# Supplementary Information (SI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_nil104_2
_database_code_depnum_ccdc_archive 'CCDC 2367079'
loop_
_audit_author_name
_audit_author_address
'Christoph Janiak'
;University of Duesseldorf
Germany
;
_audit_update_record             
;
2024-07-01 deposited with the CCDC.	2025-01-23 downloaded from the CCDC.
;
_audit_creation_date             2023-11-30
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            
tetrakis-[(μ₃-methanolato-κ³O:O:O)(methanol-\kO)(2-oxyacetophenone-κ²O,O')nickel(II)]
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H56 Ni4 O16'
_chemical_formula_sum            'C40 H56 Ni4 O16'
_chemical_formula_weight         1027.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         C40H56Ni4O16
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'
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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.08705(9)
_cell_length_b                   15.15100(7)
_cell_length_c                   15.82527(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.2175(5)
_cell_angle_gamma                90
_cell_volume                     4557.51(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    95263
_cell_measurement_temperature    298.60(14)
_cell_measurement_theta_max      76.1070
_cell_measurement_theta_min      2.3110
_shelx_estimated_absorpt_T_max   0.744
_shelx_estimated_absorpt_T_min   0.521
_exptl_absorpt_coefficient_mu    2.417
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear green'
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 -1 0.0803
1 1 -1 0.1013
-2 -1 -2 0.1626
-2 -2 1 0.1032
2 1 2 0.0971
1 -2 1 0.1497
1 2 0 0.0483
-2 0 -1 0.1098
-1 2 -1 0.0851
2 0 1 0.0911
1 -2 -1 0.1970
1 0 0 0.0390
2 -2 -1 0.1771
-1 2 1 0.0845
-2 1 -1 0.0955
0 -1 2 0.1184
0 0 -1 0.1527
-2 1 2 0.0988
-2 1 0 0.0731
1 -1 -2 0.1678
-1 0 0 0.0878
-1 2 -2 0.0941
1 2 -1 0.0662
-1 0 1 0.1132

_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0015 2.0001 -0.9986 -0.1304 0.1624 0.0868
0.9983 1.0011 -0.9987 -0.0044 0.1308 0.0888
-1.9971 -1.0005 -2.0001 0.0045 0.1358 -0.2491
-1.9965 -2.0018 0.9979 0.0261 -0.1713 -0.2104
1.9971 1.0005 2.0001 -0.0045 -0.1358 0.2491
1.0006 -1.9992 0.9989 0.1825 -0.1580 -0.0250
0.9974 2.0004 0.0012 -0.0957 0.0765 0.1814
-1.9980 -0.0012 -1.0001 -0.0868 0.0815 -0.1564
-1.0006 1.9992 -0.9989 -0.1825 0.1580 0.0250
1.9980 0.0012 1.0001 0.0868 -0.0815 0.1564
1.0007 -1.9982 -1.0001 0.2174 0.0227 -0.0907
0.9990 0.0008 0.0003 0.0521 0.0044 0.0618
1.9997 -1.9974 -0.9998 0.2695 0.0272 -0.0289
-1.0007 1.9982 1.0001 -0.2174 -0.0227 0.0907
-1.9988 0.9986 -0.9997 -0.1608 0.1175 -0.0966
0.0007 -1.0008 1.9985 0.0391 -0.2167 0.0059
0.0001 0.0005 -0.9995 0.0174 0.0903 -0.0328
-1.9990 0.9971 1.9988 -0.2130 -0.1535 0.0019
-1.9988 0.9981 -0.0002 -0.1782 0.0272 -0.0638
0.9999 -0.9979 -1.9992 0.1609 0.1491 -0.0637
-0.9990 -0.0008 -0.0003 -0.0521 -0.0044 -0.0618
-1.0005 1.9997 -1.9984 -0.1651 0.2483 -0.0078
0.9975 2.0009 -0.9983 -0.0783 0.1668 0.1486
-0.9991 -0.0014 0.9992 -0.0696 -0.0948 -0.0290

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            160640
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.437
_diffrn_reflns_theta_min         2.324
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.60(14)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -109.00 -76.00   0.50    0.16    --  -47.91 -54.00 112.00   66
  2  ω    -23.00  48.00   0.50    0.16    --   47.91 -54.00 112.00  142
  3  ω     53.00  80.00   0.50    0.16    --   47.91  54.00-104.00   54
  4  ω     94.00 119.00   0.50    0.16    --   47.91  54.00-104.00   50
  5  ω    -67.00 -41.00   0.50    0.62    --  -84.25  54.00-104.00   52
  6  ω   -134.00 -94.00   0.50    0.62    --  -84.25 -54.00 112.00   80
  7  ω     93.00 175.00   0.50    0.62    --  105.75  54.00-104.00  164
  8  ω    -20.00  18.00   0.50    0.16    --   12.00 101.00-124.30   76
  9  ω     -9.00  17.00   0.50    0.16    --   20.00 101.00 -34.50   52
 10  ω     -6.00  22.00   0.50    0.16    --   24.00  98.00 176.46   56
 11  ω      2.00  27.00   0.50    0.16    --   32.00  97.00  67.62   50
 12  ω     17.00  42.00   0.50    0.16    --   44.00  88.00  90.18   50
 13  ω     15.00  40.00   0.50    0.16    --   44.00  92.00  17.54   50
 14  ω     16.00  41.00   0.50    0.16    --   44.00  91.00 158.76   50
 15  ω     17.00  42.00   0.50    0.16    --   44.00  88.00 -75.21   50
 16  ω     17.00  42.00   0.50    0.16    --   44.00  89.00-162.16   50
 17  ω   -117.00 -70.00   0.50    0.16    --  -47.91 -77.00 -30.00   94
 18  ω    -63.00 -26.00   0.50    0.16    --  -47.91 -77.00 120.00   74
 19  ω    -52.00 -26.00   0.50    0.16    --  -47.91 -77.00-150.00   52
 20  ω   -119.00 -48.00   0.50    0.16    --  -47.91-178.00 -60.00  142
 21  ω    -59.00  18.00   0.50    0.16    --  -47.91  54.00-104.00  154
 22  ω   -101.00 -75.00   0.50    0.16    --  -47.91 -77.00-150.00   52
 23  ω    -58.00 -28.00   0.50    0.16    --  -47.91 -77.00 -30.00   60
 24  ω     48.00  85.00   0.50    0.16    --   47.91  19.00  30.00   74
 25  ω     39.00 110.00   0.50    0.16    --   47.91  19.00-180.00  142
 26  ω     38.00  73.00   0.50    0.16    --   47.91  19.00 120.00   70
 27  ω     89.00 116.00   0.50    0.16    --   47.91  19.00  30.00   54
 28  ω    -74.00 -34.00   0.50    0.16    --  -56.00 -77.00-171.43   80
 29  ω   -127.00-102.00   0.50    0.16    --  -56.00 -77.00  60.27   50
 30  ω    -65.00 -34.00   0.50    0.16    --  -56.00 -77.00  60.27   62
 31  ω   -126.00 -81.00   0.50    0.16    --  -56.00 -77.00-171.43   90
 32  ω    -79.00 -35.00   0.50    0.16    --  -56.00 -74.00-133.84   88
 33  ω    -60.00 -35.00   0.50    0.16    --  -56.00 -76.00  17.61   50
 34  ω   -120.00 -94.00   0.50    0.16    --  -56.00 -76.00  17.61   52
 35  ω    -64.00 -39.00   0.50    0.16    --  -60.00 -75.00 -85.45   50
 36  ω    -64.00 -38.00   0.50    0.16    --  -60.00 -77.00 -68.15   52
 37  ω    -73.00 -38.00   0.50    0.16    --  -60.00 -77.00 -38.47   70
 38  ω     39.00  84.00   0.50    0.16    --   60.00  75.00 155.20   90
 39  ω   -128.00-102.00   0.50    0.16    --  -64.00 -77.00 166.79   52
 40  ω    -68.00 -42.00   0.50    0.16    --  -64.00 -77.00 166.79   52
 41  ω    -69.00 -43.00   0.50    0.16    --  -64.00 -74.00 -91.78   52
 42  ω    -77.00 -45.00   0.50    0.16    --  -64.00 -69.00 102.19   64
 43  ω    -71.00 -46.00   0.50    0.16    --  -68.00 -77.00 107.78   50
 44  ω    -72.00 -47.00   0.50    0.16    --  -68.00 -75.00-161.13   50
 45  ω    -72.00 -47.00   0.50    0.16    --  -68.00 -76.00  15.91   50
 46  ω    -75.00 -49.00   0.50    0.16    --  -68.00 -75.00  61.84   52
 47  ω    -71.00 -46.00   0.50    0.16    --  -68.00 -77.00 -10.72   50
 48  ω    -77.00 -50.00   0.50    0.16    --  -72.00 -77.00-152.73   54
 49  ω    -76.00 -51.00   0.50    0.16    --  -72.00 -76.00 153.06   50
 50  ω    -80.00 -51.00   0.50    0.16    --  -72.00 -75.00-102.72   58
 51  ω    -82.00 -51.00   0.50    0.16    --  -72.00 -75.00 178.57   62
 52  ω    -81.00 -51.00   0.50    0.16    --  -72.00 -74.00-139.93   60
 53  ω    -90.00 -55.00   0.50    0.16    --  -76.00 -76.00 -48.00   70
 54  ω    -81.00 -55.00   0.50    0.16    --  -76.00 -74.00  99.11   52
 55  ω    -81.00 -55.00   0.50    0.16    --  -76.00 -76.00  49.42   52
 56  ω    -81.00 -55.00   0.50    0.16    --  -76.00 -76.00-113.53   52
 57  ω    -83.00 -58.00   0.50    0.62    --  -80.00 -77.00 151.29   50
 58  ω    -85.00 -59.00   0.50    0.62    --  -80.00 -76.00 -62.57   52
 59  ω    -90.00 -64.00   0.50    0.62    --  -84.25 -74.00-109.48   52
 60  ω   -153.00-116.00   0.50    0.62    --  -84.25 -77.00-124.76   74
 61  ω   -102.00 -64.00   0.50    0.62    --  -84.25 -76.00  76.67   76
 62  ω    -90.00 -62.00   0.50    0.62    --  -84.25 -77.00  60.00   56
 63  ω   -125.00 -64.00   0.50    0.62    --  -84.25 -72.00-163.46  122
 64  ω    -90.00 -63.00   0.50    0.62    --  -84.25 -76.00-136.77   54
 65  ω   -152.00-124.00   0.50    0.62    --  -84.25 -76.00-136.77   56
 66  ω   -153.00-127.00   0.50    0.62    --  -84.25 -76.00  76.67   52
 67  ω    -90.00 -64.00   0.50    0.62    --  -84.25 -73.00  91.45   52
 68  ω    -98.00 -63.00   0.50    0.62    --  -84.25 -76.00 127.35   70
 69  ω   -153.00 -68.00   0.50    0.62    --  -84.25 -65.00  95.83  170
 70  ω    -92.00 -63.00   0.50    0.62    --  -84.25 -76.00 174.65   58
 71  ω   -141.00-115.00   0.50    0.62    --  -84.25 -73.00  91.45   52
 72  ω    -91.00 -66.00   0.50    0.62    --  -84.25 -69.00-178.92   50
 73  ω   -155.00-113.00   0.50    0.62    --  -84.25 -76.00 127.35   84
 74  ω   -100.00 -64.00   0.50    0.62    --  -84.25 -74.00  16.95   72
 75  ω    -91.00 -65.00   0.50    0.62    --  -84.25 -73.00 -15.46   52
 76  ω   -114.00 -62.00   0.50    0.62    --  -84.25 -77.00 150.00  104
 77  ω    -89.00 -63.00   0.50    0.62    --  -84.25 -76.00  38.87   52
 78  ω   -150.00-119.00   0.50    0.62    --  -84.25 -76.00  38.87   62
 79  ω   -105.00 -64.00   0.50    0.62    --  -84.25 -77.00  90.00   82
 80  ω   -156.00-121.00   0.50    0.62    --  -84.25 -77.00  90.00   70
 81  ω    -87.00 -62.00   0.50    0.62    --  -84.25 -77.00-180.00   50
 82  ω   -145.00-108.00   0.50    0.62    --  -84.25 -77.00-180.00   74
 83  ω    -90.00 -64.00   0.50    0.62    --  -84.25 -75.00 -87.59   52
 84  ω   -123.00 -64.00   0.50    0.62    --  -84.25 -75.00   7.81  118
 85  ω   -147.00-118.00   0.50    0.62    --  -84.25 -77.00  60.00   58
 86  ω   -155.00-115.00   0.50    0.62    --  -84.25 -75.00 -87.59   80
 87  ω   -101.00 -62.00   0.50    0.62    --  -84.25 -77.00   0.00   78
 88  ω   -100.00 -64.00   0.50    0.62    --  -84.25 -72.00 -53.10   72
 89  ω   -139.00-113.00   0.50    0.62    --  -84.25 -77.00   0.00   52
 90  ω    -89.00 -64.00   0.50    0.62    --  -84.25 -72.00 -77.43   50
 91  ω   -141.00-116.00   0.50    0.62    --  -84.25 -72.00 -77.43   50
 92  ω    -88.00 -62.00   0.50    0.62    --  -84.25 -77.00-124.76   52
 93  ω   -156.00-125.00   0.50    0.62    --  -84.25 -74.00  16.95   62
 94  ω    -87.00 -62.00   0.50    0.62    --  -84.25 -77.00 -30.00   50
 95  ω   -115.00 -90.00   0.50    0.62    --  -84.25 -77.00 -30.00   50
 96  ω    -88.00 -63.00   0.50    0.62    --  -84.25 -75.00 -21.30   50
 97  ω     87.00 177.00   0.50    0.62    --  105.75  77.00 120.00  180
 98  ω     35.00  61.00   0.50    0.62    --  105.75 -57.00  30.00   52
 99  ω     38.00 102.00   0.50    0.62    --  105.75 -99.00 -90.00  128
100  ω     86.00 175.00   0.50    0.62    --  105.75  77.00 -60.00  178
101  ω     37.00 102.00   0.50    0.62    --  105.75 -99.00-180.00  130
102  ω     68.00 105.00   0.50    0.62    --  105.75 -99.00  60.00   74
103  ω     36.00  65.00   0.50    0.62    --  105.75 -99.00  60.00   58
104  ω     42.00 104.00   0.50    0.62    --  105.75 -99.00  30.00  124
105  ω     37.00 103.00   0.50    0.62    --  105.75 -99.00 120.00  132
106  ω     36.00 106.00   0.50    0.62    --  105.75 -99.00   0.00  140
107  ω     37.00 111.00   0.50    0.62    --  105.75-125.00 120.00  148
108  ω     39.00 109.00   0.50    0.62    --  105.75-115.00 166.34  140
109  ω    150.00 175.00   0.50    0.62    --  105.75  77.00  30.00   50
110  ω     87.00 126.00   0.50    0.62    --  105.75  77.00  30.00   78
111  ω     87.00 172.00   0.50    0.62    --  105.75  77.00 -90.00  170
112  ω     77.00 110.00   0.50    0.62    --  105.75-125.00   0.00   66
113  ω     97.00 163.00   0.50    0.62    --  105.75  19.00   0.00  132
114  ω     37.00  72.00   0.50    0.62    --  105.75-125.00   0.00   70
115  ω     96.00 176.00   0.50    0.62    --  105.75  38.00-120.00  160
116  ω    102.00 178.00   0.50    0.62    --  105.75  38.00-180.00  152
117  ω     35.00  60.00   0.50    0.62    --  105.75 -57.00   0.00   50
118  ω     37.00  91.00   0.50    0.62    --  105.75 -99.00-150.00  108
119  ω     36.00 103.00   0.50    0.62    --  105.75 -99.00 -60.00  134
120  ω     97.00 139.00   0.50    0.62    --  105.75  57.00  30.00   84
121  ω    112.00 176.00   0.50    0.62    --  105.75  38.00  90.00  128
122  ω    100.00 140.00   0.50    0.62    --  105.75  19.00-120.00   80
123  ω     38.00 109.00   0.50    0.62    --  105.75-112.00 -86.94  142
124  ω     35.00  60.00   0.50    0.62    --  105.75 -57.00-180.00   50
125  ω     35.00  60.00   0.50    0.62    --  105.75 -57.00 -90.00   50
;
_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      0.0522528000
_diffrn_orient_matrix_UB_12      -0.0738712000
_diffrn_orient_matrix_UB_13      -0.0174614000
_diffrn_orient_matrix_UB_21      0.0044366000
_diffrn_orient_matrix_UB_22      0.0360773000
_diffrn_orient_matrix_UB_23      -0.0903745000
_diffrn_orient_matrix_UB_31      0.0617907000
_diffrn_orient_matrix_UB_32      0.0598565000
_diffrn_orient_matrix_UB_33      0.0328896000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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                8883
_reflns_number_total             9486
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         9486
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0318
_refine_ls_restrained_S_all      1.069
_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)+(0.0515P)²+1.4514P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0980
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O7-H7
 1 with sigma of 0.02
 O10-C32A \\sim O10-C32B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O7, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O16, C13
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7A), C15(H15), C16(H16A), C17(H17), C18(H18),
 C25(H25), C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36), C37(H37)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32A(H32A,H32B,H32C),
 C32B(H32D,H32E,H32F), C40(H40A,H40B,H40C)
;
_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 0.80821(2) 0.52969(2) 0.36088(2) 0.04776(9) Uani 1 1 d . . . . .
Ni2 Ni 0.70260(2) 0.53851(2) 0.20442(2) 0.04872(9) Uani 1 1 d . . . . .
Ni3 Ni 0.68522(2) 0.40019(2) 0.34701(2) 0.04804(9) Uani 1 1 d . . . . .
Ni4 Ni 0.79985(2) 0.37777(2) 0.22637(2) 0.04545(9) Uani 1 1 d . . . . .
O1 O 0.80737(6) 0.51321(8) 0.23203(8) 0.0462(3) Uani 1 1 d . . . . .
O2 O 0.69387(6) 0.40403(8) 0.21934(7) 0.0463(3) Uani 1 1 d . . . . .
O3 O 0.79365(6) 0.39659(8) 0.35433(7) 0.0447(2) Uani 1 1 d . . . . .
O4 O 0.70114(6) 0.53347(8) 0.33330(8) 0.0492(3) Uani 1 1 d . . . . .
O5 O 0.78861(7) 0.24630(8) 0.23526(9) 0.0560(3) Uani 1 1 d . . . . .
O6 O 0.90521(7) 0.35860(9) 0.23524(9) 0.0559(3) Uani 1 1 d . . . . .
O7 O 0.79235(8) 0.38458(10) 0.09244(9) 0.0633(3) Uani 1 1 d D . . . .
O8 O 0.71015(7) 0.53017(10) 0.07981(9) 0.0610(3) Uani 1 1 d . . . . .
O9 O 0.59932(7) 0.56640(11) 0.17796(9) 0.0644(4) Uani 1 1 d . . . . .
O10 O 0.72391(9) 0.67606(10) 0.21875(11) 0.0736(4) Uani 1 1 d D . . . .
O11 O 0.81499(7) 0.66033(9) 0.35762(10) 0.0662(4) Uani 1 1 d . . . . .
O12 O 0.91476(7) 0.52622(9) 0.38157(9) 0.0559(3) Uani 1 1 d . . . . .
O13 O 0.79720(8) 0.51786(11) 0.49272(9) 0.0659(4) Uani 1 1 d . . . . .
O14 O 0.68805(7) 0.40801(11) 0.47223(8) 0.0625(4) Uani 1 1 d . . . . .
O15 O 0.57844(7) 0.40172(10) 0.34283(8) 0.0610(3) Uani 1 1 d . . . . .
O16 O 0.68148(7) 0.26021(10) 0.33909(10) 0.0626(4) Uani 1 1 d . . . . .
C1 C 0.85869(10) 0.55847(14) 0.18872(14) 0.0604(5) Uani 1 1 d . . . . .
H1A H 0.868160 0.614927 0.214832 0.091 Uiso 1 1 calc R U . . .
H1B H 0.841326 0.566680 0.130398 0.091 Uiso 1 1 calc R U . . .
H1C H 0.901223 0.524352 0.191695 0.091 Uiso 1 1 calc R U . . .
C2 C 0.84922(15) 0.3767(2) 0.04199(18) 0.0909(8) Uani 1 1 d . . . . .
H2A H 0.833048 0.387426 -0.016327 0.136 Uiso 1 1 calc R U . . .
H2B H 0.868528 0.318295 0.047702 0.136 Uiso 1 1 calc R U . . .
H2C H 0.884815 0.419102 0.060255 0.136 Uiso 1 1 calc R U . . .
C3 C 0.83686(10) 0.18813(12) 0.25758(11) 0.0522(4) Uani 1 1 d . . . . .
C4 C 0.81486(12) 0.10032(13) 0.27229(14) 0.0627(5) Uani 1 1 d . . . . .
H4 H 0.767236 0.086669 0.263824 0.075 Uiso 1 1 calc R U . . .
C5 C 0.86164(14) 0.03506(14) 0.29860(15) 0.0720(6) Uani 1 1 d . . . . .
H5 H 0.845311 -0.021836 0.306874 0.086 Uiso 1 1 calc R U . . .
C6 C 0.93272(13) 0.05278(16) 0.31295(16) 0.0753(6) Uani 1 1 d . . . . .
H6 H 0.964090 0.008394 0.331488 0.090 Uiso 1 1 calc R U . . .
C7 C 0.95631(12) 0.13599(15) 0.29964(15) 0.0660(5) Uani 1 1 d . . . . .
H7A H 1.004208 0.147460 0.309708 0.079 Uiso 1 1 calc R U . . .
C8 C 0.91071(10) 0.20590(13) 0.27102(12) 0.0530(4) Uani 1 1 d . . . . .
C9 C 0.94064(9) 0.29310(13) 0.25914(12) 0.0527(4) Uani 1 1 d . . . . .
C10 C 1.01855(11) 0.30860(16) 0.27629(17) 0.0720(6) Uani 1 1 d . . . . .
H10A H 1.033257 0.293644 0.334141 0.108 Uiso 1 1 calc R U . . .
H10B H 1.028780 0.369622 0.266620 0.108 Uiso 1 1 calc R U . . .
H10C H 1.043305 0.272434 0.239040 0.108 Uiso 1 1 calc R U . . .
C11 C 0.64462(10) 0.35651(15) 0.16291(13) 0.0607(5) Uani 1 1 d . . . . .
H11A H 0.600015 0.354096 0.186370 0.091 Uiso 1 1 calc R U . . .
H11B H 0.661632 0.297642 0.155518 0.091 Uiso 1 1 calc R U . . .
H11C H 0.639175 0.385920 0.108980 0.091 Uiso 1 1 calc R U . . .
C12 C 0.83352(10) 0.34230(13) 0.41395(12) 0.0529(4) Uani 1 1 d . . . . .
H12A H 0.882498 0.356798 0.414232 0.079 Uiso 1 1 calc R U . . .
H12B H 0.826544 0.281452 0.398469 0.079 Uiso 1 1 calc R U . . .
H12C H 0.818465 0.351921 0.469467 0.079 Uiso 1 1 calc R U . . .
C13 C 0.68389(15) 0.20402(19) 0.41204(19) 0.0897(8) Uani 1 1 d . . . . .
H13A H 0.685048 0.143463 0.394367 0.135 Uiso 1 1 calc R U . . .
H13B H 0.642909 0.213933 0.441701 0.135 Uiso 1 1 calc R U . . .
H13C H 0.725334 0.216986 0.448955 0.135 Uiso 1 1 calc R U . . .
C14 C 0.63730(10) 0.39596(14) 0.52057(12) 0.0548(4) Uani 1 1 d . . . . .
C15 C 0.65515(12) 0.39199(17) 0.60867(13) 0.0711(6) Uani 1 1 d . . . . .
H15 H 0.701933 0.399257 0.629529 0.085 Uiso 1 1 calc R U . . .
C16 C 0.60588(14) 0.3778(2) 0.66444(15) 0.0884(8) Uani 1 1 d . . . . .
H16A H 0.619403 0.375806 0.722370 0.106 Uiso 1 1 calc R U . . .
C17 C 0.53582(15) 0.3664(2) 0.63528(17) 0.0988(10) Uani 1 1 d . . . . .
H17 H 0.502448 0.355269 0.673260 0.119 Uiso 1 1 calc R U . . .
C18 C 0.51640(12) 0.3715(2) 0.55110(16) 0.0804(7) Uani 1 1 d . . . . .
H18 H 0.469071 0.364974 0.532391 0.096 Uiso 1 1 calc R U . . .
C19 C 0.56510(10) 0.38639(14) 0.49020(13) 0.0574(4) Uani 1 1 d . . . . .
C20 C 0.54006(10) 0.39250(14) 0.40101(13) 0.0579(5) Uani 1 1 d . . . . .
C21 C 0.46224(12) 0.3884(2) 0.37458(17) 0.0871(8) Uani 1 1 d . . . . .
H21A H 0.445207 0.329973 0.384126 0.131 Uiso 1 1 calc R U . . .
H21B H 0.453884 0.402746 0.315433 0.131 Uiso 1 1 calc R U . . .
H21C H 0.438053 0.429953 0.407362 0.131 Uiso 1 1 calc R U . . .
C22 C 0.65827(11) 0.59314(16) 0.37566(15) 0.0684(6) Uani 1 1 d . . . . .
H22A H 0.651011 0.570202 0.430735 0.103 Uiso 1 1 calc R U . . .
H22B H 0.613688 0.599943 0.343019 0.103 Uiso 1 1 calc R U . . .
H22C H 0.681267 0.649435 0.381726 0.103 Uiso 1 1 calc R U . . .
C23 C 0.79588(18) 0.5831(2) 0.55510(18) 0.0968(9) Uani 1 1 d . . . . .
H23A H 0.754411 0.618589 0.543925 0.145 Uiso 1 1 calc R U . . .
H23B H 0.836872 0.619707 0.554406 0.145 Uiso 1 1 calc R U . . .
H23C H 0.795456 0.555746 0.609769 0.145 Uiso 1 1 calc R U . . .
C24 C 0.86494(11) 0.70810(13) 0.39590(13) 0.0587(4) Uani 1 1 d . . . . .
C25 C 0.84943(15) 0.79634(15) 0.41564(16) 0.0758(6) Uani 1 1 d . . . . .
H25 H 0.804522 0.818214 0.400447 0.091 Uiso 1 1 calc R U . . .
C26 C 0.89886(18) 0.85059(17) 0.45664(17) 0.0876(8) Uani 1 1 d . . . . .
H26 H 0.886957 0.908349 0.469166 0.105 Uiso 1 1 calc R U . . .
C27 C 0.96603(18) 0.82055(18) 0.47951(18) 0.0912(8) Uani 1 1 d . . . . .
H27 H 0.999326 0.857688 0.507449 0.109 Uiso 1 1 calc R U . . .
C28 C 0.98323(14) 0.73602(16) 0.46086(16) 0.0757(6) Uani 1 1 d . . . . .
H28 H 1.028878 0.716558 0.475901 0.091 Uiso 1 1 calc R U . . .
C29 C 0.93444(11) 0.67693(13) 0.41960(12) 0.0566(4) Uani 1 1 d . . . . .
C30 C 0.95659(9) 0.58651(13) 0.40333(11) 0.0516(4) Uani 1 1 d . . . . .
C31 C 1.03313(10) 0.56189(17) 0.41315(15) 0.0678(5) Uani 1 1 d . . . . .
H31A H 1.059512 0.603870 0.383466 0.102 Uiso 1 1 calc R U . . .
H31B H 1.039006 0.504071 0.390010 0.102 Uiso 1 1 calc R U . . .
H31C H 1.049802 0.562008 0.472239 0.102 Uiso 1 1 calc R U . . .
C32A C 0.7358(4) 0.7394(4) 0.1590(4) 0.102(2) Uani 0.768(14) 1 d D . P A 1
H32A H 0.762922 0.714286 0.116800 0.153 Uiso 0.768(14) 1 calc R U P A 1
H32B H 0.761266 0.787894 0.186209 0.153 Uiso 0.768(14) 1 calc R U P A 1
H32C H 0.691655 0.760178 0.132550 0.153 Uiso 0.768(14) 1 calc R U P A 1
C32B C 0.6892(15) 0.7516(8) 0.1957(16) 0.110(9) Uani 0.232(14) 1 d D . P A 2
H32D H 0.671747 0.748217 0.137009 0.164 Uiso 0.232(14) 1 calc R U P A 2
H32E H 0.720791 0.800782 0.204117 0.164 Uiso 0.232(14) 1 calc R U P A 2
H32F H 0.650553 0.759276 0.229831 0.164 Uiso 0.232(14) 1 calc R U P A 2
H10 H 0.755(2) 0.682(3) 0.266(3) 0.164 Uiso 1 1 d . U . . .
C33 C 0.66605(11) 0.55750(14) 0.01842(12) 0.0591(5) Uani 1 1 d . . . . .
C34 C 0.68695(14) 0.5551(2) -0.06486(15) 0.0790(7) Uani 1 1 d . . . . .
H34 H 0.730437 0.531151 -0.074205 0.095 Uiso 1 1 calc R U . . .
C35 C 0.6443(2) 0.5875(3) -0.13237(18) 0.1203(13) Uani 1 1 d . . . . .
H35 H 0.659687 0.586365 -0.186439 0.144 Uiso 1 1 calc R U . . .
C36 C 0.5789(2) 0.6217(3) -0.1210(2) 0.1463(18) Uani 1 1 d . . . . .
H36 H 0.550874 0.644372 -0.167076 0.176 Uiso 1 1 calc R U . . .
H7 H 0.765(2) 0.436(2) 0.076(3) 0.220 Uiso 1 1 d D U . . .
H13 H 0.760(3) 0.487(4) 0.493(3) 0.220 Uiso 1 1 d . U . . .
H16 H 0.709(3) 0.244(4) 0.305(4) 0.220 Uiso 1 1 d . U . . .
C37 C 0.55547(17) 0.6223(3) -0.04265(18) 0.1086(11) Uani 1 1 d . . . . .
H37 H 0.510989 0.644855 -0.035992 0.130 Uiso 1 1 calc R U . . .
C38 C 0.59695(12) 0.58944(16) 0.02942(14) 0.0681(5) Uani 1 1 d . . . . .
C39 C 0.56691(11) 0.58812(16) 0.10979(14) 0.0659(5) Uani 1 1 d . . . . .
C40 C 0.49070(14) 0.6135(3) 0.1151(2) 0.1050(11) Uani 1 1 d . . . . .
H40A H 0.484404 0.674767 0.101046 0.158 Uiso 1 1 calc R U . . .
H40B H 0.478156 0.603345 0.171643 0.158 Uiso 1 1 calc R U . . .
H40C H 0.461223 0.578331 0.075839 0.158 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0529(12) . ?
Ni1 O3 2.0370(12) . ?
Ni1 O4 2.0513(12) . ?
Ni1 O11 1.9846(14) . ?
Ni1 O12 2.0310(13) . ?
Ni1 O13 2.1234(15) . ?
Ni2 O1 2.0441(12) . ?
Ni2 O2 2.0597(13) . ?
Ni2 O4 2.0438(13) . ?
Ni2 O8 1.9942(14) . ?
Ni2 O9 2.0223(13) . ?
Ni2 O10 2.1314(16) . ?
Ni3 O2 2.0428(12) . ?
Ni3 O3 2.0630(11) . ?
Ni3 O4 2.0565(13) . ?
Ni3 O14 1.9811(13) . ?
Ni3 O15 2.0333(13) . ?
Ni3 O16 2.1253(15) . ?
Ni4 O1 2.0584(12) . ?
Ni4 O2 2.0547(12) . ?
Ni4 O3 2.0590(12) . ?
Ni4 O5 2.0098(13) . ?
Ni4 O6 2.0241(13) . ?
Ni4 O7 2.1137(14) . ?
O1 C1 1.422(2) . ?
O2 C11 1.431(2) . ?
O3 C12 1.420(2) . ?
O4 C22 1.427(2) . ?
O5 C3 1.300(2) . ?
O6 C9 1.240(2) . ?
O7 C2 1.410(3) . ?
O7 H7 0.955(19) . ?
O8 C33 1.294(2) . ?
O9 C39 1.238(2) . ?
O10 C32A 1.381(4) . ?
O10 C32B 1.355(11) . ?
O10 H10 0.91(4) . ?
O11 C24 1.302(2) . ?
O12 C30 1.241(2) . ?
O13 C23 1.399(3) . ?
O13 H13 0.86(5) . ?
O14 C14 1.301(2) . ?
O15 C20 1.236(2) . ?
O16 C13 1.432(3) . ?
O16 H16 0.82(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.421(3) . ?
C3 C8 1.432(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.371(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.381(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.362(3) . ?
C7 H7A 0.9300 . ?
C7 C8 1.419(3) . ?
C8 C9 1.458(3) . ?
C9 C10 1.506(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.406(3) . ?
C14 C19 1.425(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.364(3) . ?
C16 H16A 0.9300 . ?
C16 C17 1.385(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.352(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.417(3) . ?
C19 C20 1.451(3) . ?
C20 C21 1.507(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.410(3) . ?
C24 C29 1.426(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.370(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.377(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.361(4) . ?
C28 H28 0.9300 . ?
C28 C29 1.409(3) . ?
C29 C30 1.463(3) . ?
C30 C31 1.502(3) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32A H32A 0.9600 . ?
C32A H32B 0.9600 . ?
C32A H32C 0.9600 . ?
C32B H32D 0.9600 . ?
C32B H32E 0.9600 . ?
C32B H32F 0.9600 . ?
C33 C34 1.412(3) . ?
C33 C38 1.430(3) . ?
C34 H34 0.9300 . ?
C34 C35 1.374(4) . ?
C35 H35 0.9300 . ?
C35 C36 1.377(5) . ?
C36 H36 0.9300 . ?
C36 C37 1.356(5) . ?
C37 H37 0.9300 . ?
C37 C38 1.418(3) . ?
C38 C39 1.442(3) . ?
C39 C40 1.514(3) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O13 166.69(6) . . ?
O3 Ni1 O1 80.81(5) . . ?
O3 Ni1 O4 83.58(5) . . ?
O3 Ni1 O13 86.63(6) . . ?
O4 Ni1 O1 82.79(5) . . ?
O4 Ni1 O13 91.47(5) . . ?
O11 Ni1 O1 95.17(6) . . ?
O11 Ni1 O3 174.26(5) . . ?
O11 Ni1 O4 91.87(5) . . ?
O11 Ni1 O12 87.90(6) . . ?
O11 Ni1 O13 97.02(7) . . ?
O12 Ni1 O1 94.26(5) . . ?
O12 Ni1 O3 96.46(5) . . ?
O12 Ni1 O4 177.01(5) . . ?
O12 Ni1 O13 91.52(6) . . ?
O1 Ni2 O2 82.98(5) . . ?
O1 Ni2 O10 89.26(6) . . ?
O2 Ni2 O10 166.33(6) . . ?
O4 Ni2 O1 83.19(5) . . ?
O4 Ni2 O2 80.79(5) . . ?
O4 Ni2 O10 87.14(6) . . ?
O8 Ni2 O1 92.42(5) . . ?
O8 Ni2 O2 93.70(6) . . ?
O8 Ni2 O4 173.32(5) . . ?
O8 Ni2 O9 88.01(6) . . ?
O8 Ni2 O10 97.87(7) . . ?
O9 Ni2 O1 178.71(6) . . ?
O9 Ni2 O2 98.22(6) . . ?
O9 Ni2 O4 96.48(5) . . ?
O9 Ni2 O10 89.47(7) . . ?
O2 Ni3 O3 83.42(5) . . ?
O2 Ni3 O4 80.90(5) . . ?
O2 Ni3 O16 88.59(6) . . ?
O3 Ni3 O16 90.30(5) . . ?
O4 Ni3 O3 82.81(5) . . ?
O4 Ni3 O16 168.00(6) . . ?
O14 Ni3 O2 172.02(5) . . ?
O14 Ni3 O3 90.54(5) . . ?
O14 Ni3 O4 93.21(6) . . ?
O14 Ni3 O15 88.16(5) . . ?
O14 Ni3 O16 96.68(6) . . ?
O15 Ni3 O2 97.95(5) . . ?
O15 Ni3 O3 178.40(5) . . ?
O15 Ni3 O4 98.20(6) . . ?
O15 Ni3 O16 88.92(6) . . ?
O1 Ni4 O3 80.16(5) . . ?
O1 Ni4 O7 89.61(6) . . ?
O2 Ni4 O1 82.75(5) . . ?
O2 Ni4 O3 83.23(5) . . ?
O2 Ni4 O7 87.69(5) . . ?
O3 Ni4 O7 167.07(5) . . ?
O5 Ni4 O1 172.96(6) . . ?
O5 Ni4 O2 94.87(5) . . ?
O5 Ni4 O3 93.00(5) . . ?
O5 Ni4 O6 87.97(5) . . ?
O5 Ni4 O7 96.93(6) . . ?
O6 Ni4 O1 94.31(5) . . ?
O6 Ni4 O2 176.97(5) . . ?
O6 Ni4 O3 95.58(5) . . ?
O6 Ni4 O7 93.03(6) . . ?
Ni1 O1 Ni4 99.13(5) . . ?
Ni2 O1 Ni1 96.24(5) . . ?
Ni2 O1 Ni4 96.58(5) . . ?
C1 O1 Ni1 118.47(12) . . ?
C1 O1 Ni2 120.66(11) . . ?
C1 O1 Ni4 120.54(12) . . ?
Ni3 O2 Ni2 98.99(5) . . ?
Ni3 O2 Ni4 96.24(5) . . ?
Ni4 O2 Ni2 96.21(5) . . ?
C11 O2 Ni2 118.79(11) . . ?
C11 O2 Ni3 119.70(11) . . ?
C11 O2 Ni4 121.61(12) . . ?
Ni1 O3 Ni3 96.21(5) . . ?
Ni1 O3 Ni4 99.63(5) . . ?
Ni4 O3 Ni3 95.48(5) . . ?
C12 O3 Ni1 118.52(11) . . ?
C12 O3 Ni3 121.80(11) . . ?
C12 O3 Ni4 119.88(11) . . ?
Ni1 O4 Ni3 95.97(5) . . ?
Ni2 O4 Ni1 96.29(5) . . ?
Ni2 O4 Ni3 99.06(5) . . ?
C22 O4 Ni1 121.37(12) . . ?
C22 O4 Ni2 120.37(12) . . ?
C22 O4 Ni3 118.43(13) . . ?
C3 O5 Ni4 127.84(12) . . ?
C9 O6 Ni4 130.28(13) . . ?
Ni4 O7 H7 107(3) . . ?
C2 O7 Ni4 125.33(16) . . ?
C2 O7 H7 110(3) . . ?
C33 O8 Ni2 128.41(14) . . ?
C39 O9 Ni2 129.51(14) . . ?
Ni2 O10 H10 107(3) . . ?
C32A O10 Ni2 130.5(3) . . ?
C32A O10 H10 111(3) . . ?
C32B O10 Ni2 135.5(8) . . ?
C32B O10 H10 113(3) . . ?
C24 O11 Ni1 126.09(13) . . ?
C30 O12 Ni1 129.43(13) . . ?
Ni1 O13 H13 102(3) . . ?
C23 O13 Ni1 130.06(18) . . ?
C23 O13 H13 108(4) . . ?
C14 O14 Ni3 128.75(12) . . ?
C20 O15 Ni3 129.42(13) . . ?
Ni3 O16 H16 108(4) . . ?
C13 O16 Ni3 123.19(17) . . ?
C13 O16 H16 113(4) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O7 C2 H2A 109.5 . . ?
O7 C2 H2B 109.5 . . ?
O7 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O5 C3 C4 117.82(18) . . ?
O5 C3 C8 125.19(17) . . ?
C4 C3 C8 116.97(17) . . ?
C3 C4 H4 119.0 . . ?
C5 C4 C3 122.1(2) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.8(2) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 H6 120.4 . . ?
C7 C6 C5 119.2(2) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 H7A 118.7 . . ?
C6 C7 C8 122.6(2) . . ?
C8 C7 H7A 118.7 . . ?
C3 C8 C9 122.89(16) . . ?
C7 C8 C3 118.30(19) . . ?
C7 C8 C9 118.78(18) . . ?
O6 C9 C8 123.72(17) . . ?
O6 C9 C10 115.61(18) . . ?
C8 C9 C10 120.67(17) . . ?
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 . . ?
O2 C11 H11A 109.5 . . ?
O2 C11 H11B 109.5 . . ?
O2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O3 C12 H12A 109.5 . . ?
O3 C12 H12B 109.5 . . ?
O3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O16 C13 H13A 109.5 . . ?
O16 C13 H13B 109.5 . . ?
O16 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O14 C14 C15 117.58(18) . . ?
O14 C14 C19 124.40(17) . . ?
C15 C14 C19 118.02(18) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 122.0(2) . . ?
C16 C15 H15 119.0 . . ?
C15 C16 H16A 119.8 . . ?
C15 C16 C17 120.4(2) . . ?
C17 C16 H16A 119.8 . . ?
C16 C17 H17 120.3 . . ?
C18 C17 C16 119.4(2) . . ?
C18 C17 H17 120.3 . . ?
C17 C18 H18 118.6 . . ?
C17 C18 C19 122.8(2) . . ?
C19 C18 H18 118.6 . . ?
C14 C19 C20 122.99(17) . . ?
C18 C19 C14 117.45(19) . . ?
C18 C19 C20 119.55(19) . . ?
O15 C20 C19 124.52(17) . . ?
O15 C20 C21 115.72(19) . . ?
C19 C20 C21 119.76(19) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O13 C23 H23A 109.5 . . ?
O13 C23 H23B 109.5 . . ?
O13 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O11 C24 C25 118.1(2) . . ?
O11 C24 C29 124.25(18) . . ?
C25 C24 C29 117.7(2) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 C24 121.6(3) . . ?
C26 C25 H25 119.2 . . ?
C25 C26 H26 119.6 . . ?
C25 C26 C27 120.7(3) . . ?
C27 C26 H26 119.6 . . ?
C26 C27 H27 120.3 . . ?
C28 C27 C26 119.4(2) . . ?
C28 C27 H27 120.3 . . ?
C27 C28 H28 118.8 . . ?
C27 C28 C29 122.4(3) . . ?
C29 C28 H28 118.8 . . ?
C24 C29 C30 122.73(17) . . ?
C28 C29 C24 118.1(2) . . ?
C28 C29 C30 119.1(2) . . ?
O12 C30 C29 123.29(17) . . ?
O12 C30 C31 116.17(18) . . ?
C29 C30 C31 120.54(17) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O10 C32A H32A 109.5 . . ?
O10 C32A H32B 109.5 . . ?
O10 C32A H32C 109.5 . . ?
H32A C32A H32B 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
O10 C32B H32D 109.5 . . ?
O10 C32B H32E 109.5 . . ?
O10 C32B H32F 109.5 . . ?
H32D C32B H32E 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
O8 C33 C34 118.2(2) . . ?
O8 C33 C38 124.12(19) . . ?
C34 C33 C38 117.67(19) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 C33 121.2(3) . . ?
C35 C34 H34 119.4 . . ?
C34 C35 H35 119.6 . . ?
C34 C35 C36 120.9(3) . . ?
C36 C35 H35 119.6 . . ?
C35 C36 H36 120.0 . . ?
C37 C36 C35 120.0(3) . . ?
C37 C36 H36 120.0 . . ?
C36 C37 H37 119.1 . . ?
C36 C37 C38 121.8(3) . . ?
C38 C37 H37 119.1 . . ?
C33 C38 C39 123.20(18) . . ?
C37 C38 C33 118.3(2) . . ?
C37 C38 C39 118.5(2) . . ?
O9 C39 C38 124.39(19) . . ?
O9 C39 C40 115.2(2) . . ?
C38 C39 C40 120.4(2) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O10 H10 O11 0.91(4) 1.80(4) 2.686(2) 164(4) . yes
O7 H7 O8 0.955(19) 1.78(2) 2.704(2) 162(5) . yes
O13 H13 O14 0.86(5) 1.82(5) 2.663(2) 166(5) . yes
O16 H16 O5 0.82(6) 1.96(6) 2.745(2) 160(6) . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O11 C24 C25 -155.14(17) . . . . ?
Ni1 O11 C24 C29 24.6(3) . . . . ?
Ni1 O12 C30 C29 0.5(3) . . . . ?
Ni1 O12 C30 C31 -179.90(13) . . . . ?
Ni2 O8 C33 C34 171.55(17) . . . . ?
Ni2 O8 C33 C38 -9.0(3) . . . . ?
Ni2 O9 C39 C38 6.8(4) . . . . ?
Ni2 O9 C39 C40 -173.8(2) . . . . ?
Ni3 O14 C14 C15 170.43(16) . . . . ?
Ni3 O14 C14 C19 -9.5(3) . . . . ?
Ni3 O15 C20 C19 6.3(3) . . . . ?
Ni3 O15 C20 C21 -174.29(17) . . . . ?
Ni4 O5 C3 C4 170.24(14) . . . . ?
Ni4 O5 C3 C8 -7.8(3) . . . . ?
Ni4 O6 C9 C8 13.0(3) . . . . ?
Ni4 O6 C9 C10 -166.70(15) . . . . ?
O5 C3 C4 C5 -177.9(2) . . . . ?
O5 C3 C8 C7 176.71(19) . . . . ?
O5 C3 C8 C9 -1.3(3) . . . . ?
O8 C33 C34 C35 -176.4(3) . . . . ?
O8 C33 C38 C37 176.3(3) . . . . ?
O8 C33 C38 C39 -5.0(4) . . . . ?
O11 C24 C25 C26 179.3(2) . . . . ?
O11 C24 C29 C28 -179.9(2) . . . . ?
O11 C24 C29 C30 -0.4(3) . . . . ?
O14 C14 C15 C16 -178.7(2) . . . . ?
O14 C14 C19 C18 178.5(2) . . . . ?
O14 C14 C19 C20 -2.4(3) . . . . ?
C3 C4 C5 C6 0.8(4) . . . . ?
C3 C8 C9 O6 -1.2(3) . . . . ?
C3 C8 C9 C10 178.46(19) . . . . ?
C4 C3 C8 C7 -1.4(3) . . . . ?
C4 C3 C8 C9 -179.41(18) . . . . ?
C4 C5 C6 C7 -0.8(4) . . . . ?
C5 C6 C7 C8 -0.3(4) . . . . ?
C6 C7 C8 C3 1.4(3) . . . . ?
C6 C7 C8 C9 179.5(2) . . . . ?
C7 C8 C9 O6 -179.23(19) . . . . ?
C7 C8 C9 C10 0.4(3) . . . . ?
C8 C3 C4 C5 0.3(3) . . . . ?
C14 C15 C16 C17 0.3(5) . . . . ?
C14 C19 C20 O15 4.0(3) . . . . ?
C14 C19 C20 C21 -175.4(2) . . . . ?
C15 C14 C19 C18 -1.4(3) . . . . ?
C15 C14 C19 C20 177.7(2) . . . . ?
C15 C16 C17 C18 -1.6(5) . . . . ?
C16 C17 C18 C19 1.4(5) . . . . ?
C17 C18 C19 C14 0.1(4) . . . . ?
C17 C18 C19 C20 -179.0(3) . . . . ?
C18 C19 C20 O15 -176.9(2) . . . . ?
C18 C19 C20 C21 3.7(3) . . . . ?
C19 C14 C15 C16 1.2(4) . . . . ?
C24 C25 C26 C27 0.5(4) . . . . ?
C24 C29 C30 O12 -12.9(3) . . . . ?
C24 C29 C30 C31 167.58(19) . . . . ?
C25 C24 C29 C28 -0.2(3) . . . . ?
C25 C24 C29 C30 179.4(2) . . . . ?
C25 C26 C27 C28 0.1(5) . . . . ?
C26 C27 C28 C29 -0.8(4) . . . . ?
C27 C28 C29 C24 0.8(4) . . . . ?
C27 C28 C29 C30 -178.7(2) . . . . ?
C28 C29 C30 O12 166.7(2) . . . . ?
C28 C29 C30 C31 -12.9(3) . . . . ?
C29 C24 C25 C26 -0.4(4) . . . . ?
C33 C34 C35 C36 -1.4(6) . . . . ?
C33 C38 C39 O9 6.2(4) . . . . ?
C33 C38 C39 C40 -173.2(3) . . . . ?
C34 C33 C38 C37 -4.2(4) . . . . ?
C34 C33 C38 C39 174.4(2) . . . . ?
C34 C35 C36 C37 -1.1(8) . . . . ?
C35 C36 C37 C38 0.8(7) . . . . ?
C36 C37 C38 C33 1.9(6) . . . . ?
C36 C37 C38 C39 -176.8(4) . . . . ?
C37 C38 C39 O9 -175.2(3) . . . . ?
C37 C38 C39 C40 5.5(4) . . . . ?
C38 C33 C34 C35 4.1(4) . . . . ?

_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 2.401
_oxdiff_exptl_absorpt_empirical_full_min 0.743
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/methanol'
####################################################################### 
# 
# 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_ena015
_database_code_depnum_ccdc_archive 'CCDC 2367080'
loop_
_audit_author_name
_audit_author_address
'Christoph Janiak'
;University of Duesseldorf
Germany
;
_audit_update_record             
;
2025-01-06 deposited with the CCDC.	2025-01-23 downloaded from the CCDC.
;
_audit_creation_date             2023-06-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            
"tetrakis-[(μ₃-methanolato-κ³O:O:O)(aqua-\kO)(2-oxybenzophenonato-κ²O,O')nickel(II)] monohydrate"
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H56 Ni4 O16, H2 O'
_chemical_formula_sum            'C56 H58 Ni4 O17'
_chemical_formula_weight         1237.86
_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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.6867(17)
_cell_length_b                   13.294(3)
_cell_length_c                   18.419(4)
_cell_angle_alpha                76.144(9)
_cell_angle_beta                 74.388(10)
_cell_angle_gamma                82.908(7)
_cell_volume                     2670.5(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9078
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.35
_shelx_estimated_absorpt_T_max   0.892
_shelx_estimated_absorpt_T_min   0.542
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0688 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.7983.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.477
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            80855
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         2.329
_diffrn_reflns.reduction_process narrow--frame
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO PHOTON100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine--focus tube'
_diffrn_radiation_monochromator  'TRIUMPH curved--crystal'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10384
_reflns_number_total             12233
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX v4, Bruker AXS'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         12233
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0436
_refine_ls_restrained_S_all      1.181
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+7.2589P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0933
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O16(H16A,H16B)
2.b Rotating group:
 O14(H14A,H14B), O13(H13A,H13B), O15(H15A,H15B), O17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C9(H9), C4(H4), C5(H5), C39(H39), C2(H2), C41(H41), C31(H31),
 C44(H44), C15(H15), C35(H35), C12(H12), C48(H48), C43(H43), C36(H36), C42(H42),
  C3(H3), C28(H28), C30(H30), C22(H22), C37(H37), C11(H11), C29(H29), C16(H16),
 C38(H38), C52(H52), C26(H26), C10(H10), C51(H51), C49(H49), C18(H18), C25(H25),
  C17(H17), C50(H50), C24(H24), C23(H23)
2.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C54(H54A,H54B,
 H54C)
;
_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
Ni2 Ni 0.27428(3) 0.24822(3) 0.21988(2) 0.01965(8) Uani 1 1 d . . . . .
Ni3 Ni 0.36937(3) 0.37244(3) 0.30878(2) 0.01983(8) Uani 1 1 d . . . . .
Ni1 Ni 0.54622(3) 0.23845(3) 0.21331(2) 0.01983(8) Uani 1 1 d . . . . .
Ni4 Ni 0.37200(3) 0.13161(3) 0.35674(2) 0.02015(8) Uani 1 1 d . . . . .
O10 O 0.48669(16) 0.24718(14) 0.32737(10) 0.0183(4) Uani 1 1 d . . . . .
O9 O 0.40945(16) 0.34740(14) 0.19855(10) 0.0175(4) Uani 1 1 d . . . . .
O12 O 0.40996(17) 0.14082(14) 0.24052(10) 0.0182(4) Uani 1 1 d . . . . .
O2 O 0.59106(17) 0.23370(15) 0.10016(11) 0.0224(4) Uani 1 1 d . . . . .
O11 O 0.25535(16) 0.25770(14) 0.33155(10) 0.0185(4) Uani 1 1 d . . . . .
O1 O 0.66626(17) 0.12055(16) 0.23098(11) 0.0243(4) Uani 1 1 d . . . . .
O6 O 0.32017(18) 0.40026(15) 0.41617(11) 0.0238(4) Uani 1 1 d . . . . .
O4 O 0.29365(19) 0.23009(16) 0.11152(11) 0.0274(4) Uani 1 1 d . . . . .
O8 O 0.32614(19) 0.13464(16) 0.47089(11) 0.0266(4) Uani 1 1 d . . . . .
O5 O 0.49359(18) 0.47482(16) 0.28154(11) 0.0258(4) Uani 1 1 d . . . . .
O7 O 0.25276(19) 0.02702(15) 0.37671(11) 0.0247(4) Uani 1 1 d . . . . .
O3 O 0.14527(18) 0.36226(15) 0.20103(11) 0.0240(4) Uani 1 1 d . . . . .
O14 O 0.22605(18) 0.48191(16) 0.28156(12) 0.0268(4) Uani 1 1 d . . . . .
H14A H 0.186522 0.455639 0.257387 0.040 Uiso 1 1 d R U . . .
H14B H 0.255570 0.536659 0.248369 0.040 Uiso 1 1 d R U . . .
O13 O 0.66545(18) 0.35556(17) 0.19657(11) 0.0272(4) Uani 1 1 d . . . . .
H13A H 0.631561 0.400644 0.224386 0.041 Uiso 1 1 d R U . . .
H13B H 0.726300 0.328313 0.214877 0.041 Uiso 1 1 d R U . . .
O15 O 0.5183(2) 0.01901(17) 0.36449(12) 0.0313(5) Uani 1 1 d . . . . .
H15A H 0.579400 0.038092 0.326268 0.047 Uiso 1 1 d R U . . .
H15B H 0.500729 -0.039096 0.357423 0.047 Uiso 1 1 d R U . . .
O17 O 0.1521(2) 0.12712(17) 0.26110(13) 0.0313(5) Uani 1 1 d . . . . .
H17A H 0.165864 0.087017 0.303120 0.047 Uiso 1 1 d R U . . .
H17B H 0.167126 0.086988 0.228169 0.047 Uiso 1 1 d R U . . .
O16 O -0.0888(2) 0.2820(2) 0.21821(17) 0.0498(7) Uani 1 1 d G . . . .
H16A H -0.018428 0.300529 0.214821 0.075 Uiso 1 1 d G U . . .
H16B H -0.075160 0.229388 0.195897 0.075 Uiso 1 1 d G U . . .
C1 C 0.7639(2) 0.1039(2) 0.17948(15) 0.0212(5) Uani 1 1 d . . . . .
C40 C 0.2185(2) -0.0383(2) 0.44300(16) 0.0221(5) Uani 1 1 d . . . . .
C7 C 0.6821(2) 0.1913(2) 0.06377(15) 0.0200(5) Uani 1 1 d . . . . .
C33 C 0.3308(2) 0.4826(2) 0.43406(15) 0.0208(5) Uani 1 1 d . . . . .
C46 C 0.2463(3) 0.0843(2) 0.52113(15) 0.0225(5) Uani 1 1 d . . . . .
C8 C 0.6850(2) 0.1949(2) -0.01884(15) 0.0206(5) Uani 1 1 d . . . . .
C14 C 0.1525(2) 0.4248(2) 0.13223(16) 0.0236(6) Uani 1 1 d . . . . .
C34 C 0.2603(2) 0.4938(2) 0.51330(15) 0.0208(5) Uani 1 1 d . . . . .
C13 C 0.6376(3) 0.2843(2) -0.06090(16) 0.0253(6) Uani 1 1 d . . . . .
H13 H 0.609308 0.342683 -0.038284 0.030 Uiso 1 1 calc R U . . .
C45 C 0.2114(2) -0.0141(2) 0.51562(16) 0.0220(5) Uani 1 1 d . . . . .
C9 C 0.7253(3) 0.1091(2) -0.05254(17) 0.0263(6) Uani 1 1 d . . . . .
H9 H 0.757749 0.047914 -0.024355 0.032 Uiso 1 1 calc R U . . .
C4 C 0.9861(3) 0.0708(2) 0.07597(17) 0.0277(6) Uani 1 1 d . . . . .
H4 H 1.062055 0.063260 0.041721 0.033 Uiso 1 1 calc R U . . .
C5 C 0.8927(3) 0.1218(2) 0.04851(16) 0.0236(6) Uani 1 1 d . . . . .
H5 H 0.904288 0.146687 -0.005621 0.028 Uiso 1 1 calc R U . . .
C27 C 0.4821(2) 0.5568(2) 0.31066(15) 0.0209(5) Uani 1 1 d . . . . .
C32 C 0.4024(2) 0.5667(2) 0.38341(16) 0.0214(5) Uani 1 1 d . . . . .
C20 C 0.2555(2) 0.2886(2) 0.05839(16) 0.0231(6) Uani 1 1 d . . . . .
C6 C 0.7790(2) 0.1391(2) 0.09740(15) 0.0209(5) Uani 1 1 d . . . . .
C21 C 0.2617(3) 0.2437(2) -0.01009(16) 0.0259(6) Uani 1 1 d . . . . .
C39 C 0.1392(3) 0.4785(2) 0.53314(16) 0.0250(6) Uani 1 1 d . . . . .
H39 H 0.105007 0.457980 0.498058 0.030 Uiso 1 1 calc R U . . .
C2 C 0.8604(3) 0.0448(2) 0.20502(17) 0.0280(6) Uani 1 1 d . . . . .
H2 H 0.849917 0.014537 0.258438 0.034 Uiso 1 1 calc R U . . .
C47 C 0.1844(3) 0.1317(2) 0.58843(15) 0.0236(6) Uani 1 1 d . . . . .
C19 C 0.2048(3) 0.3943(2) 0.06097(16) 0.0246(6) Uani 1 1 d . . . . .
C41 C 0.1829(3) -0.1363(2) 0.44378(17) 0.0256(6) Uani 1 1 d . . . . .
H41 H 0.184028 -0.153278 0.396322 0.031 Uiso 1 1 calc R U . . .
C53 C 0.4349(3) 0.4294(2) 0.13248(16) 0.0238(6) Uani 1 1 d . . . . .
H53A H 0.457395 0.400947 0.085841 0.036 Uiso 1 1 calc R U . . .
H53B H 0.500738 0.466871 0.134565 0.036 Uiso 1 1 calc R U . . .
H53C H 0.364204 0.477254 0.131355 0.036 Uiso 1 1 calc R U . . .
C31 C 0.3924(3) 0.6625(2) 0.40625(18) 0.0290(6) Uani 1 1 d . . . . .
H31 H 0.338950 0.669721 0.453982 0.035 Uiso 1 1 calc R U . . .
C44 C 0.1745(3) -0.0907(2) 0.58385(17) 0.0253(6) Uani 1 1 d . . . . .
H44 H 0.171044 -0.075338 0.632206 0.030 Uiso 1 1 calc R U . . .
C55 C 0.5637(3) 0.2460(3) 0.37526(17) 0.0285(6) Uani 1 1 d . . . . .
H55A H 0.582751 0.317205 0.371370 0.043 Uiso 1 1 calc R U . . .
H55B H 0.637266 0.204426 0.358624 0.043 Uiso 1 1 calc R U . . .
H55C H 0.524502 0.215701 0.428912 0.043 Uiso 1 1 calc R U . . .
C15 C 0.1045(3) 0.5283(2) 0.12829(18) 0.0277(6) Uani 1 1 d . . . . .
H15 H 0.064328 0.549749 0.174790 0.033 Uiso 1 1 calc R U . . .
C56 C 0.4286(3) 0.0495(2) 0.21067(17) 0.0265(6) Uani 1 1 d . . . . .
H56A H 0.366719 0.001808 0.240557 0.040 Uiso 1 1 calc R U . . .
H56B H 0.506964 0.015894 0.214343 0.040 Uiso 1 1 calc R U . . .
H56C H 0.425081 0.067779 0.156483 0.040 Uiso 1 1 calc R U . . .
C54 C 0.1419(3) 0.2636(2) 0.38351(17) 0.0259(6) Uani 1 1 d . . . . .
H54A H 0.086068 0.307337 0.356175 0.039 Uiso 1 1 calc R U . . .
H54B H 0.148117 0.293710 0.425819 0.039 Uiso 1 1 calc R U . . .
H54C H 0.113026 0.193736 0.404464 0.039 Uiso 1 1 calc R U . . .
C35 C 0.3115(3) 0.5178(2) 0.56676(17) 0.0269(6) Uani 1 1 d . . . . .
H35 H 0.394535 0.526196 0.554370 0.032 Uiso 1 1 calc R U . . .
C12 C 0.6319(3) 0.2880(3) -0.13586(17) 0.0314(7) Uani 1 1 d . . . . .
H12 H 0.600393 0.349163 -0.164656 0.038 Uiso 1 1 calc R U . . .
C48 C 0.0638(3) 0.1186(2) 0.62279(17) 0.0287(6) Uani 1 1 d . . . . .
H48 H 0.021966 0.074655 0.606512 0.034 Uiso 1 1 calc R U . . .
C43 C 0.1435(3) -0.1862(2) 0.58245(18) 0.0299(6) Uani 1 1 d . . . . .
H43 H 0.120431 -0.236689 0.628976 0.036 Uiso 1 1 calc R U . . .
C36 C 0.2398(3) 0.5294(2) 0.63855(17) 0.0310(7) Uani 1 1 d . . . . .
H36 H 0.274548 0.544295 0.675534 0.037 Uiso 1 1 calc R U . . .
C42 C 0.1465(3) -0.2079(2) 0.51176(19) 0.0295(6) Uani 1 1 d . . . . .
H42 H 0.122979 -0.273149 0.510320 0.035 Uiso 1 1 calc R U . . .
C3 C 0.9688(3) 0.0297(3) 0.15524(18) 0.0298(6) Uani 1 1 d . . . . .
H3 H 1.032235 -0.008784 0.174715 0.036 Uiso 1 1 calc R U . . .
C28 C 0.5501(3) 0.6425(2) 0.26804(17) 0.0273(6) Uani 1 1 d . . . . .
H28 H 0.605970 0.636912 0.220790 0.033 Uiso 1 1 calc R U . . .
C30 C 0.4568(3) 0.7454(2) 0.36236(19) 0.0346(7) Uani 1 1 d . . . . .
H30 H 0.446867 0.809290 0.378567 0.041 Uiso 1 1 calc R U . . .
C22 C 0.1728(3) 0.2674(3) -0.04966(18) 0.0345(7) Uani 1 1 d . . . . .
H22 H 0.111492 0.319207 -0.037592 0.041 Uiso 1 1 calc R U . . .
C37 C 0.1188(3) 0.5193(2) 0.65629(17) 0.0297(6) Uani 1 1 d . . . . .
H37 H 0.070192 0.530346 0.704475 0.036 Uiso 1 1 calc R U . . .
C11 C 0.6721(3) 0.2024(3) -0.16878(18) 0.0339(7) Uani 1 1 d . . . . .
H11 H 0.668240 0.205076 -0.220079 0.041 Uiso 1 1 calc R U . . .
C29 C 0.5375(3) 0.7332(2) 0.29310(18) 0.0302(6) Uani 1 1 d . . . . .
H29 H 0.584647 0.788986 0.262800 0.036 Uiso 1 1 calc R U . . .
C16 C 0.1141(3) 0.5986(2) 0.05955(19) 0.0315(7) Uani 1 1 d . . . . .
H16 H 0.081677 0.667798 0.059381 0.038 Uiso 1 1 calc R U . . .
C38 C 0.0680(3) 0.4931(2) 0.60411(17) 0.0300(6) Uani 1 1 d . . . . .
H38 H -0.015165 0.485155 0.616706 0.036 Uiso 1 1 calc R U . . .
C52 C 0.2448(3) 0.1968(2) 0.61231(17) 0.0296(6) Uani 1 1 d . . . . .
H52 H 0.326429 0.207182 0.588102 0.035 Uiso 1 1 calc R U . . .
C26 C 0.3527(3) 0.1699(2) -0.02878(17) 0.0306(7) Uani 1 1 d . . . . .
H26 H 0.414009 0.153812 -0.002042 0.037 Uiso 1 1 calc R U . . .
C10 C 0.7177(3) 0.1133(3) -0.12707(18) 0.0328(7) Uani 1 1 d . . . . .
H10 H 0.744138 0.054641 -0.149562 0.039 Uiso 1 1 calc R U . . .
C51 C 0.1857(3) 0.2464(3) 0.67148(19) 0.0353(7) Uani 1 1 d . . . . .
H51 H 0.227397 0.289146 0.688816 0.042 Uiso 1 1 calc R U . . .
C49 C 0.0049(3) 0.1704(3) 0.68119(18) 0.0343(7) Uani 1 1 d . . . . .
H49 H -0.077407 0.162179 0.704469 0.041 Uiso 1 1 calc R U . . .
C18 C 0.2133(3) 0.4696(3) -0.00896(18) 0.0310(7) Uani 1 1 d . . . . .
H18 H 0.249873 0.449434 -0.056457 0.037 Uiso 1 1 calc R U . . .
C25 C 0.3537(4) 0.1195(3) -0.08699(19) 0.0400(8) Uani 1 1 d . . . . .
H25 H 0.416648 0.069768 -0.100787 0.048 Uiso 1 1 calc R U . . .
C17 C 0.1706(3) 0.5704(3) -0.01019(19) 0.0361(7) Uani 1 1 d . . . . .
H17 H 0.179316 0.620077 -0.057627 0.043 Uiso 1 1 calc R U . . .
C50 C 0.0657(3) 0.2335(3) 0.70525(18) 0.0380(8) Uani 1 1 d . . . . .
H50 H 0.025115 0.268354 0.745215 0.046 Uiso 1 1 calc R U . . .
C24 C 0.2630(4) 0.1416(3) -0.12490(18) 0.0423(9) Uani 1 1 d . . . . .
H24 H 0.262723 0.105526 -0.163550 0.051 Uiso 1 1 calc R U . . .
C23 C 0.1735(4) 0.2157(3) -0.10677(19) 0.0432(9) Uani 1 1 d . . . . .
H23 H 0.112063 0.231399 -0.133399 0.052 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 O9 2.0785(19) . ?
Ni2 O12 2.0501(19) . ?
Ni2 O11 2.0415(18) . ?
Ni2 O4 2.017(2) . ?
Ni2 O3 2.039(2) . ?
Ni2 O17 2.146(2) . ?
Ni3 O10 2.0458(19) . ?
Ni3 O9 2.0557(18) . ?
Ni3 O11 2.0428(19) . ?
Ni3 O6 2.0163(19) . ?
Ni3 O5 1.995(2) . ?
Ni3 O14 2.162(2) . ?
Ni1 O10 2.0545(18) . ?
Ni1 O9 2.0495(18) . ?
Ni1 O12 2.0594(19) . ?
Ni1 O2 2.0221(19) . ?
Ni1 O1 1.997(2) . ?
Ni1 O13 2.130(2) . ?
Ni4 O10 2.0421(19) . ?
Ni4 O12 2.0422(18) . ?
Ni4 O11 2.0705(19) . ?
Ni4 O8 2.034(2) . ?
Ni4 O7 1.992(2) . ?
Ni4 O15 2.141(2) . ?
O10 C55 1.417(3) . ?
O9 C53 1.417(3) . ?
O12 C56 1.419(3) . ?
O2 C7 1.244(3) . ?
O11 C54 1.417(3) . ?
O1 C1 1.306(3) . ?
O6 C33 1.245(3) . ?
O4 C20 1.244(3) . ?
O8 C46 1.252(3) . ?
O5 C27 1.303(3) . ?
O7 C40 1.312(3) . ?
O3 C14 1.327(3) . ?
O14 H14A 0.8710 . ?
O14 H14B 0.8706 . ?
O13 H13A 0.8705 . ?
O13 H13B 0.8704 . ?
O15 H15A 0.8708 . ?
O15 H15B 0.8704 . ?
O17 H17A 0.8703 . ?
O17 H17B 0.8705 . ?
O16 H16A 0.8697 . ?
O16 H16B 0.8704 . ?
C1 C6 1.440(4) . ?
C1 C2 1.415(4) . ?
C40 C45 1.428(4) . ?
C40 C41 1.412(4) . ?
C7 C8 1.502(4) . ?
C7 C6 1.458(4) . ?
C33 C34 1.503(4) . ?
C33 C32 1.460(4) . ?
C46 C45 1.452(4) . ?
C46 C47 1.495(4) . ?
C8 C13 1.395(4) . ?
C8 C9 1.400(4) . ?
C14 C19 1.423(4) . ?
C14 C15 1.413(4) . ?
C34 C39 1.391(4) . ?
C34 C35 1.394(4) . ?
C13 H13 0.9500 . ?
C13 C12 1.389(4) . ?
C45 C44 1.416(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.363(4) . ?
C4 C3 1.399(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.418(4) . ?
C27 C32 1.436(4) . ?
C27 C28 1.416(4) . ?
C32 C31 1.417(4) . ?
C20 C21 1.501(4) . ?
C20 C19 1.462(4) . ?
C21 C22 1.388(4) . ?
C21 C26 1.386(4) . ?
C39 H39 0.9500 . ?
C39 C38 1.391(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.373(4) . ?
C47 C48 1.395(4) . ?
C47 C52 1.393(4) . ?
C19 C18 1.417(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.377(4) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C31 H31 0.9500 . ?
C31 C30 1.373(4) . ?
C44 H44 0.9500 . ?
C44 C43 1.370(4) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C15 H15 0.9500 . ?
C15 C16 1.368(4) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C35 H35 0.9500 . ?
C35 C36 1.394(4) . ?
C12 H12 0.9500 . ?
C12 C11 1.389(5) . ?
C48 H48 0.9500 . ?
C48 C49 1.394(4) . ?
C43 H43 0.9500 . ?
C43 C42 1.390(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.378(5) . ?
C42 H42 0.9500 . ?
C3 H3 0.9500 . ?
C28 H28 0.9500 . ?
C28 C29 1.369(4) . ?
C30 H30 0.9500 . ?
C30 C29 1.399(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.386(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.384(4) . ?
C11 H11 0.9500 . ?
C11 C10 1.380(5) . ?
C29 H29 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.393(5) . ?
C38 H38 0.9500 . ?
C52 H52 0.9500 . ?
C52 C51 1.388(4) . ?
C26 H26 0.9500 . ?
C26 C25 1.391(4) . ?
C10 H10 0.9500 . ?
C51 H51 0.9500 . ?
C51 C50 1.386(5) . ?
C49 H49 0.9500 . ?
C49 C50 1.378(5) . ?
C18 H18 0.9500 . ?
C18 C17 1.368(5) . ?
C25 H25 0.9500 . ?
C25 C24 1.386(6) . ?
C17 H17 0.9500 . ?
C50 H50 0.9500 . ?
C24 H24 0.9500 . ?
C24 C23 1.375(6) . ?
C23 H23 0.9500 . ?

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
O9 Ni2 O17 167.69(8) . . ?
O12 Ni2 O9 80.54(7) . . ?
O12 Ni2 O17 89.59(8) . . ?
O11 Ni2 O9 82.79(7) . . ?
O11 Ni2 O12 83.44(7) . . ?
O11 Ni2 O17 88.82(8) . . ?
O4 Ni2 O9 99.14(8) . . ?
O4 Ni2 O12 94.31(8) . . ?
O4 Ni2 O11 176.77(8) . . ?
O4 Ni2 O3 87.80(8) . . ?
O4 Ni2 O17 88.86(9) . . ?
O3 Ni2 O9 95.91(8) . . ?
O3 Ni2 O12 176.11(8) . . ?
O3 Ni2 O11 94.58(8) . . ?
O3 Ni2 O17 93.72(9) . . ?
O10 Ni3 O9 84.20(7) . . ?
O10 Ni3 O14 167.62(8) . . ?
O9 Ni3 O14 88.88(7) . . ?
O11 Ni3 O10 81.58(8) . . ?
O11 Ni3 O9 83.33(7) . . ?
O11 Ni3 O14 87.43(8) . . ?
O6 Ni3 O10 98.75(8) . . ?
O6 Ni3 O9 176.55(8) . . ?
O6 Ni3 O11 95.30(8) . . ?
O6 Ni3 O14 87.89(8) . . ?
O5 Ni3 O10 93.59(8) . . ?
O5 Ni3 O9 92.99(8) . . ?
O5 Ni3 O11 174.18(8) . . ?
O5 Ni3 O6 88.62(8) . . ?
O5 Ni3 O14 97.03(9) . . ?
O10 Ni1 O12 83.68(7) . . ?
O10 Ni1 O13 89.09(8) . . ?
O9 Ni1 O10 84.14(7) . . ?
O9 Ni1 O12 81.00(7) . . ?
O9 Ni1 O13 91.63(8) . . ?
O12 Ni1 O13 170.14(8) . . ?
O2 Ni1 O10 175.28(8) . . ?
O2 Ni1 O9 91.61(7) . . ?
O2 Ni1 O12 93.64(8) . . ?
O2 Ni1 O13 93.10(8) . . ?
O1 Ni1 O10 95.13(8) . . ?
O1 Ni1 O9 173.69(8) . . ?
O1 Ni1 O12 92.68(8) . . ?
O1 Ni1 O2 88.86(8) . . ?
O1 Ni1 O13 94.63(9) . . ?
O10 Ni4 O12 84.43(7) . . ?
O10 Ni4 O11 81.00(7) . . ?
O10 Ni4 O15 89.47(8) . . ?
O12 Ni4 O11 82.91(7) . . ?
O12 Ni4 O15 89.78(8) . . ?
O11 Ni4 O15 168.48(8) . . ?
O8 Ni4 O10 93.92(8) . . ?
O8 Ni4 O12 175.00(8) . . ?
O8 Ni4 O11 92.17(8) . . ?
O8 Ni4 O15 94.93(9) . . ?
O7 Ni4 O10 174.13(8) . . ?
O7 Ni4 O12 91.45(8) . . ?
O7 Ni4 O11 94.38(8) . . ?
O7 Ni4 O8 89.84(8) . . ?
O7 Ni4 O15 94.69(9) . . ?
Ni3 O10 Ni1 95.22(8) . . ?
Ni4 O10 Ni3 99.03(8) . . ?
Ni4 O10 Ni1 95.29(7) . . ?
C55 O10 Ni3 119.56(17) . . ?
C55 O10 Ni1 123.34(17) . . ?
C55 O10 Ni4 118.68(17) . . ?
Ni3 O9 Ni2 95.54(7) . . ?
Ni1 O9 Ni2 98.84(8) . . ?
Ni1 O9 Ni3 95.07(8) . . ?
C53 O9 Ni2 123.18(16) . . ?
C53 O9 Ni3 122.11(16) . . ?
C53 O9 Ni1 116.18(16) . . ?
Ni2 O12 Ni1 99.45(8) . . ?
Ni4 O12 Ni2 96.37(7) . . ?
Ni4 O12 Ni1 95.13(7) . . ?
C56 O12 Ni2 120.11(16) . . ?
C56 O12 Ni1 119.67(17) . . ?
C56 O12 Ni4 120.64(17) . . ?
C7 O2 Ni1 127.91(18) . . ?
Ni2 O11 Ni3 97.09(8) . . ?
Ni2 O11 Ni4 95.75(7) . . ?
Ni3 O11 Ni4 98.21(8) . . ?
C54 O11 Ni2 121.82(17) . . ?
C54 O11 Ni3 120.10(16) . . ?
C54 O11 Ni4 118.44(17) . . ?
C1 O1 Ni1 124.04(18) . . ?
C33 O6 Ni3 126.01(18) . . ?
C20 O4 Ni2 128.58(19) . . ?
C46 O8 Ni4 125.22(18) . . ?
C27 O5 Ni3 124.24(17) . . ?
C40 O7 Ni4 123.76(18) . . ?
C14 O3 Ni2 121.46(17) . . ?
Ni3 O14 H14A 109.5 . . ?
Ni3 O14 H14B 109.5 . . ?
H14A O14 H14B 104.5 . . ?
Ni1 O13 H13A 109.6 . . ?
Ni1 O13 H13B 109.4 . . ?
H13A O13 H13B 104.5 . . ?
Ni4 O15 H15A 109.6 . . ?
Ni4 O15 H15B 109.2 . . ?
H15A O15 H15B 104.5 . . ?
Ni2 O17 H17A 109.3 . . ?
Ni2 O17 H17B 109.1 . . ?
H17A O17 H17B 104.5 . . ?
H16A O16 H16B 104.5 . . ?
O1 C1 C6 124.2(3) . . ?
O1 C1 C2 118.6(2) . . ?
C2 C1 C6 117.2(2) . . ?
O7 C40 C45 123.2(3) . . ?
O7 C40 C41 119.2(3) . . ?
C41 C40 C45 117.6(3) . . ?
O2 C7 C8 115.0(2) . . ?
O2 C7 C6 123.9(2) . . ?
C6 C7 C8 121.1(2) . . ?
O6 C33 C34 115.4(2) . . ?
O6 C33 C32 124.8(2) . . ?
C32 C33 C34 119.7(2) . . ?
O8 C46 C45 123.2(2) . . ?
O8 C46 C47 116.6(3) . . ?
C45 C46 C47 120.1(2) . . ?
C13 C8 C7 118.4(2) . . ?
C13 C8 C9 119.4(3) . . ?
C9 C8 C7 122.0(3) . . ?
O3 C14 C19 124.1(3) . . ?
O3 C14 C15 118.8(3) . . ?
C15 C14 C19 117.0(3) . . ?
C39 C34 C33 117.6(2) . . ?
C39 C34 C35 119.6(3) . . ?
C35 C34 C33 122.8(3) . . ?
C8 C13 H13 120.0 . . ?
C12 C13 C8 120.0(3) . . ?
C12 C13 H13 120.0 . . ?
C40 C45 C46 121.9(3) . . ?
C44 C45 C40 118.7(3) . . ?
C44 C45 C46 119.3(3) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0(3) . . ?
C10 C9 H9 120.0 . . ?
C5 C4 H4 120.4 . . ?
C5 C4 C3 119.1(3) . . ?
C3 C4 H4 120.4 . . ?
C4 C5 H5 118.6 . . ?
C4 C5 C6 122.7(3) . . ?
C6 C5 H5 118.6 . . ?
O5 C27 C32 123.9(2) . . ?
O5 C27 C28 118.7(2) . . ?
C28 C27 C32 117.4(2) . . ?
C27 C32 C33 122.6(2) . . ?
C31 C32 C33 119.0(2) . . ?
C31 C32 C27 118.3(3) . . ?
O4 C20 C21 115.9(3) . . ?
O4 C20 C19 123.6(3) . . ?
C19 C20 C21 120.5(3) . . ?
C1 C6 C7 122.3(2) . . ?
C5 C6 C1 118.0(3) . . ?
C5 C6 C7 119.7(2) . . ?
C22 C21 C20 121.3(3) . . ?
C26 C21 C20 118.4(3) . . ?
C26 C21 C22 120.1(3) . . ?
C34 C39 H39 119.8 . . ?
C34 C39 C38 120.3(3) . . ?
C38 C39 H39 119.8 . . ?
C1 C2 H2 118.9 . . ?
C3 C2 C1 122.2(3) . . ?
C3 C2 H2 118.9 . . ?
C48 C47 C46 120.3(3) . . ?
C52 C47 C46 119.6(3) . . ?
C52 C47 C48 119.8(3) . . ?
C14 C19 C20 121.6(3) . . ?
C18 C19 C14 119.1(3) . . ?
C18 C19 C20 119.3(3) . . ?
C40 C41 H41 119.2 . . ?
C42 C41 C40 121.5(3) . . ?
C42 C41 H41 119.2 . . ?
O9 C53 H53A 109.5 . . ?
O9 C53 H53B 109.5 . . ?
O9 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C32 C31 H31 118.6 . . ?
C30 C31 C32 122.8(3) . . ?
C30 C31 H31 118.6 . . ?
C45 C44 H44 118.9 . . ?
C43 C44 C45 122.2(3) . . ?
C43 C44 H44 118.9 . . ?
O10 C55 H55A 109.5 . . ?
O10 C55 H55B 109.5 . . ?
O10 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 122.0(3) . . ?
C16 C15 H15 119.0 . . ?
O12 C56 H56A 109.5 . . ?
O12 C56 H56B 109.5 . . ?
O12 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O11 C54 H54A 109.5 . . ?
O11 C54 H54B 109.5 . . ?
O11 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C34 C35 H35 120.3 . . ?
C34 C35 C36 119.5(3) . . ?
C36 C35 H35 120.3 . . ?
C13 C12 H12 120.0 . . ?
C13 C12 C11 120.1(3) . . ?
C11 C12 H12 120.0 . . ?
C47 C48 H48 120.2 . . ?
C49 C48 C47 119.6(3) . . ?
C49 C48 H48 120.2 . . ?
C44 C43 H43 120.6 . . ?
C44 C43 C42 118.8(3) . . ?
C42 C43 H43 120.6 . . ?
C35 C36 H36 119.7 . . ?
C37 C36 C35 120.5(3) . . ?
C37 C36 H36 119.7 . . ?
C41 C42 C43 121.1(3) . . ?
C41 C42 H42 119.5 . . ?
C43 C42 H42 119.5 . . ?
C4 C3 H3 119.8 . . ?
C2 C3 C4 120.3(3) . . ?
C2 C3 H3 119.8 . . ?
C27 C28 H28 119.1 . . ?
C29 C28 C27 121.8(3) . . ?
C29 C28 H28 119.1 . . ?
C31 C30 H30 120.9 . . ?
C31 C30 C29 118.2(3) . . ?
C29 C30 H30 120.9 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.1(3) . . ?
C23 C22 H22 120.0 . . ?
C36 C37 H37 119.9 . . ?
C36 C37 C38 120.2(3) . . ?
C38 C37 H37 119.9 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 C12 120.1(3) . . ?
C10 C11 H11 120.0 . . ?
C28 C29 C30 121.4(3) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C15 C16 H16 119.5 . . ?
C15 C16 C17 121.1(3) . . ?
C17 C16 H16 119.5 . . ?
C39 C38 H38 120.1 . . ?
C37 C38 C39 119.8(3) . . ?
C37 C38 H38 120.1 . . ?
C47 C52 H52 120.0 . . ?
C51 C52 C47 120.0(3) . . ?
C51 C52 H52 120.0 . . ?
C21 C26 H26 120.3 . . ?
C21 C26 C25 119.5(3) . . ?
C25 C26 H26 120.3 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.4(3) . . ?
C11 C10 H10 119.8 . . ?
C52 C51 H51 120.0 . . ?
C50 C51 C52 120.0(3) . . ?
C50 C51 H51 120.0 . . ?
C48 C49 H49 119.9 . . ?
C50 C49 C48 120.2(3) . . ?
C50 C49 H49 119.9 . . ?
C19 C18 H18 119.0 . . ?
C17 C18 C19 122.1(3) . . ?
C17 C18 H18 119.0 . . ?
C26 C25 H25 119.9 . . ?
C24 C25 C26 120.2(3) . . ?
C24 C25 H25 119.9 . . ?
C16 C17 H17 120.7 . . ?
C18 C17 C16 118.6(3) . . ?
C18 C17 H17 120.7 . . ?
C51 C50 H50 119.8 . . ?
C49 C50 C51 120.4(3) . . ?
C49 C50 H50 119.8 . . ?
C25 C24 H24 119.9 . . ?
C23 C24 C25 120.2(3) . . ?
C23 C24 H24 119.9 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 120.0(3) . . ?
C24 C23 H23 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni2 O4 C20 C21 -167.36(19) . . . . ?
Ni2 O4 C20 C19 11.4(4) . . . . ?
Ni2 O3 C14 C19 33.5(4) . . . . ?
Ni2 O3 C14 C15 -147.3(2) . . . . ?
Ni3 O6 C33 C34 165.04(18) . . . . ?
Ni3 O6 C33 C32 -13.1(4) . . . . ?
Ni3 O5 C27 C32 23.2(4) . . . . ?
Ni3 O5 C27 C28 -155.6(2) . . . . ?
Ni1 O2 C7 C8 175.66(17) . . . . ?
Ni1 O2 C7 C6 -2.8(4) . . . . ?
Ni1 O1 C1 C6 -24.9(4) . . . . ?
Ni1 O1 C1 C2 157.2(2) . . . . ?
Ni4 O8 C46 C45 28.5(4) . . . . ?
Ni4 O8 C46 C47 -150.3(2) . . . . ?
Ni4 O7 C40 C45 32.3(4) . . . . ?
Ni4 O7 C40 C41 -149.8(2) . . . . ?
O2 C7 C8 C13 37.3(4) . . . . ?
O2 C7 C8 C9 -137.8(3) . . . . ?
O2 C7 C6 C1 19.5(4) . . . . ?
O2 C7 C6 C5 -160.5(3) . . . . ?
O1 C1 C6 C7 -4.4(4) . . . . ?
O1 C1 C6 C5 175.6(3) . . . . ?
O1 C1 C2 C3 -175.5(3) . . . . ?
O6 C33 C34 C39 -52.1(4) . . . . ?
O6 C33 C34 C35 127.3(3) . . . . ?
O6 C33 C32 C27 -9.1(4) . . . . ?
O6 C33 C32 C31 170.3(3) . . . . ?
O4 C20 C21 C22 143.4(3) . . . . ?
O4 C20 C21 C26 -30.6(4) . . . . ?
O4 C20 C19 C14 -25.2(4) . . . . ?
O4 C20 C19 C18 151.5(3) . . . . ?
O8 C46 C45 C40 -30.9(4) . . . . ?
O8 C46 C45 C44 146.1(3) . . . . ?
O8 C46 C47 C48 145.4(3) . . . . ?
O8 C46 C47 C52 -28.8(4) . . . . ?
O5 C27 C32 C33 3.5(4) . . . . ?
O5 C27 C32 C31 -175.9(3) . . . . ?
O5 C27 C28 C29 176.3(3) . . . . ?
O7 C40 C45 C46 -2.3(4) . . . . ?
O7 C40 C45 C44 -179.4(3) . . . . ?
O7 C40 C41 C42 179.8(3) . . . . ?
O3 C14 C19 C20 0.2(4) . . . . ?
O3 C14 C19 C18 -176.5(3) . . . . ?
O3 C14 C15 C16 176.6(3) . . . . ?
C1 C2 C3 C4 -1.8(5) . . . . ?
C40 C45 C44 C43 -1.1(4) . . . . ?
C40 C41 C42 C43 0.0(5) . . . . ?
C7 C8 C13 C12 -175.9(3) . . . . ?
C7 C8 C9 C10 175.0(3) . . . . ?
C33 C34 C39 C38 -176.7(3) . . . . ?
C33 C34 C35 C36 178.5(3) . . . . ?
C33 C32 C31 C30 179.6(3) . . . . ?
C46 C45 C44 C43 -178.2(3) . . . . ?
C46 C47 C48 C49 -174.6(3) . . . . ?
C46 C47 C52 C51 175.8(3) . . . . ?
C8 C7 C6 C1 -158.9(3) . . . . ?
C8 C7 C6 C5 21.1(4) . . . . ?
C8 C13 C12 C11 0.7(5) . . . . ?
C8 C9 C10 C11 0.9(5) . . . . ?
C14 C19 C18 C17 -1.4(5) . . . . ?
C14 C15 C16 C17 1.0(5) . . . . ?
C34 C33 C32 C27 172.8(2) . . . . ?
C34 C33 C32 C31 -7.7(4) . . . . ?
C34 C39 C38 C37 -2.4(5) . . . . ?
C34 C35 C36 C37 -1.3(5) . . . . ?
C13 C8 C9 C10 -0.1(4) . . . . ?
C13 C12 C11 C10 0.1(5) . . . . ?
C45 C40 C41 C42 -2.2(4) . . . . ?
C45 C46 C47 C48 -33.5(4) . . . . ?
C45 C46 C47 C52 152.4(3) . . . . ?
C45 C44 C43 C42 -1.2(5) . . . . ?
C9 C8 C13 C12 -0.7(4) . . . . ?
C4 C5 C6 C1 2.0(4) . . . . ?
C4 C5 C6 C7 -178.0(3) . . . . ?
C5 C4 C3 C2 -3.0(5) . . . . ?
C27 C32 C31 C30 -0.9(5) . . . . ?
C27 C28 C29 C30 0.2(5) . . . . ?
C32 C33 C34 C39 126.1(3) . . . . ?
C32 C33 C34 C35 -54.4(4) . . . . ?
C32 C27 C28 C29 -2.7(4) . . . . ?
C32 C31 C30 C29 -1.6(5) . . . . ?
C20 C21 C22 C23 -172.4(3) . . . . ?
C20 C21 C26 C25 173.6(3) . . . . ?
C20 C19 C18 C17 -178.2(3) . . . . ?
C6 C1 C2 C3 6.5(4) . . . . ?
C6 C7 C8 C13 -144.1(3) . . . . ?
C6 C7 C8 C9 40.7(4) . . . . ?
C21 C20 C19 C14 153.5(3) . . . . ?
C21 C20 C19 C18 -29.7(4) . . . . ?
C21 C22 C23 C24 -0.8(5) . . . . ?
C21 C26 C25 C24 -1.2(5) . . . . ?
C39 C34 C35 C36 -2.0(4) . . . . ?
C2 C1 C6 C7 173.6(3) . . . . ?
C2 C1 C6 C5 -6.4(4) . . . . ?
C47 C46 C45 C40 147.9(3) . . . . ?
C47 C46 C45 C44 -35.1(4) . . . . ?
C47 C48 C49 C50 -0.5(5) . . . . ?
C47 C52 C51 C50 -1.9(5) . . . . ?
C19 C14 C15 C16 -4.1(4) . . . . ?
C19 C20 C21 C22 -35.4(4) . . . . ?
C19 C20 C21 C26 150.6(3) . . . . ?
C19 C18 C17 C16 -1.8(5) . . . . ?
C41 C40 C45 C46 179.8(3) . . . . ?
C41 C40 C45 C44 2.8(4) . . . . ?
C31 C30 C29 C28 2.0(5) . . . . ?
C44 C43 C42 C41 1.8(5) . . . . ?
C15 C14 C19 C20 -179.0(3) . . . . ?
C15 C14 C19 C18 4.2(4) . . . . ?
C15 C16 C17 C18 2.1(5) . . . . ?
C35 C34 C39 C38 3.9(4) . . . . ?
C35 C36 C37 C38 2.8(5) . . . . ?
C12 C11 C10 C9 -0.9(5) . . . . ?
C48 C47 C52 C51 1.6(5) . . . . ?
C48 C49 C50 C51 0.3(5) . . . . ?
C36 C37 C38 C39 -1.0(5) . . . . ?
C3 C4 C5 C6 2.8(5) . . . . ?
C28 C27 C32 C33 -177.6(3) . . . . ?
C28 C27 C32 C31 3.0(4) . . . . ?
C22 C21 C26 C25 -0.5(5) . . . . ?
C52 C47 C48 C49 -0.4(4) . . . . ?
C52 C51 C50 C49 0.9(5) . . . . ?
C26 C21 C22 C23 1.5(5) . . . . ?
C26 C25 C24 C23 1.9(5) . . . . ?
C25 C24 C23 C22 -0.9(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/methanol'
