#------------------------------------------------------------------------------
#$Date: 2022-04-12 01:18:21 +0300 (Tue, 12 Apr 2022) $
#$Revision: 274454 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/67/1566781.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_1566781
loop_
_publ_author_name
'Somerville, Rosie J.'
'Campos, Jesús'
'Carmona, Ernesto'
'Grabowsky, Simon'
'Malaspina, Lorraine A.'
'Balcells, David'
'Hevia, Eva'
'Nova, Ainara'
'Pérez-Jiménez, Marina'
'Borys, Andryj M.'
_publ_section_title
;
 Unmasking the constitution and bonding of the proposed lithium nickelate
 “Li3NiPh3(solv)3”: Revealing the hidden C6H4 ligand
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01244H
_journal_year                    2022
_chemical_formula_moiety         'C80 H126 Na6 Ni2 O6'
_chemical_formula_sum            'C80 H126 Na6 Ni2 O6'
_chemical_formula_weight         1439.13
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-10T17:48:57-00:00
_audit_update_record
;
2021-12-08 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.7306(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.45144(13)
_cell_length_b                   17.82545(10)
_cell_length_c                   22.25202(14)
_cell_measurement_reflns_used    72089
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.496
_cell_measurement_theta_min      3.296
_cell_volume                     8009.22(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
        List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -94.00  -8.00   0.50    0.35    --  -23.00 -57.00 -67.00  172
  2  ω    -38.00  50.00   0.50    0.35    --  -23.00  57.00  74.00  176
  3  ω    -23.00  63.00   0.50    0.35    --   47.95 -57.00 -67.00  172
  4  ω     33.00 119.00   0.50    0.35    --   47.95  57.00  74.00  172
  5  ω     98.00 177.00   0.50    2.00    --  113.25  57.00  74.00  158
  6  ω    -95.00   0.00   0.50    0.35    --  -23.00 -77.00-180.00  190
  7  ω    -70.00 -12.00   0.50    0.35    --  -23.00 125.00 120.00  116
  8  ω    -95.00 -10.00   0.50    0.35    --  -23.00 -45.00 -30.00  170
  9  ω    -70.00 -12.00   0.50    0.35    --  -23.00 125.00  90.00  116
 10  ω     25.00 120.00   0.50    0.35    --   47.95  77.00  30.00  190
 11  ω    -26.00  23.00   0.50    0.35    --   47.95 -19.00-180.00   98
 12  ω     42.00 141.00   0.50    2.00    --  113.25 -88.00  52.49  198
 13  ω     42.00  68.00   0.50    2.00    --  113.25 -61.00  90.00   52
 14  ω     42.00 106.00   0.50    2.00    --  113.25 -94.00 -30.00  128
 15  ω     98.00 177.00   0.50    2.00    --  113.25  58.00  42.51  158
 16  ω     91.00 177.00   0.50    2.00    --  113.25  77.00-180.00  172
 17  ω     97.00 177.00   0.50    2.00    --  113.25  61.00 -90.00  160
 18  ω     42.00 105.00   0.50    2.00    --  113.25 -92.00-104.65  126
 19  ω    101.00 177.00   0.50    2.00    --  113.25  45.00  30.00  152
 20  ω     97.00 177.00   0.50    2.00    --  113.25  61.00   0.00  160
 21  ω     97.00 177.00   0.50    2.00    --  113.25  61.00 120.00  160
 22  ω     42.00 106.00   0.50    2.00    --  113.25 -94.00-150.00  128
 23  ω    101.00 177.00   0.50    2.00    --  113.25  31.00  21.05  152
 24  ω    100.00 177.00   0.50    2.00    --  113.25  48.00 -34.62  154
 25  ω     42.00 102.00   0.50    2.00    --  113.25 -77.00  60.00  120
 26  ω     97.00 177.00   0.50    2.00    --  113.25  61.00-150.00  160
 27  ω    101.00 177.00   0.50    2.00    --  113.25  45.00-180.00  152
 28  ω     97.00 177.00   0.50    2.00    --  113.25  61.00  30.00  160
 29  ω     91.00 177.00   0.50    2.00    --  113.25  77.00 -30.00  172
 30  ω     42.00 102.00   0.50    2.00    --  113.25 -77.00 150.00  120
 31  ω     93.00 177.00   0.50    2.00    --  113.25  71.00-107.31  168
 32  ω     42.00  68.00   0.50    2.00    --  113.25 -61.00 120.00   52
 33  ω    101.00 177.00   0.50    2.00    --  113.25  30.00  30.00  152
 34  ω     42.00 102.00   0.50    2.00    --  113.25 -77.00-150.00  120
 35  ω     42.00  68.00   0.50    2.00    --  113.25 -61.00 150.00   52
 36  ω    101.00 177.00   0.50    2.00    --  113.25  43.00  36.70  152
 37  ω     93.00 177.00   0.50    2.00    --  113.25  71.00 -76.17  168
 38  ω     42.00  68.00   0.50    2.00    --  113.25 -61.00 -60.00   52
 39  ω     96.00 177.00   0.50    2.00    --  113.25  64.00  47.77  162
 40  ω     42.00 106.00   0.50    2.00    --  113.25 -94.00-120.00  128
 41  ω    100.00 177.00   0.50    2.00    --  113.25  15.00 -90.00  154
 42  ω     42.00  68.00   0.50    2.00    --  113.25 -61.00  60.00   52
 43  ω     42.00 102.00   0.50    2.00    --  113.25 -77.00   0.00  120
 44  ω     42.00 102.00   0.50    2.00    --  113.25 -77.00 120.00  120
 45  ω    101.00 177.00   0.50    2.00    --  113.25  45.00  60.00  152
 46  ω    101.00 177.00   0.50    2.00    --  113.25  30.00  60.00  152
 47  ω    106.00 177.00   0.50    2.00    --  113.25 102.00 -54.24  142
 48  ω    -70.00 -12.00   0.50    0.35    --  -23.00 125.00 -60.00  116
 49  ω     25.00 120.00   0.50    0.35    --   47.95  77.00 -30.00  190
 50  ω     -1.00  81.00   0.50    0.35    --   47.95 -99.00 -60.00  164
 51  ω     25.00 120.00   0.50    0.35    --   47.95  77.00 120.00  190
 52  ω     25.00 120.00   0.50    0.35    --   47.95  77.00 -60.00  190
 53  ω     25.00 120.00   0.50    0.35    --   47.95  77.00 150.00  190
 54  ω     25.00 120.00   0.50    0.35    --   47.95  77.00  90.00  190
 55  ω     -1.00  81.00   0.50    0.35    --   47.95 -99.00 120.00  164
 56  ω     25.00 120.00   0.50    0.35    --   47.95  77.00-120.00  190
 57  ω     25.00 120.00   0.50    0.35    --   47.95  77.00   0.00  190
 58  ω     36.00 121.00   0.50    0.35    --   47.95  38.00 -30.00  170
 59  ω     25.00 120.00   0.50    0.35    --   47.95  77.00-150.00  190
 60  ω     42.00  68.00   0.50    2.00    --  113.25 -61.00 -90.00   52
 61  ω     95.00 177.00   0.50    2.00    --  113.25  67.00 131.85  164
;
_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      0.0386938
_diffrn_orient_matrix_UB_12      -0.0582229
_diffrn_orient_matrix_UB_13      0.0497782
_diffrn_orient_matrix_UB_21      -0.0656476
_diffrn_orient_matrix_UB_22      -0.0315972
_diffrn_orient_matrix_UB_23      0.003143
_diffrn_orient_matrix_UB_31      -0.0032203
_diffrn_orient_matrix_UB_32      -0.0555127
_diffrn_orient_matrix_UB_33      -0.0540805
_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  0.0467
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            113505
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.498
_diffrn_reflns_theta_min         3.307
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.43875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8086
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0672P)²+12.1959P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0
_reflns_number_gt                7681
_reflns_number_total             8086
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc01244h5.cif
_cod_data_source_block           21EH115_AMB-502
_cod_original_cell_volume        8009.21(9)
_cod_database_code               1566781
_shelx_estimated_absorpt_t_min   0.763
_shelx_estimated_absorpt_t_max   0.847
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.449
_oxdiff_exptl_absorpt_empirical_full_min 0.602
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
        1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
        2. Restrained distances
 C37-C36 \\sim C37A-C36A
 with sigma of 0.002
        3. Rigid bond restraints
 C36, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3A, C38A, C39A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
        4. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
        5. Others
 Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C40A)=Sof(H40B)=Sof(H40C)=Sof(H40A)=
 Sof(O3A)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 1-FVAR(1)
 Sof(O3)=Sof(C38)=Sof(H38C)=Sof(H38D)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=
 Sof(C39)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40)=Sof(H40D)=Sof(H40E)=FVAR(1)
 Sof(O2A)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(C37A)=Sof(H37D)=Sof(H37E)=
 Sof(H37F)=Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C35A)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=1-FVAR(2)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=
 Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(O2)=Sof(C34)=Sof(H34C)=Sof(H34D)=FVAR(2)
        6.a Ternary CH refined with riding coordinates:
 C14(H14), C13(H13), C29(H29), C22(H22), C28(H28), C25(H25), C26(H26)
        6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C20(H20A,H20B), C16(H16A,H16B), C30(H30A,H30B), C19(H19A,
 H19B), C27(H27A,H27B), C23(H23A,H23B), C32(H32A,H32B), C38A(H38A,H38B),
 C34A(H34A,H34B), C38(H38C,H38D), C24(H24A,H24B), C36(H36A,H36B), C21(H21A,
 H21B), C40(H40D,H40E), C36A(H36C,H36D), C34(H34C,H34D)
        6.c Me refined with riding coordinates:
 C35(H35A,H35B,H35C), C35A(H35D,H35E,H35F)
        6.d Aromatic/amide H refined with riding coordinates:
 C12(H12), C6(H6), C8(H8), C2(H2), C5(H5), C11(H11), C4(H4), C3(H3), C9(H9),
 C10(H10), C18(H18), C17(H17)
        6.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C40A(H40B,H40C,H40A), C41(H41A,H41B,
 H41C), C39A(H39A,H39B,H39C), C37(H37A,H37B,H37C), C37A(H37D,H37E,H37F),
 C39(H39D,H39E,H39F)
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.27987(2) 0.42710(2) 0.38516(2) 0.03155(11) Uani 1 1 d . . . . .
Na2 Na 0.34737(4) 0.07003(5) 0.59804(4) 0.0396(2) Uani 1 1 d . . . . .
Na3 Na 0.29325(5) 0.42599(5) 0.25489(4) 0.0447(2) Uani 1 1 d . . . . .
Na1 Na 0.35737(5) 0.30880(5) 0.47395(4) 0.0455(2) Uani 1 1 d . . . . .
O1 O 0.41590(7) -0.03312(9) 0.60352(8) 0.0448(4) Uani 1 1 d . . . . .
O2A O 0.3296(8) 0.5467(7) 0.2344(6) 0.041(2) Uani 0.405(7) 1 d . . P A 2
C7 C 0.20204(9) 0.43965(11) 0.30804(9) 0.0317(4) Uani 1 1 d . . . . .
C1 C 0.33042(9) 0.34861(11) 0.35964(9) 0.0334(4) Uani 1 1 d . . . . .
C12 C 0.15394(9) 0.38187(11) 0.28476(10) 0.0350(4) Uani 1 1 d . . . . .
H12 H 0.159384 0.336967 0.308991 0.042 Uiso 1 1 calc R U . . .
C6 C 0.30124(10) 0.27834(12) 0.33573(10) 0.0372(4) Uani 1 1 d . . . . .
H6 H 0.25515 0.272371 0.32786 0.045 Uiso 1 1 calc R U . . .
C8 C 0.18815(10) 0.50391(12) 0.26822(10) 0.0365(4) Uani 1 1 d . . . . .
H8 H 0.216733 0.545998 0.281205 0.044 Uiso 1 1 calc R U . . .
C14 C 0.27172(10) 0.49953(12) 0.44829(10) 0.0361(4) Uani 1 1 d . . . . .
H14 H 0.237022 0.486078 0.467196 0.043 Uiso 1 1 calc R U . . .
C2 C 0.39909(10) 0.35105(13) 0.36826(10) 0.0390(4) Uani 1 1 d . . . . .
H2 H 0.422483 0.396246 0.383705 0.047 Uiso 1 1 calc R U . . .
C5 C 0.33561(11) 0.21798(13) 0.32316(11) 0.0424(5) Uani 1 1 d . . . . .
H5 H 0.313016 0.172402 0.307481 0.051 Uiso 1 1 calc R U . . .
C13 C 0.33211(10) 0.45577(13) 0.47342(10) 0.0385(4) Uani 1 1 d . . . . .
H13 H 0.329837 0.41764 0.505578 0.046 Uiso 1 1 calc R U . . .
C11 C 0.09957(10) 0.38694(12) 0.22891(10) 0.0408(5) Uani 1 1 d . . . . .
H11 H 0.068709 0.346796 0.216786 0.049 Uiso 1 1 calc R U . . .
C4 C 0.40292(11) 0.22385(13) 0.33337(11) 0.0431(5) Uani 1 1 d . . . . .
H4 H 0.426933 0.182499 0.325361 0.052 Uiso 1 1 calc R U . . .
C3 C 0.43409(10) 0.29079(14) 0.35532(11) 0.0444(5) Uani 1 1 d . . . . .
H3 H 0.47996 0.296086 0.361759 0.053 Uiso 1 1 calc R U . . .
C9 C 0.13504(11) 0.50905(13) 0.21111(10) 0.0421(5) Uani 1 1 d . . . . .
H9 H 0.129425 0.553087 0.185777 0.051 Uiso 1 1 calc R U . . .
C10 C 0.09029(11) 0.45032(14) 0.19095(11) 0.0442(5) Uani 1 1 d . . . . .
H10 H 0.054131 0.453564 0.151992 0.053 Uiso 1 1 calc R U . . .
C29 C 0.33729(10) 0.19896(12) 0.53531(11) 0.0414(5) Uani 1 1 d . . . . .
H29 H 0.290404 0.180967 0.518719 0.05 Uiso 1 1 calc R U . . .
C22 C 0.34931(11) 0.24598(14) 0.58688(11) 0.0471(5) Uani 1 1 d . . . . .
H22 H 0.309518 0.260709 0.597947 0.056 Uiso 1 1 calc R U . . .
C15 C 0.27103(12) 0.58115(12) 0.43006(11) 0.0447(5) Uani 1 1 d . . . . .
H15A H 0.225695 0.594642 0.402252 0.054 Uiso 1 1 calc R U . . .
H15B H 0.300863 0.587961 0.404892 0.054 Uiso 1 1 calc R U . . .
C20 C 0.40047(11) 0.48875(15) 0.48816(11) 0.0491(5) Uani 1 1 d . . . . .
H20A H 0.402382 0.516678 0.450364 0.059 Uiso 1 1 calc R U . . .
H20B H 0.433228 0.447507 0.496699 0.059 Uiso 1 1 calc R U . . .
C16 C 0.29284(12) 0.63623(13) 0.48819(12) 0.0486(5) Uani 1 1 d . . . . .
H16A H 0.262711 0.680048 0.478598 0.058 Uiso 1 1 calc R U . . .
H16B H 0.288478 0.610582 0.526035 0.058 Uiso 1 1 calc R U . . .
C28 C 0.37970(11) 0.15530(14) 0.51415(12) 0.0469(5) Uani 1 1 d . . . . .
H28 H 0.361912 0.138651 0.468595 0.056 Uiso 1 1 calc R U . . .
C30 C 0.44584(12) -0.06302(14) 0.66765(12) 0.0488(5) Uani 1 1 d . . . . .
H30A H 0.437225 -0.028012 0.698489 0.059 Uiso 1 1 calc R U . . .
H30B H 0.494387 -0.06608 0.677758 0.059 Uiso 1 1 calc R U . . .
C19 C 0.41969(12) 0.54277(16) 0.54703(12) 0.0551(6) Uani 1 1 d . . . . .
H19A H 0.389105 0.534327 0.571188 0.066 Uiso 1 1 calc R U . . .
H19B H 0.465024 0.530499 0.57559 0.066 Uiso 1 1 calc R U . . .
C27 C 0.45439(11) 0.15538(15) 0.54466(13) 0.0508(6) Uani 1 1 d . . . . .
H27A H 0.466411 0.143627 0.590665 0.061 Uiso 1 1 calc R U . . .
H27B H 0.47331 0.115773 0.52478 0.061 Uiso 1 1 calc R U . . .
C25 C 0.48439(11) 0.29398(15) 0.56920(12) 0.0511(6) Uani 1 1 d . . . . .
H25 H 0.517268 0.331425 0.564753 0.061 Uiso 1 1 calc R U . . .
C23 C 0.41472(12) 0.25546(15) 0.63927(12) 0.0514(6) Uani 1 1 d . . . . .
H23A H 0.435157 0.205281 0.650384 0.062 Uiso 1 1 calc R U . . .
H23B H 0.406224 0.274984 0.677439 0.062 Uiso 1 1 calc R U . . .
C18 C 0.41722(13) 0.62263(17) 0.52895(12) 0.0555(6) Uani 1 1 d . . . . .
H18 H 0.458425 0.647103 0.536024 0.067 Uiso 1 1 calc R U . . .
C17 C 0.36318(14) 0.66339(15) 0.50387(12) 0.0559(6) Uani 1 1 d . . . . .
H17 H 0.369159 0.714456 0.494873 0.067 Uiso 1 1 calc R U . . .
C32 C 0.44023(14) -0.06544(18) 0.55817(13) 0.0612(7) Uani 1 1 d . . . . .
H32A H 0.446869 -0.119925 0.56649 0.073 Uiso 1 1 calc R U . . .
H32B H 0.483654 -0.042887 0.562301 0.073 Uiso 1 1 calc R U . . .
C31 C 0.42027(13) -0.13847(17) 0.67560(15) 0.0629(7) Uani 1 1 d . . . . .
H31A H 0.427072 -0.172993 0.644095 0.094 Uiso 1 1 calc R U . . .
H31B H 0.372873 -0.135057 0.669234 0.094 Uiso 1 1 calc R U . . .
H31C H 0.444008 -0.157137 0.718706 0.094 Uiso 1 1 calc R U . . .
C35 C 0.2595(7) 0.5345(5) 0.1197(5) 0.057(3) Uani 0.595(7) 1 d . . P A 1
H35A H 0.245242 0.56285 0.079614 0.085 Uiso 0.595(7) 1 calc R U P A 1
H35B H 0.274131 0.48442 0.112204 0.085 Uiso 0.595(7) 1 calc R U P A 1
H35C H 0.222323 0.529934 0.135751 0.085 Uiso 0.595(7) 1 calc R U P A 1
O3 O 0.2669(2) 0.3427(2) 0.16893(15) 0.0477(10) Uani 0.533(5) 1 d . . P A 1
C26 C 0.48372(16) 0.23008(19) 0.53705(16) 0.0703(8) Uani 1 1 d . . . . .
H26 H 0.514814 0.228829 0.512211 0.084 Uiso 1 1 calc R U . . .
C33 C 0.39462(16) -0.0537(2) 0.49379(15) 0.0759(9) Uani 1 1 d . . . . .
H33A H 0.412792 -0.076407 0.463143 0.114 Uiso 1 1 calc R U . . .
H33B H 0.388364 0.000242 0.485371 0.114 Uiso 1 1 calc R U . . .
H33C H 0.35192 -0.076979 0.489385 0.114 Uiso 1 1 calc R U . . .
C38A C 0.4010(7) 0.3459(11) 0.1876(8) 0.074(3) Uani 0.467(5) 1 d . U P A 2
H38A H 0.401759 0.338865 0.143731 0.089 Uiso 0.467(5) 1 calc R U P A 2
H38B H 0.419856 0.300583 0.212989 0.089 Uiso 0.467(5) 1 calc R U P A 2
C34A C 0.3144(5) 0.5803(5) 0.1699(6) 0.037(2) Uani 0.405(7) 1 d . . P A 2
H34A H 0.299516 0.63277 0.170779 0.045 Uiso 0.405(7) 1 calc R U P A 2
H34B H 0.355216 0.581339 0.158519 0.045 Uiso 0.405(7) 1 calc R U P A 2
C38 C 0.3156(5) 0.2967(9) 0.1593(7) 0.051(2) Uani 0.533(5) 1 d . . P A 1
H38C H 0.305832 0.287136 0.113241 0.062 Uiso 0.533(5) 1 calc R U P A 1
H38D H 0.317764 0.248008 0.181387 0.062 Uiso 0.533(5) 1 calc R U P A 1
C24 C 0.46481(19) 0.30687(19) 0.6252(2) 0.0822(10) Uani 1 1 d . . . . .
H24A H 0.447103 0.358571 0.621921 0.099 Uiso 1 1 calc R U . . .
H24B H 0.505665 0.305714 0.663112 0.099 Uiso 1 1 calc R U . . .
C40A C 0.2209(7) 0.3187(11) 0.1487(8) 0.068(4) Uani 0.467(5) 1 d . . P A 2
H40B H 0.214017 0.315235 0.189986 0.103 Uiso 0.467(5) 1 calc R U P A 2
H40C H 0.191598 0.283187 0.118664 0.103 Uiso 0.467(5) 1 calc R U P A 2
H40A H 0.210894 0.369824 0.131944 0.103 Uiso 0.467(5) 1 calc R U P A 2
O3A O 0.3339(2) 0.3587(2) 0.18654(17) 0.0556(13) Uani 0.467(5) 1 d . U P A 2
C36 C 0.3793(5) 0.5804(5) 0.2644(4) 0.091(3) Uani 0.595(7) 1 d D U P A 1
H36A H 0.359064 0.629757 0.266753 0.109 Uiso 0.595(7) 1 calc R U P A 1
H36B H 0.417343 0.588546 0.249429 0.109 Uiso 0.595(7) 1 calc R U P A 1
C41 C 0.1830(3) 0.2466(3) 0.1626(3) 0.0602(14) Uani 0.533(5) 1 d . . P A 1
H41A H 0.212317 0.205694 0.159607 0.09 Uiso 0.533(5) 1 calc R U P A 1
H41B H 0.136972 0.233103 0.139053 0.09 Uiso 0.533(5) 1 calc R U P A 1
H41C H 0.188289 0.255391 0.207572 0.09 Uiso 0.533(5) 1 calc R U P A 1
C39A C 0.4406(3) 0.4153(5) 0.2181(3) 0.075(2) Uani 0.467(5) 1 d . U P A 2
H39A H 0.41926 0.460117 0.194498 0.113 Uiso 0.467(5) 1 calc R U P A 2
H39B H 0.485721 0.411214 0.216903 0.113 Uiso 0.467(5) 1 calc R U P A 2
H39C H 0.442278 0.419342 0.262563 0.113 Uiso 0.467(5) 1 calc R U P A 2
C37 C 0.4018(4) 0.5455(5) 0.3268(3) 0.104(3) Uani 0.595(7) 1 d D U P A 1
H37A H 0.431714 0.50392 0.326968 0.156 Uiso 0.595(7) 1 calc R U P A 1
H37B H 0.363518 0.526309 0.336729 0.156 Uiso 0.595(7) 1 calc R U P A 1
H37C H 0.42523 0.582574 0.35903 0.156 Uiso 0.595(7) 1 calc R U P A 1
C37A C 0.3533(3) 0.6582(4) 0.3029(3) 0.059(2) Uani 0.405(7) 1 d D . P A 2
H37D H 0.355382 0.693127 0.269565 0.088 Uiso 0.405(7) 1 calc R U P A 2
H37E H 0.38219 0.676174 0.344592 0.088 Uiso 0.405(7) 1 calc R U P A 2
H37F H 0.307598 0.655252 0.302712 0.088 Uiso 0.405(7) 1 calc R U P A 2
C21 C 0.2911(9) 0.3005(12) 0.1572(10) 0.084(5) Uani 0.467(5) 1 d . . P A 2
H21A H 0.304243 0.254533 0.183437 0.101 Uiso 0.467(5) 1 calc R U P A 2
H21B H 0.295157 0.290136 0.114946 0.101 Uiso 0.467(5) 1 calc R U P A 2
C39 C 0.3810(5) 0.3396(7) 0.1874(6) 0.056(2) Uani 0.533(5) 1 d . . P A 1
H39D H 0.378229 0.387122 0.164517 0.083 Uiso 0.533(5) 1 calc R U P A 1
H39E H 0.417284 0.309319 0.182863 0.083 Uiso 0.533(5) 1 calc R U P A 1
H39F H 0.389241 0.34971 0.232709 0.083 Uiso 0.533(5) 1 calc R U P A 1
C40 C 0.1999(7) 0.3133(10) 0.1360(8) 0.065(3) Uani 0.533(5) 1 d . . P A 1
H40D H 0.167416 0.352798 0.135933 0.078 Uiso 0.533(5) 1 calc R U P A 1
H40E H 0.195337 0.30314 0.090967 0.078 Uiso 0.533(5) 1 calc R U P A 1
C36A C 0.3749(5) 0.5845(6) 0.2906(5) 0.066(3) Uani 0.405(7) 1 d D . P A 2
H36C H 0.380852 0.552474 0.328485 0.079 Uiso 0.405(7) 1 calc R U P A 2
H36D H 0.418657 0.589439 0.285107 0.079 Uiso 0.405(7) 1 calc R U P A 2
O2 O 0.3322(6) 0.5329(6) 0.2213(5) 0.063(2) Uani 0.595(7) 1 d . . P A 1
C34 C 0.3125(8) 0.5727(8) 0.1654(9) 0.109(5) Uani 0.595(7) 1 d . U P A 1
H34C H 0.350074 0.57794 0.149325 0.13 Uiso 0.595(7) 1 calc R U P A 1
H34D H 0.298127 0.623576 0.172935 0.13 Uiso 0.595(7) 1 calc R U P A 1
C35A C 0.2639(12) 0.5392(13) 0.1219(10) 0.095(8) Uani 0.405(7) 1 d . . P A 2
H35D H 0.255407 0.563174 0.080281 0.143 Uiso 0.405(7) 1 calc R U P A 2
H35E H 0.27885 0.487545 0.120304 0.143 Uiso 0.405(7) 1 calc R U P A 2
H35F H 0.223168 0.53896 0.132559 0.143 Uiso 0.405(7) 1 calc R U P A 2
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 '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
-1 1 0 0.0768
1 -1 0 0.1098
0 0 1 0.111
0 -1 0 0.1009
0 1 1 0.1205
1 1 0 0.0994
-1 -1 0 0.0431
-1 0 1 0.0779
1 0 -1 0.1045
1 1 1 0.1099
1 -1 -1 0.1067
-1 1 1 0.1042
-1 0 -1 0.0644
1 0 1 0.0958
14 1 -3 0.0963
11 4 3 0.0917
-13 -3 0 0.0377
-14 1 6 0.0642
-4 -3 -11 0.0606
3 -6 10 0.1012
-4 9 -7 0.0964
-1 3 -13 0.084
8 7 -11 0.0887
4 11 0 0.1038
12 4 -8 0.0932
-12 -6 6 0.0461
11 -4 4 0.0905
2 11 -6 0.0941
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
Na2 Ni1 Na3 121.91(3) 7_556 . ?
Na2 Ni1 Na1 105.52(3) 7_556 . ?
Na1 Ni1 Na3 114.87(3) . . ?
C7 Ni1 Na2 63.07(6) . 7_556 ?
C7 Ni1 Na3 59.18(6) . . ?
C7 Ni1 Na1 141.22(6) . . ?
C7 Ni1 C1 102.58(8) . . ?
C7 Ni1 C13 150.62(9) . . ?
C1 Ni1 Na2 133.58(6) . 7_556 ?
C1 Ni1 Na3 58.40(6) . . ?
C1 Ni1 Na1 56.65(6) . . ?
C1 Ni1 C13 106.77(8) . . ?
C14 Ni1 Na2 64.97(6) . 7_556 ?
C14 Ni1 Na3 139.12(6) . . ?
C14 Ni1 Na1 98.96(6) . . ?
C14 Ni1 C7 107.25(8) . . ?
C14 Ni1 C1 150.12(8) . . ?
C14 Ni1 C13 43.38(8) . . ?
C13 Ni1 Na2 96.38(6) . 7_556 ?
C13 Ni1 Na3 138.98(7) . . ?
C13 Ni1 Na1 61.40(7) . . ?
O1 Na2 Ni1 128.04(5) . 7_556 ?
O1 Na2 C7 108.70(6) . 7_556 ?
O1 Na2 C12 113.82(7) . 7_556 ?
O1 Na2 C14 98.96(7) . 7_556 ?
O1 Na2 C29 130.31(7) . . ?
O1 Na2 C28 100.20(7) . . ?
C7 Na2 Ni1 41.33(4) 7_556 7_556 ?
C7 Na2 C12 30.52(6) 7_556 7_556 ?
C7 Na2 C14 72.15(6) 7_556 7_556 ?
C7 Na2 C29 119.15(7) 7_556 . ?
C7 Na2 C28 148.76(7) 7_556 . ?
C12 Na2 Ni1 63.79(4) 7_556 7_556 ?
C14 Na2 Ni1 40.90(4) 7_556 7_556 ?
C14 Na2 C12 101.13(6) 7_556 7_556 ?
C29 Na2 Ni1 98.06(5) . 7_556 ?
C29 Na2 C12 101.71(7) . 7_556 ?
C29 Na2 C14 107.25(7) . 7_556 ?
C29 Na2 C28 30.31(7) . . ?
C28 Na2 Ni1 124.16(6) . 7_556 ?
C28 Na2 C12 124.89(7) . 7_556 ?
C28 Na2 C14 115.33(7) . 7_556 ?
Ni1 Na3 C2 59.73(4) . . ?
Ni1 Na3 C40A 124.4(3) . . ?
Ni1 Na3 C21 134.0(4) . . ?
O2A Na3 Ni1 108.8(3) . . ?
O2A Na3 C7 110.2(3) . . ?
O2A Na3 C1 129.1(3) . . ?
O2A Na3 C8 84.2(3) . . ?
O2A Na3 C2 110.5(3) . . ?
O2A Na3 C40A 122.4(5) . . ?
O2A Na3 C21 116.4(5) . . ?
C7 Na3 Ni1 40.07(4) . . ?
C7 Na3 C8 30.50(6) . . ?
C7 Na3 C2 97.32(6) . . ?
C7 Na3 C40A 98.4(3) . . ?
C7 Na3 C21 123.1(3) . . ?
C1 Na3 Ni1 40.29(5) . . ?
C1 Na3 C7 72.12(6) . . ?
C1 Na3 C8 100.75(7) . . ?
C1 Na3 C2 27.41(6) . . ?
C1 Na3 C40A 106.7(4) . . ?
C1 Na3 C21 100.0(4) . . ?
C8 Na3 Ni1 62.87(5) . . ?
C8 Na3 C2 122.48(6) . . ?
C8 Na3 C40A 100.4(3) . . ?
C8 Na3 C21 128.3(3) . . ?
C2 Na3 C21 95.4(3) . . ?
O3 Na3 Ni1 135.90(10) . . ?
O3 Na3 C7 114.70(12) . . ?
O3 Na3 C1 108.32(10) . . ?
O3 Na3 C8 115.40(11) . . ?
O3 Na3 C2 107.69(10) . . ?
C40A Na3 C2 114.1(4) . . ?
C40A Na3 C21 28.1(5) . . ?
O3A Na3 Ni1 144.35(10) . . ?
O3A Na3 O2A 96.9(3) . . ?
O3A Na3 C7 147.81(13) . . ?
O3A Na3 C1 104.15(10) . . ?
O3A Na3 C8 146.48(12) . . ?
O3A Na3 C2 88.66(10) . . ?
O3A Na3 C40A 51.0(4) . . ?
O3A Na3 C21 24.7(3) . . ?
O2 Na3 Ni1 118.0(2) . . ?
O2 Na3 C7 118.5(3) . . ?
O2 Na3 C1 134.2(3) . . ?
O2 Na3 C8 91.0(3) . . ?
O2 Na3 C2 112.2(3) . . ?
O2 Na3 O3 105.9(2) . . ?
C1 Na1 Ni1 40.85(5) . . ?
C1 Na1 C6 28.75(6) . . ?
C1 Na1 C2 29.50(6) . . ?
C1 Na1 C13 75.04(7) . . ?
C1 Na1 C22 162.82(8) . . ?
C1 Na1 C28 122.83(8) . . ?
C1 Na1 C25 128.01(7) . . ?
C1 Na1 C26 118.43(8) . . ?
C6 Na1 Ni1 59.97(4) . . ?
C6 Na1 C26 113.23(8) . . ?
C2 Na1 Ni1 62.11(5) . . ?
C2 Na1 C6 47.77(6) . . ?
C2 Na1 C26 91.39(7) . . ?
C13 Na1 Ni1 40.34(5) . . ?
C13 Na1 C6 99.49(6) . . ?
C13 Na1 C2 81.88(7) . . ?
C13 Na1 C22 108.71(8) . . ?
C13 Na1 C28 161.46(8) . . ?
C13 Na1 C25 103.65(8) . . ?
C13 Na1 C26 128.29(8) . . ?
C29 Na1 Ni1 138.89(6) . . ?
C29 Na1 C1 138.50(8) . . ?
C29 Na1 C6 109.85(8) . . ?
C29 Na1 C2 143.70(8) . . ?
C29 Na1 C13 134.10(8) . . ?
C29 Na1 C22 29.24(8) . . ?
C29 Na1 C28 29.09(7) . . ?
C29 Na1 C25 79.57(7) . . ?
C29 Na1 C26 70.65(7) . . ?
C22 Na1 Ni1 133.27(6) . . ?
C22 Na1 C6 137.10(8) . . ?
C22 Na1 C2 164.40(7) . . ?
C22 Na1 C28 52.77(7) . . ?
C22 Na1 C25 68.23(7) . . ?
C22 Na1 C26 73.08(8) . . ?
C28 Na1 Ni1 151.42(6) . . ?
C28 Na1 C6 96.66(7) . . ?
C28 Na1 C2 115.99(7) . . ?
C28 Na1 C26 50.83(7) . . ?
C25 Na1 Ni1 137.63(6) . . ?
C25 Na1 C6 135.32(7) . . ?
C25 Na1 C2 98.57(7) . . ?
C25 Na1 C28 70.23(7) . . ?
C25 Na1 C26 26.70(8) . . ?
C26 Na1 Ni1 150.22(6) . . ?
C30 O1 Na2 113.71(14) . . ?
C32 O1 Na2 131.73(16) . . ?
C32 O1 C30 113.96(19) . . ?
C34A O2A Na3 124.7(9) . . ?
C36A O2A Na3 114.7(8) . . ?
C36A O2A C34A 120.3(12) . . ?
Ni1 C7 Na2 75.61(6) . 7_556 ?
Ni1 C7 Na3 80.75(7) . . ?
Na3 C7 Na2 155.48(8) . 7_556 ?
C12 C7 Ni1 122.22(14) . . ?
C12 C7 Na2 78.83(11) . 7_556 ?
C12 C7 Na3 109.17(13) . . ?
C8 C7 Ni1 125.20(15) . . ?
C8 C7 Na2 119.37(13) . 7_556 ?
C8 C7 Na3 79.86(12) . . ?
C8 C7 C12 112.53(17) . . ?
Ni1 C1 Na3 81.31(7) . . ?
Ni1 C1 Na1 82.50(7) . . ?
Na1 C1 Na3 163.03(9) . . ?
C6 C1 Ni1 121.26(14) . . ?
C6 C1 Na3 99.76(12) . . ?
C6 C1 Na1 92.97(13) . . ?
C2 C1 Ni1 125.91(16) . . ?
C2 C1 Na3 95.47(13) . . ?
C2 C1 Na1 89.90(12) . . ?
C2 C1 C6 112.54(18) . . ?
Na2 C12 H12 76.3 7_556 . ?
C7 C12 Na2 70.64(11) . 7_556 ?
C7 C12 H12 117.9 . . ?
C11 C12 Na2 123.53(14) . 7_556 ?
C11 C12 C7 124.29(19) . . ?
C11 C12 H12 117.9 . . ?
Na1 C6 H6 104.2 . . ?
C1 C6 Na1 58.28(10) . . ?
C1 C6 H6 117.9 . . ?
C5 C6 Na1 107.21(14) . . ?
C5 C6 C1 124.27(19) . . ?
C5 C6 H6 117.9 . . ?
Na3 C8 H8 87.9 . . ?
C7 C8 Na3 69.64(11) . . ?
C7 C8 H8 118.1 . . ?
C9 C8 Na3 112.49(15) . . ?
C9 C8 C7 123.89(19) . . ?
C9 C8 H8 118.1 . . ?
Ni1 C14 H14 113.8 . . ?
C13 C14 Ni1 68.79(11) . . ?
C13 C14 H14 113.8 . . ?
C13 C14 C15 123.21(19) . . ?
C15 C14 Ni1 115.97(15) . . ?
C15 C14 H14 113.8 . . ?
Na3 C2 H2 94.7 . . ?
Na1 C2 Na3 115.88(7) . . ?
Na1 C2 H2 101.4 . . ?
C1 C2 Na3 57.12(10) . . ?
C1 C2 Na1 60.60(11) . . ?
C1 C2 H2 118.2 . . ?
C3 C2 Na3 117.74(14) . . ?
C3 C2 Na1 107.69(15) . . ?
C3 C2 C1 123.7(2) . . ?
C3 C2 H2 118.2 . . ?
C6 C5 H5 119.9 . . ?
C6 C5 C4 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
Ni1 C13 H13 112.8 . . ?
C14 C13 Ni1 67.83(11) . . ?
C14 C13 H13 112.8 . . ?
C14 C13 C20 123.3(2) . . ?
C20 C13 Ni1 120.07(15) . . ?
C20 C13 H13 112.8 . . ?
C12 C11 H11 119.9 . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 H11 119.9 . . ?
C5 C4 H4 120.7 . . ?
C3 C4 C5 118.6(2) . . ?
C3 C4 H4 120.7 . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.6 . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.5(2) . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 118.49(19) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
Na1 C29 H29 112.7 . . ?
C22 C29 Na1 87.72(14) . . ?
C22 C29 H29 112.7 . . ?
C22 C29 C28 131.5(2) . . ?
C28 C29 Na1 90.02(14) . . ?
C28 C29 H29 112.7 . . ?
Na1 C22 H22 115.5 . . ?
C29 C22 Na1 63.04(12) . . ?
C29 C22 H22 115.5 . . ?
C29 C22 C23 125.5(2) . . ?
C23 C22 Na1 109.04(15) . . ?
C23 C22 H22 115.5 . . ?
C14 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C14 C15 C16 114.19(19) . . ?
H15A C15 H15B 107.6 . . ?
C16 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
C13 C20 H20A 109.1 . . ?
C13 C20 H20B 109.1 . . ?
C13 C20 C19 112.55(19) . . ?
H20A C20 H20B 107.8 . . ?
C19 C20 H20A 109.1 . . ?
C19 C20 H20B 109.1 . . ?
C15 C16 H16A 109 . . ?
C15 C16 H16B 109 . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 C15 112.9(2) . . ?
C17 C16 H16A 109 . . ?
C17 C16 H16B 109 . . ?
Na2 C28 H28 116 . . ?
C29 C28 Na2 74.27(13) . . ?
C29 C28 H28 116 . . ?
C29 C28 C27 124.1(2) . . ?
C27 C28 Na2 99.90(15) . . ?
C27 C28 H28 116 . . ?
O1 C30 H30A 109 . . ?
O1 C30 H30B 109 . . ?
O1 C30 C31 113.0(2) . . ?
H30A C30 H30B 107.8 . . ?
C31 C30 H30A 109 . . ?
C31 C30 H30B 109 . . ?
C20 C19 H19A 109 . . ?
C20 C19 H19B 109 . . ?
H19A C19 H19B 107.8 . . ?
C18 C19 C20 113.0(2) . . ?
C18 C19 H19A 109 . . ?
C18 C19 H19B 109 . . ?
C28 C27 H27A 109.3 . . ?
C28 C27 H27B 109.3 . . ?
H27A C27 H27B 107.9 . . ?
C26 C27 C28 111.7(2) . . ?
C26 C27 H27A 109.3 . . ?
C26 C27 H27B 109.3 . . ?
Na1 C25 H25 113.2 . . ?
C26 C25 Na1 81.17(19) . . ?
C26 C25 H25 113.2 . . ?
C26 C25 C24 129.3(3) . . ?
C24 C25 Na1 98.2(2) . . ?
C24 C25 H25 113.2 . . ?
C22 C23 H23A 108.1 . . ?
C22 C23 H23B 108.1 . . ?
C22 C23 C24 116.6(3) . . ?
H23A C23 H23B 107.3 . . ?
C24 C23 H23A 108.1 . . ?
C24 C23 H23B 108.1 . . ?
C19 C18 H18 116.9 . . ?
C17 C18 C19 126.2(2) . . ?
C17 C18 H18 116.9 . . ?
C16 C17 H17 117 . . ?
C18 C17 C16 126.0(2) . . ?
C18 C17 H17 117 . . ?
O1 C32 H32A 109.4 . . ?
O1 C32 H32B 109.4 . . ?
O1 C32 C33 111.1(2) . . ?
H32A C32 H32B 108 . . ?
C33 C32 H32A 109.4 . . ?
C33 C32 H32B 109.4 . . ?
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 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
C38 O3 Na3 120.7(6) . . ?
C38 O3 C40 111.6(9) . . ?
C40 O3 Na3 124.1(8) . . ?
Na1 C26 H26 115.1 . . ?
C27 C26 Na1 97.03(17) . . ?
C27 C26 H26 115.1 . . ?
C25 C26 Na1 72.13(18) . . ?
C25 C26 C27 128.3(3) . . ?
C25 C26 H26 115.1 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
H38A C38A H38B 108.7 . . ?
O3A C38A H38A 110.5 . . ?
O3A C38A H38B 110.5 . . ?
O3A C38A C39A 106.2(11) . . ?
C39A C38A H38A 110.5 . . ?
C39A C38A H38B 110.5 . . ?
O2A C34A H34A 109.2 . . ?
O2A C34A H34B 109.2 . . ?
H34A C34A H34B 107.9 . . ?
C35A C34A O2A 112.1(11) . . ?
C35A C34A H34A 109.2 . . ?
C35A C34A H34B 109.2 . . ?
O3 C38 H38C 110.6 . . ?
O3 C38 H38D 110.6 . . ?
O3 C38 C39 105.8(10) . . ?
H38C C38 H38D 108.7 . . ?
C39 C38 H38C 110.6 . . ?
C39 C38 H38D 110.6 . . ?
C25 C24 C23 120.4(3) . . ?
C25 C24 H24A 107.2 . . ?
C25 C24 H24B 107.2 . . ?
C23 C24 H24A 107.2 . . ?
C23 C24 H24B 107.2 . . ?
H24A C24 H24B 106.9 . . ?
H40B C40A H40C 109.5 . . ?
H40B C40A H40A 109.5 . . ?
H40C C40A H40A 109.5 . . ?
C21 C40A H40B 109.5 . . ?
C21 C40A H40C 109.5 . . ?
C21 C40A H40A 109.5 . . ?
C38A O3A Na3 131.3(8) . . ?
C21 O3A Na3 111.0(6) . . ?
C21 O3A C38A 112.5(10) . . ?
H36A C36 H36B 108.3 . . ?
C37 C36 H36A 109.9 . . ?
C37 C36 H36B 109.9 . . ?
O2 C36 H36A 109.9 . . ?
O2 C36 H36B 109.9 . . ?
O2 C36 C37 108.8(8) . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
C38A C39A H39A 109.5 . . ?
C38A C39A H39B 109.5 . . ?
C38A C39A H39C 109.5 . . ?
H39A C39A H39B 109.5 . . ?
H39A C39A H39C 109.5 . . ?
H39B C39A H39C 109.5 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
H37D C37A H37E 109.5 . . ?
H37D C37A H37F 109.5 . . ?
H37E C37A H37F 109.5 . . ?
C36A C37A H37D 109.5 . . ?
C36A C37A H37E 109.5 . . ?
C36A C37A H37F 109.5 . . ?
Na3 C21 H21A 104.4 . . ?
Na3 C21 H21B 144.4 . . ?
C40A C21 Na3 72.9(10) . . ?
C40A C21 H21A 109.2 . . ?
C40A C21 H21B 109.2 . . ?
O3A C21 C40A 112.0(14) . . ?
O3A C21 H21A 109.2 . . ?
O3A C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C38 C39 H39D 109.5 . . ?
C38 C39 H39E 109.5 . . ?
C38 C39 H39F 109.5 . . ?
H39D C39 H39E 109.5 . . ?
H39D C39 H39F 109.5 . . ?
H39E C39 H39F 109.5 . . ?
O3 C40 H40D 108.4 . . ?
O3 C40 H40E 108.4 . . ?
C41 C40 O3 115.5(11) . . ?
C41 C40 H40D 108.4 . . ?
C41 C40 H40E 108.4 . . ?
H40D C40 H40E 107.5 . . ?
O2A C36A H36C 108.6 . . ?
O2A C36A H36D 108.6 . . ?
C37A C36A O2A 114.6(8) . . ?
C37A C36A H36C 108.6 . . ?
C37A C36A H36D 108.6 . . ?
H36C C36A H36D 107.6 . . ?
C36 O2 Na3 122.0(7) . . ?
C34 O2 Na3 133.6(10) . . ?
C34 O2 C36 103.6(12) . . ?
C35 C34 H34C 109.8 . . ?
C35 C34 H34D 109.8 . . ?
O2 C34 C35 109.2(12) . . ?
O2 C34 H34C 109.8 . . ?
O2 C34 H34D 109.8 . . ?
H34C C34 H34D 108.3 . . ?
C34A C35A H35D 109.5 . . ?
C34A C35A H35E 109.5 . . ?
C34A C35A H35F 109.5 . . ?
H35D C35A H35E 109.5 . . ?
H35D C35A H35F 109.5 . . ?
H35E C35A H35F 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 Na2 2.8777(8) 7_556 ?
Ni1 Na3 3.0079(9) . ?
Ni1 Na1 2.9826(9) . ?
Ni1 C7 1.9618(19) . ?
Ni1 C1 1.968(2) . ?
Ni1 C14 1.959(2) . ?
Ni1 C13 1.972(2) . ?
Na2 O1 2.3316(17) . ?
Na2 C7 2.649(2) 7_556 ?
Na2 C12 2.754(2) 7_556 ?
Na2 C14 2.711(2) 7_556 ?
Na2 C29 2.660(2) . ?
Na2 C28 2.674(3) . ?
Na3 O2A 2.384(15) . ?
Na3 C7 2.617(2) . ?
Na3 C1 2.592(2) . ?
Na3 C8 2.748(2) . ?
Na3 C2 3.072(2) . ?
Na3 O3 2.335(4) . ?
Na3 C40A 3.028(16) . ?
Na3 O3A 2.325(4) . ?
Na3 C21 3.11(2) . ?
Na3 O2 2.304(13) . ?
Na1 C1 2.513(2) . ?
Na1 C6 2.950(2) . ?
Na1 C2 2.884(2) . ?
Na1 C13 2.675(2) . ?
Na1 C29 2.506(2) . ?
Na1 C22 2.809(2) . ?
Na1 C28 2.868(3) . ?
Na1 C25 2.844(3) . ?
Na1 C26 2.952(4) . ?
O1 C30 1.454(3) . ?
O1 C32 1.406(3) . ?
O2A C34A 1.488(16) . ?
O2A C36A 1.463(15) . ?
C7 C12 1.426(3) . ?
C7 C8 1.417(3) . ?
C1 C6 1.421(3) . ?
C1 C2 1.420(3) . ?
C12 H12 0.95 . ?
C12 C11 1.391(3) . ?
C6 H6 0.95 . ?
C6 C5 1.385(3) . ?
C8 H8 0.95 . ?
C8 C9 1.394(3) . ?
C14 H14 1 . ?
C14 C13 1.453(3) . ?
C14 C15 1.509(3) . ?
C2 H2 0.95 . ?
C2 C3 1.395(3) . ?
C5 H5 0.95 . ?
C5 C4 1.388(3) . ?
C13 H13 1 . ?
C13 C20 1.510(3) . ?
C11 H11 0.95 . ?
C11 C10 1.384(3) . ?
C4 H4 0.95 . ?
C4 C3 1.374(3) . ?
C3 H3 0.95 . ?
C9 H9 0.95 . ?
C9 C10 1.388(3) . ?
C10 H10 0.95 . ?
C29 H29 1 . ?
C29 C22 1.373(3) . ?
C29 C28 1.394(3) . ?
C22 H22 1 . ?
C22 C23 1.501(3) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C15 C16 1.564(3) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C20 C19 1.565(3) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C16 C17 1.509(4) . ?
C28 H28 1 . ?
C28 C27 1.514(3) . ?
C30 H30A 0.99 . ?
C30 H30B 0.99 . ?
C30 C31 1.485(4) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C19 C18 1.475(4) . ?
C27 H27A 0.99 . ?
C27 H27B 0.99 . ?
C27 C26 1.506(4) . ?
C25 H25 1 . ?
C25 C26 1.342(4) . ?
C25 C24 1.462(4) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C23 C24 1.523(4) . ?
C18 H18 0.95 . ?
C18 C17 1.321(4) . ?
C17 H17 0.95 . ?
C32 H32A 0.99 . ?
C32 H32B 0.99 . ?
C32 C33 1.452(4) . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C31 H31C 0.98 . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C35 H35C 0.98 . ?
C35 C34 1.42(2) . ?
O3 C38 1.401(11) . ?
O3 C40 1.472(11) . ?
C26 H26 1 . ?
C33 H33A 0.98 . ?
C33 H33B 0.98 . ?
C33 H33C 0.98 . ?
C38A H38A 0.99 . ?
C38A H38B 0.99 . ?
C38A O3A 1.450(11) . ?
C38A C39A 1.52(2) . ?
C34A H34A 0.99 . ?
C34A H34B 0.99 . ?
C34A C35A 1.44(3) . ?
C38 H38C 0.99 . ?
C38 H38D 0.99 . ?
C38 C39 1.534(17) . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
C40A H40B 0.98 . ?
C40A H40C 0.98 . ?
C40A H40A 0.98 . ?
C40A C21 1.49(2) . ?
O3A C21 1.39(2) . ?
C36 H36A 0.99 . ?
C36 H36B 0.99 . ?
C36 C37 1.449(9) . ?
C36 O2 1.416(12) . ?
C41 H41A 0.98 . ?
C41 H41B 0.98 . ?
C41 H41C 0.98 . ?
C41 C40 1.43(2) . ?
C39A H39A 0.98 . ?
C39A H39B 0.98 . ?
C39A H39C 0.98 . ?
C37 H37A 0.98 . ?
C37 H37B 0.98 . ?
C37 H37C 0.98 . ?
C37A H37D 0.98 . ?
C37A H37E 0.98 . ?
C37A H37F 0.98 . ?
C37A C36A 1.451(9) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C39 H39D 0.98 . ?
C39 H39E 0.98 . ?
C39 H39F 0.98 . ?
C40 H40D 0.99 . ?
C40 H40E 0.99 . ?
C36A H36C 0.99 . ?
C36A H36D 0.99 . ?
O2 C34 1.369(18) . ?
C34 H34C 0.99 . ?
C34 H34D 0.99 . ?
C35A H35D 0.98 . ?
C35A H35E 0.98 . ?
C35A H35F 0.98 . ?
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 C7 C12 Na2 64.92(12) . . . 7_556 ?
Ni1 C7 C12 C11 -177.11(16) . . . . ?
Ni1 C7 C8 Na3 70.98(13) . . . . ?
Ni1 C7 C8 C9 175.00(16) . . . . ?
Ni1 C1 C6 Na1 -83.03(13) . . . . ?
Ni1 C1 C6 C5 -173.01(17) . . . . ?
Ni1 C1 C2 Na3 -83.22(15) . . . . ?
Ni1 C1 C2 Na1 80.65(14) . . . . ?
Ni1 C1 C2 C3 173.17(16) . . . . ?
Ni1 C14 C13 C20 112.3(2) . . . . ?
Ni1 C14 C15 C16 -156.67(16) . . . . ?
Ni1 C13 C20 C19 151.39(18) . . . . ?
Na2 O1 C30 C31 111.7(2) . . . . ?
Na2 O1 C32 C33 -29.3(4) . . . . ?
Na2 C7 C12 C11 118.0(2) 7_556 . . . ?
Na2 C7 C8 Na3 163.73(13) 7_556 . . . ?
Na2 C7 C8 C9 -92.3(2) 7_556 . . . ?
Na2 C12 C11 C10 90.1(2) 7_556 . . . ?
Na2 C28 C27 C26 -143.3(2) . . . . ?
Na3 O2A C34A C35A 12.1(14) . . . . ?
Na3 O2A C36A C37A -124.0(9) . . . . ?
Na3 C7 C12 Na2 155.95(10) . . . 7_556 ?
Na3 C7 C12 C11 -86.1(2) . . . . ?
Na3 C7 C8 C9 104.0(2) . . . . ?
Na3 C1 C6 Na1 -168.73(11) . . . . ?
Na3 C1 C6 C5 101.3(2) . . . . ?
Na3 C1 C2 Na1 163.87(10) . . . . ?
Na3 C1 C2 C3 -103.6(2) . . . . ?
Na3 C8 C9 C10 82.2(2) . . . . ?
Na3 C2 C3 C4 -67.8(3) . . . . ?
Na3 O3 C38 C39 -28.8(13) . . . . ?
Na3 O3 C40 C41 -87.9(13) . . . . ?
Na3 O3A C21 C40A 30.0(16) . . . . ?
Na3 O2 C34 C35 -4.3(18) . . . . ?
Na1 C1 C6 C5 -90.0(2) . . . . ?
Na1 C1 C2 Na3 -163.87(10) . . . . ?
Na1 C1 C2 C3 92.5(2) . . . . ?
Na1 C6 C5 C4 -63.4(2) . . . . ?
Na1 C2 C3 C4 65.5(2) . . . . ?
Na1 C29 C22 C23 -95.0(2) . . . . ?
Na1 C29 C28 Na2 174.03(8) . . . . ?
Na1 C29 C28 C27 82.6(2) . . . . ?
Na1 C22 C23 C24 10.8(3) . . . . ?
Na1 C25 C26 C27 -84.8(3) . . . . ?
Na1 C25 C24 C23 59.9(3) . . . . ?
C7 C12 C11 C10 1.7(3) . . . . ?
C7 C8 C9 C10 2.4(3) . . . . ?
C1 C6 C5 C4 -0.5(3) . . . . ?
C1 C2 C3 C4 -0.5(3) . . . . ?
C12 C7 C8 Na3 -106.68(16) . . . . ?
C12 C7 C8 C9 -2.7(3) . . . . ?
C12 C11 C10 C9 -2.2(3) . . . . ?
C6 C1 C2 Na3 102.96(16) . . . . ?
C6 C1 C2 Na1 -93.17(16) . . . . ?
C6 C1 C2 C3 -0.7(3) . . . . ?
C6 C5 C4 C3 -0.8(3) . . . . ?
C8 C7 C12 Na2 -117.35(16) . . . 7_556 ?
C8 C7 C12 C11 0.6(3) . . . . ?
C8 C9 C10 C11 0.2(3) . . . . ?
C14 C13 C20 C19 69.5(3) . . . . ?
C14 C15 C16 C17 101.6(2) . . . . ?
C2 C1 C6 Na1 91.12(16) . . . . ?
C2 C1 C6 C5 1.1(3) . . . . ?
C5 C4 C3 C2 1.3(3) . . . . ?
C13 C14 C15 C16 -76.0(3) . . . . ?
C13 C20 C19 C18 -105.3(3) . . . . ?
C29 C22 C23 C24 80.7(3) . . . . ?
C29 C28 C27 C26 -65.7(3) . . . . ?
C22 C29 C28 Na2 87.1(3) . . . . ?
C22 C29 C28 C27 -4.4(4) . . . . ?
C22 C23 C24 C25 -54.8(4) . . . . ?
C15 C14 C13 Ni1 -107.9(2) . . . . ?
C15 C14 C13 C20 4.4(3) . . . . ?
C15 C16 C17 C18 -70.5(3) . . . . ?
C20 C19 C18 C17 75.0(3) . . . . ?
C28 C29 C22 Na1 88.0(3) . . . . ?
C28 C29 C22 C23 -7.0(4) . . . . ?
C28 C27 C26 Na1 3.8(2) . . . . ?
C28 C27 C26 C25 76.5(4) . . . . ?
C30 O1 C32 C33 160.3(3) . . . . ?
C19 C18 C17 C16 -0.4(4) . . . . ?
C32 O1 C30 C31 -76.1(3) . . . . ?
C26 C25 C24 C23 -25.4(5) . . . . ?
C38A O3A C21 Na3 157.5(10) . . . . ?
C38A O3A C21 C40A -172.5(13) . . . . ?
C34A O2A C36A C37A 61.5(15) . . . . ?
C38 O3 C40 C41 70.7(15) . . . . ?
C24 C25 C26 Na1 93.4(3) . . . . ?
C24 C25 C26 C27 8.6(6) . . . . ?
C36 O2 C34 C35 -173.6(10) . . . . ?
C39A C38A O3A Na3 -30.9(14) . . . . ?
C39A C38A O3A C21 177.5(11) . . . . ?
C37 C36 O2 Na3 6.5(12) . . . . ?
C37 C36 O2 C34 177.4(10) . . . . ?
C40 O3 C38 C39 171.8(11) . . . . ?
C36A O2A C34A C35A -173.9(12) . . . . ?
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
-0.9988 1.0004 -0.0005 -0.0969 0.034 -0.0523
0.9988 -1.0004 0.0005 0.0969 -0.034 0.0523
0 -0.0006 0.9996 0.0498 0.0032 -0.054
-0.001 -0.9998 0 0.0582 0.0317 0.0555
0.001 0.9993 0.9995 -0.0084 -0.0285 -0.1095
1.0009 0.9992 0.0004 -0.0194 -0.0973 -0.0587
-1.0009 -0.9992 -0.0004 0.0194 0.0973 0.0587
-0.9999 0 0.9991 0.011 0.0688 -0.0508
0.9999 0 -0.9991 -0.011 -0.0688 0.0508
1.0009 0.9987 1 0.0304 -0.0941 -0.1127
0.9988 -0.9999 -0.9991 0.0471 -0.0371 0.1063
-0.9988 0.9999 0.9991 -0.0471 0.0371 -0.1063
-0.9999 0.0012 -1 -0.0885 0.0625 0.0572
0.9999 -0.0012 1 0.0885 -0.0625 -0.0572
13.7758 0.8349 -3.0672 0.3318 -0.9404 0.0752
11.0085 4.3774 2.6961 0.3053 -0.8525 -0.4243
-12.7148 -2.8159 -0.0064 -0.3284 0.9237 0.1976
-13.854 0.9926 5.6263 -0.3138 0.8958 -0.3148
-4.0583 -3.388 -10.956 -0.5051 0.339 0.7937
2.8509 -5.7396 10.4766 0.966 0.0271 -0.2571
-4.0722 8.564 -6.812 -0.9953 -0.0247 -0.0939
-1.4206 2.5246 -12.6974 -0.834 -0.0264 0.5511
7.6644 6.5377 -11.0453 -0.6339 -0.7444 0.2097
3.6539 11.1236 -0.1493 -0.5137 -0.5918 -0.6212
12.2955 4.4823 -7.9237 -0.1796 -0.9737 0.1401
-11.9831 -5.5758 6.4642 0.1827 0.9832 -0.0015
10.68 -3.8799 3.7048 0.8236 -0.5669 -0.0194
2.3096 10.5641 -5.8835 -0.8186 -0.5039 -0.2757
