.7420(3) 0.160(3) Uani 1 1 d . . . . .
H1WA H 0.6396(14) 0.752(3) 0.4378(18) 0.056(11) Uiso 1 1 d . . . . .
H1WB H 0.6792(15) 0.758(3) 0.475(2) 0.076(14) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O4 2.0964(17) . ?
Ni1 O10 2.0897(17) 2_655 ?
Ni1 O10 2.0441(16) . ?
Ni1 O5 2.0246(17) . ?
Ni1 N5 2.097(2) . ?
Ni1 N1 2.098(2) . ?
Ni2 O4 2.1118(17) 2_655 ?
Ni2 O10 2.0520(17) . ?
Ni2 O11 2.0259(17) . ?
Ni2 O6 2.0747(17) 2_655 ?
Ni2 O3 2.0571(17) . ?
Ni2 O2 2.0083(18) . ?
Ni3 O11 1.9934(17) . ?
Ni3 O7 2.161(2) . ?
Ni3 O1W 2.065(2) . ?
Ni3 O1 1.995(2) . ?
Ni3 O9 2.137(2) . ?
Ni3 N4 2.062(2) . ?
O4 Ni2 2.1119(17) 2_655 ?
O4 C16 1.278(3) . ?
O10 Ni1 2.0899(17) 2_655 ?
O10 C30 1.387(3) . ?
O11 C31 1.382(3) . ?
O5 C8 1.261(3) . ?
O6 Ni2 2.0748(17) 2_655 ?
O6 C8 1.264(3) . ?
O3 C16 1.250(3) . ?
O2 C24 1.250(3) . ?
O7 N7 1.266(3) . ?
O1W H1WA 0.80(4) . ?
O1W H1WB 0.80(5) . ?
O1 C24 1.249(3) . ?
N5 N6 1.386(3) . ?
N5 C35 1.341(3) . ?
O9 N7 1.265(4) . ?
N2 N1 1.355(3) . ?
N2 C30 1.455(3) . ?
N2 C28 1.339(4) . ?
N1 C26 1.325(4) . ?
N6 C31 1.478(3) . ?
N6 C33 1.357(3) . ?
N4 N3 1.358(3) . ?
N4 C40 1.332(4) . ?
O8 N7 1.234(3) . ?
N3 H3 0.8800 . ?
N3 C38 1.348(4) . ?
C16 C15 1.497(3) . ?
C15 C13 1.411(4) . ?
C15 C9 1.394(4) . ?
C30 H30 1.0000 . ?
C30 C31 1.544(4) . ?
C8 C4 1.505(3) . ?
C35 C34 1.387(4) . ?
C35 C36 1.497(4) . ?
C31 H31 1.0000 . ?
C13 C12 1.401(4) . ?
C13 C14 1.497(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.385(4) . ?
C24 C23 1.512(4) . ?
C23 C17 1.385(4) . ?
C23 C21 1.406(4) . ?
C33 C34 1.374(4) . ?
C33 C32 1.497(4) . ?
C4 C5 1.403(4) . ?
C4 C3 1.390(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.380(4) . ?
C34 H34 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C5 C6 1.391(4) . ?
C5 C7 1.505(5) . ?
C12 H12 0.9500 . ?
C12 C11 1.379(4) . ?
C40 C39 1.404(5) . ?
C40 C41 1.494(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.378(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C18 H18 0.9500 . ?
C18 C19 1.377(5) . ?
C11 H11 0.9500 . ?
C21 C20 1.407(5) . ?
C21 C22 1.506(5) . ?
C6 H6 0.9500 . ?
C6 C1 1.361(5) . ?
C38 C39 1.373(5) . ?
C38 C37 1.488(5) . ?
C43 N8 1.132(5) . ?
C43 C42 1.432(6) . ?
C28 C29 1.515(5) . ?
C28 C27 1.356(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C3 H3A 0.9500 . ?
C3 C2 1.385(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.368(5) . ?
C39 H39 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C26 C25 1.491(5) . ?
C26 C27 1.408(5) . ?
C20 H20 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C1 H1 0.9500 . ?
C1 C2 1.383(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C2 H2 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C27 H27 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C45 C44 1.401(7) . ?
C45 N9 1.136(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 N5 92.27(7) . . ?
O4 Ni1 N1 174.98(8) . . ?
O10 Ni1 O4 96.68(6) . . ?
O10 Ni1 O4 79.07(6) 2_655 . ?
O10 Ni1 O10 81.06(7) . 2_655 ?
O10 Ni1 N5 89.72(7) . . ?
O10 Ni1 N5 166.45(8) 2_655 . ?
O10 Ni1 N1 99.55(8) 2_655 . ?
O10 Ni1 N1 78.32(7) . . ?
O5 Ni1 O4 90.04(7) . . ?
O5 Ni1 O10 93.13(7) . 2_655 ?
O5 Ni1 O10 170.08(7) . . ?
O5 Ni1 N5 97.31(8) . . ?
O5 Ni1 N1 94.86(8) . . ?
N5 Ni1 N1 88.18(9) . . ?
O10 Ni2 O4 79.56(6) . 2_655 ?
O10 Ni2 O6 88.78(7) . 2_655 ?
O10 Ni2 O3 97.52(7) . . ?
O11 Ni2 O4 160.95(7) . 2_655 ?
O11 Ni2 O10 81.39(7) . . ?
O11 Ni2 O6 92.36(7) . 2_655 ?
O11 Ni2 O3 90.03(7) . . ?
O6 Ni2 O4 87.30(7) 2_655 2_655 ?
O3 Ni2 O4 92.40(7) . 2_655 ?
O3 Ni2 O6 173.53(7) . 2_655 ?
O2 Ni2 O4 98.83(7) . 2_655 ?
O2 Ni2 O10 174.69(7) . . ?
O2 Ni2 O11 100.15(7) . . ?
O2 Ni2 O6 86.08(7) . 2_655 ?
O2 Ni2 O3 87.58(7) . . ?
O11 Ni3 O7 104.63(8) . . ?
O11 Ni3 O1W 88.14(8) . . ?
O11 Ni3 O1 98.26(8) . . ?
O11 Ni3 O9 163.33(9) . . ?
O11 Ni3 N4 89.03(8) . . ?
O1W Ni3 O7 85.09(9) . . ?
O1W Ni3 O9 83.80(9) . . ?
O1 Ni3 O7 156.88(9) . . ?
O1 Ni3 O1W 92.56(10) . . ?
O1 Ni3 O9 96.66(9) . . ?
O1 Ni3 N4 90.57(10) . . ?
O9 Ni3 O7 60.23(9) . . ?
N4 Ni3 O7 92.97(9) . . ?
N4 Ni3 O1W 176.05(11) . . ?
N4 Ni3 O9 98.24(9) . . ?
Ni1 O4 Ni2 96.47(7) . 2_655 ?
C16 O4 Ni1 124.37(15) . . ?
C16 O4 Ni2 132.00(15) . 2_655 ?
Ni1 O10 Ni1 98.85(7) . 2_655 ?
Ni1 O10 Ni2 118.97(8) . . ?
Ni2 O10 Ni1 98.55(7) . 2_655 ?
C30 O10 Ni1 108.76(13) . . ?
C30 O10 Ni1 126.78(14) . 2_655 ?
C30 O10 Ni2 105.85(14) . . ?
Ni3 O11 Ni2 119.86(9) . . ?
C31 O11 Ni2 113.33(14) . . ?
C31 O11 Ni3 121.53(14) . . ?
C8 O5 Ni1 127.82(16) . . ?
C8 O6 Ni2 131.76(15) . 2_655 ?
C16 O3 Ni2 131.20(16) . . ?
C24 O2 Ni2 133.96(18) . . ?
N7 O7 Ni3 90.93(18) . . ?
Ni3 O1W H1WA 111(3) . . ?
Ni3 O1W H1WB 119(3) . . ?
H1WA O1W H1WB 109(4) . . ?
C24 O1 Ni3 134.75(19) . . ?
N6 N5 Ni1 119.48(16) . . ?
C35 N5 Ni1 129.79(17) . . ?
C35 N5 N6 105.2(2) . . ?
N7 O9 Ni3 92.03(16) . . ?
N1 N2 C30 118.1(2) . . ?
C28 N2 N1 112.2(2) . . ?
C28 N2 C30 129.7(2) . . ?
N2 N1 Ni1 109.07(16) . . ?
C26 N1 Ni1 144.9(2) . . ?
C26 N1 N2 105.9(2) . . ?
N5 N6 C31 121.5(2) . . ?
C33 N6 N5 110.6(2) . . ?
C33 N6 C31 126.3(2) . . ?
N3 N4 Ni3 114.77(16) . . ?
C40 N4 Ni3 139.9(2) . . ?
C40 N4 N3 105.2(2) . . ?
N4 N3 H3 123.8 . . ?
C38 N3 N4 112.5(2) . . ?
C38 N3 H3 123.8 . . ?
O9 N7 O7 116.8(2) . . ?
O8 N7 O7 121.1(3) . . ?
O8 N7 O9 122.1(3) . . ?
O4 C16 C15 117.6(2) . . ?
O3 C16 O4 123.5(2) . . ?
O3 C16 C15 118.9(2) . . ?
C13 C15 C16 122.1(2) . . ?
C9 C15 C16 117.9(2) . . ?
C9 C15 C13 119.9(2) . . ?
O10 C30 N2 109.3(2) . . ?
O10 C30 H30 108.7 . . ?
O10 C30 C31 109.2(2) . . ?
N2 C30 H30 108.7 . . ?
N2 C30 C31 112.2(2) . . ?
C31 C30 H30 108.7 . . ?
O5 C8 O6 125.2(2) . . ?
O5 C8 C4 117.8(2) . . ?
O6 C8 C4 116.9(2) . . ?
N5 C35 C34 110.7(2) . . ?
N5 C35 C36 122.1(2) . . ?
C34 C35 C36 127.2(2) . . ?
O11 C31 N6 112.7(2) . . ?
O11 C31 C30 108.22(19) . . ?
O11 C31 H31 108.2 . . ?
N6 C31 C30 111.1(2) . . ?
N6 C31 H31 108.2 . . ?
C30 C31 H31 108.2 . . ?
C15 C13 C14 123.9(2) . . ?
C12 C13 C15 117.2(2) . . ?
C12 C13 C14 118.9(3) . . ?
C15 C9 H9 119.4 . . ?
C10 C9 C15 121.2(2) . . ?
C10 C9 H9 119.4 . . ?
O2 C24 C23 116.8(2) . . ?
O1 C24 O2 125.9(3) . . ?
O1 C24 C23 117.3(2) . . ?
C17 C23 C24 117.5(2) . . ?
C17 C23 C21 119.6(3) . . ?
C21 C23 C24 122.9(3) . . ?
N6 C33 C34 106.9(2) . . ?
N6 C33 C32 123.5(2) . . ?
C34 C33 C32 129.5(2) . . ?
C5 C4 C8 123.2(3) . . ?
C3 C4 C8 117.5(3) . . ?
C3 C4 C5 119.3(3) . . ?
C23 C17 H17 119.2 . . ?
C18 C17 C23 121.5(3) . . ?
C18 C17 H17 119.2 . . ?
C35 C34 H34 126.7 . . ?
C33 C34 C35 106.6(2) . . ?
C33 C34 H34 126.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C4 C5 C7 124.1(2) . . ?
C6 C5 C4 117.9(3) . . ?
C6 C5 C7 117.9(3) . . ?
C13 C12 H12 118.9 . . ?
C11 C12 C13 122.3(3) . . ?
C11 C12 H12 118.9 . . ?
N4 C40 C39 110.1(3) . . ?
N4 C40 C41 121.9(3) . . ?
C39 C40 C41 128.0(3) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.4(2) . . ?
C11 C10 H10 120.3 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C17 C18 H18 120.3 . . ?
C19 C18 C17 119.5(3) . . ?
C19 C18 H18 120.3 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 C12 120.0(3) . . ?
C10 C11 H11 120.0 . . ?
C23 C21 C20 117.3(3) . . ?
C23 C21 C22 124.0(3) . . ?
C20 C21 C22 118.8(3) . . ?
C5 C6 H6 118.7 . . ?
C1 C6 C5 122.7(3) . . ?
C1 C6 H6 118.7 . . ?
N3 C38 C39 105.9(3) . . ?
N3 C38 C37 122.3(3) . . ?
C39 C38 C37 131.8(3) . . ?
N8 C43 C42 178.5(5) . . ?
N2 C28 C29 122.2(3) . . ?
N2 C28 C27 105.9(3) . . ?
C27 C28 C29 131.9(3) . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C3 H3A 119.4 . . ?
C2 C3 C4 121.1(3) . . ?
C2 C3 H3A 119.4 . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.8(3) . . ?
C20 C19 H19 120.1 . . ?
C40 C39 H39 126.8 . . ?
C38 C39 C40 106.4(3) . . ?
C38 C39 H39 126.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C26 C25 122.1(3) . . ?
N1 C26 C27 108.8(3) . . ?
C27 C26 C25 129.0(3) . . ?
C21 C20 H20 118.9 . . ?
C19 C20 C21 122.3(3) . . ?
C19 C20 H20 118.9 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C6 C1 H1 120.2 . . ?
C6 C1 C2 119.5(3) . . ?
C2 C1 H1 120.2 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C3 C2 H2 120.3 . . ?
C1 C2 C3 119.5(4) . . ?
C1 C2 H2 120.3 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C28 C27 C26 107.2(3) . . ?
C28 C27 H27 126.4 . . ?
C26 C27 H27 126.4 . . ?
C43 C42 H42A 109.5 . . ?
C43 C42 H42B 109.5 . . ?
C43 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C45 C44 177.6(8) . . ?
C45 C44 H44A 109.5 . . ?
C45 C44 H44B 109.5 . . ?
C45 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.650
