#------------------------------------------------------------------------------
#$Date: 2025-02-08 04:16:43 +0200 (Sat, 08 Feb 2025) $
#$Revision: 297638 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/99/7249922.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7249922
loop_
_publ_author_name
'Haque, Imdadul'
'Enamullah, Mohammed'
'Jhumur, Nisat Taslum'
'Sidhu, Baldeep K.'
'Herbert, David E.'
'Haj Hassani Sohi, Takin'
'Havlíček, Lubomír'
'Nemec, Ivan'
'Janiak, Christoph'
_publ_section_title
;
 Ferromagnetically coupled tetranuclear Ni(ii)-2-oxy-aceto- or
 benzo-phenonate complexes
;
_journal_issue                   6
_journal_name_full               'RSC Advances'
_journal_page_first              4250
_journal_page_last               4261
_journal_paper_doi               10.1039/D4RA08700C
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C40 H56 Ni4 O16'
_chemical_formula_sum            'C40 H56 Ni4 O16'
_chemical_formula_weight         1027.68
_chemical_name_common
tetrakis-[(μ₃-methanolato-κ³O:O:O)(methanol-\kO)(2-oxyacetophenone-κ²O,O')nickel(II)]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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)
;
_audit_update_record
;
2024-07-01 deposited with the CCDC.	2025-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.2175(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.08705(9)
_cell_length_b                   15.15100(7)
_cell_length_c                   15.82527(8)
_cell_measurement_reflns_used    95263
_cell_measurement_temperature    298.60(14)
_cell_measurement_theta_max      76.1070
_cell_measurement_theta_min      2.3110
_cell_volume                     4557.51(4)
_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)'
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_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_crystal_colour            'clear green'
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/methanol'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.041
_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_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0318
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8883
_reflns_number_total             9486
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra08700c2.cif
_cod_data_source_block           nil104_2
_cod_database_code               7249922
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C40H56Ni4O16
_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.
;
_shelx_estimated_absorpt_t_max   0.744
_shelx_estimated_absorpt_t_min   0.521
_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)
;
_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
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'
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 . . .
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'
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
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_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_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) . . . . ?
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
