#------------------------------------------------------------------------------
#$Date: 2019-11-02 06:03:31 +0200 (Sat, 02 Nov 2019) $
#$Revision: 220770 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/75/4127535.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_4127535
loop_
_publ_author_name
'Song, Fangyuan'
'Al-Ameed, Karrar'
'Schilling, Mauro'
'Fox, Thomas'
'Luber, Sandra'
'Patzke, Greta R.'
_publ_section_title
;
 Mechanistically Driven Control over Cubane Oxo Cluster Catalysts.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8846
_journal_page_last               8857
_journal_paper_doi               10.1021/jacs.9b01356
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C48 H46 N8 Ni4 O14, 2(N O3), 1.42(O)'
_chemical_formula_sum            'C48 H47.6 N10 Ni4 O21.42'
_chemical_formula_weight         1342.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.4557(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5327(3)
_cell_length_b                   11.87693(11)
_cell_length_c                   21.4511(2)
_cell_measurement_reflns_used    15964
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      76.9440
_cell_measurement_theta_min      4.2890
_cell_volume                     5139.55(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -61.00  25.00   0.50    1.00    --  -51.66  38.00 150.00  172
  2  ω    -61.00  25.00   0.50    1.00    --  -51.66  38.00  30.00  172
  3  ω    -65.00  21.00   0.50    1.00    --  -51.66  56.00-122.00  172
  4  ω     43.00 129.00   0.50    1.00    --   51.66  38.00-180.00  172
  5  ω     96.00 178.00   0.50    4.00    --  105.75  15.00-180.00  164
  6  ω    148.00 174.00   0.50    4.00    --  105.75  48.00 -55.50   52
  7  ω     94.00 178.00   0.50    4.00    --  105.75  51.00  72.21  168
  8  ω     95.00 178.00   0.50    4.00    --  105.75  48.00 109.36  166
  9  ω     99.00 177.00   0.50    4.00    --  105.75  51.00 124.95  156
 10  ω     94.00 178.00   0.50    4.00    --  105.75  45.00   0.00  168
 11  ω     97.00 178.00   0.50    4.00    --  105.75  30.00-120.00  162
 12  ω     97.00 178.00   0.50    4.00    --  105.75  30.00-180.00  162
 13  ω     64.00  91.00   0.50    4.00    --  105.75 -56.00 -65.45   54
 14  ω     36.00  72.00   0.50    4.00    --  105.75 -49.00 -14.82   72
 15  ω     33.00  93.00   0.50    4.00    --  105.75 -56.00 -31.23  120
 16  ω     28.00  53.00   0.50    4.00    --  105.75 -30.00-150.00   50
 17  ω     33.00  70.00   0.50    4.00    --  105.75 -45.00-120.00   74
 18  ω     30.00  66.00   0.50    4.00    --  105.75 -44.00-100.44   72
 19  ω     34.00  65.00   0.50    4.00    --  105.75 -52.00 -64.74   62
 20  ω     30.00  57.00   0.50    4.00    --  105.75 -30.00   0.00   54
 21  ω     32.00  78.00   0.50    4.00    --  105.75 -53.00  49.09   92
 22  ω     48.00  76.00   0.50    4.00    --  105.75 -45.00  90.00   56
 23  ω     43.00  82.00   0.50    4.00    --  105.75 -52.00 147.57   78
 24  ω     38.00  76.00   0.50    4.00    --  105.75 -45.00 164.58   76
 25  ω     31.00  79.00   0.50    4.00    --  105.75 -47.00 128.08   96
 26  ω     30.00  59.00   0.50    4.00    --  105.75 -30.00 150.00   58
 27  ω     30.00  69.00   0.50    4.00    --  105.75 -30.00 -90.00   78
 28  ω    -61.00  28.00   0.50    1.00    --  -51.66  19.00 150.00  178
 29  ω     39.00  65.00   0.50    4.00    --  105.75 -45.00 -90.00   52
 30  ω    111.00 137.00   0.50    4.00    --  105.75  30.00-150.00   52
 31  ω     34.00  60.00   0.50    4.00    --  105.75 -15.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0500428000
_diffrn_orient_matrix_UB_12      0.0900554000
_diffrn_orient_matrix_UB_13      0.0447238000
_diffrn_orient_matrix_UB_21      -0.0121278000
_diffrn_orient_matrix_UB_22      -0.0334126000
_diffrn_orient_matrix_UB_23      0.0627804000
_diffrn_orient_matrix_UB_31      0.0563883000
_diffrn_orient_matrix_UB_32      -0.0871809000
_diffrn_orient_matrix_UB_33      0.0221626000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30292
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.382
_diffrn_reflns_theta_min         4.320
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.462
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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 greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0733P)²+11.8044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4880
_reflns_number_total             5419
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891359(2-Ni4-NO3final)
_cod_original_cell_volume        5139.54(11)
_cod_original_formula_sum        'C48 H47.60 N10 Ni4 O21.42'
_cod_database_code               4127535
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H46 N10 Ni4 O20'
_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.
;
_reflns_odcompleteness_completeness 99.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_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
2. Restrained distances
 O6B-C24B
 2.35 with sigma of 0.005
 O6A-C24A
 2.35 with sigma of 0.005
 O5A-C24A
 2.35 with sigma of 0.005
 O5B-C24B
 2.35 with sigma of 0.005
 O9A-O10A
 2.16 with sigma of 0.005
 O8A-O10A
 2.16 with sigma of 0.005
 O9A-O8A
 2.16 with sigma of 0.005
 O8B-O10B
 2.16 with sigma of 0.005
 O10B-O9B
 2.16 with sigma of 0.005
 O8B-O9B
 2.16 with sigma of 0.005
 Ni1-O5A \\sim Ni1-O5B
 with sigma of 0.005
 O5A-C23A \\sim O5B-C23B
 with sigma of 0.005
 O6B-C23B \\sim O6A-C23A
 with sigma of 0.005
 C24B-C23B \\sim C24A-C23A
 with sigma of 0.005
 O9A-N5A \\sim O10A-N5A \\sim O8A-N5A \\sim O8B-N5B \\sim O10B-N5B \\sim O9B-N5B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O5A \\sim O5B \\sim O6A \\sim O6B \\sim C23A \\sim C23B \\sim C24A \\sim C24B:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.08
O8A \\sim O8B \\sim O9A \\sim O9B \\sim O10A \\sim O10B: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O5A, O5B, O6A, O6B, C23A, C23B, C24A, C24B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O8A, O8B, O9A, O9B, O10A, O10B, N5A, N5B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O8B)=Sof(O9B)=Sof(O10B)=Sof(N5B)=1-FVAR(1)
 Sof(O8A)=Sof(O9A)=Sof(O10)=Sof(O10A)=Sof(N5A)=FVAR(1)
 Sof(O5B)=Sof(O6B)=Sof(C23B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(O5A)=Sof(O6A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
6.a Rotating group:
 O7(H7A,H7B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22)
6.c Idealised Me refined as rotating group:
 C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.399
_oxdiff_exptl_absorpt_empirical_full_min 0.724
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.44236(2) 0.81479(4) 0.67471(2) 0.02715(13) Uani 1 1 d D . . . .
Ni2 Ni 0.44551(2) 0.61368(3) 0.77317(2) 0.02545(13) Uani 1 1 d . . . . .
O1 O 0.45284(8) 0.79175(14) 0.77371(8) 0.0264(3) Uani 1 1 d . . . . .
O2 O 0.54563(8) 0.63522(14) 0.81935(8) 0.0263(3) Uani 1 1 d . . . . .
O3 O 0.41561(10) 0.94876(16) 0.81093(11) 0.0390(4) Uani 1 1 d . . . . .
H3 H 0.384572 0.989883 0.783637 0.13(2) Uiso 1 1 calc GR . . . .
O4 O 0.59230(11) 0.58408(17) 0.93586(9) 0.0398(5) Uani 1 1 d . . . . .
H4 H 0.577038 0.648841 0.935164 0.059(12) Uiso 1 1 calc GR . . . .
O5A O 0.4239(3) 0.8083(5) 0.57362(16) 0.0334(11) Uani 0.711(10) 1 d D U P A 1
O5B O 0.4371(9) 0.8007(13) 0.5785(4) 0.0339(13) Uani 0.289(10) 1 d D U P A 2
O6A O 0.4336(3) 0.9828(3) 0.5469(2) 0.0552(15) Uani 0.711(10) 1 d D U P A 1
O6B O 0.4812(5) 0.9598(7) 0.5696(4) 0.042(3) Uani 0.289(10) 1 d D U P A 2
O7 O 0.44949(12) 0.98891(18) 0.68311(14) 0.0524(6) Uani 1 1 d . . . . .
H7A H 0.410880 1.025984 0.680821 0.13(2) Uiso 1 1 d GR . . . .
H7B H 0.457564 1.025916 0.647814 0.23(5) Uiso 1 1 d GR . . . .
O8A O 0.3379(8) 1.0987(8) 0.6671(5) 0.134(4) Uani 0.709(6) 1 d D U P B 1
O8B O 0.3371(10) 1.1021(10) 0.6775(5) 0.072(4) Uani 0.291(6) 1 d D U P B 2
O9A O 0.3263(2) 1.1338(5) 0.7601(2) 0.104(2) Uani 0.709(6) 1 d D U P B 1
O9B O 0.3017(6) 1.1465(10) 0.5692(4) 0.085(4) Uani 0.291(6) 1 d D U P B 2
O10 O 0.2914(5) 1.1852(9) 0.5292(5) 0.207(7) Uani 0.709(6) 1 d . . P B 1
O10A O 0.2900(4) 1.2510(4) 0.6737(3) 0.0896(19) Uani 0.709(6) 1 d D U P B 1
O10B O 0.2840(7) 1.2577(7) 0.6387(6) 0.067(3) Uani 0.291(6) 1 d D U P B 2
N1 N 0.34451(11) 0.82688(19) 0.66121(11) 0.0334(5) Uani 1 1 d . . . . .
N2 N 0.41555(11) 0.65587(19) 0.84701(11) 0.0323(5) Uani 1 1 d . . . . .
N3 N 0.47897(12) 0.45048(18) 0.80898(11) 0.0340(5) Uani 1 1 d . . . . .
N4 N 0.64801(11) 0.56596(19) 0.80383(11) 0.0341(5) Uani 1 1 d . . . . .
N5A N 0.3174(2) 1.1609(3) 0.7006(2) 0.0658(13) Uani 0.709(6) 1 d D U P B 1
N5B N 0.3074(5) 1.1687(6) 0.6283(4) 0.059(3) Uani 0.291(6) 1 d D U P B 2
C1 C 0.29006(14) 0.8322(3) 0.59992(15) 0.0425(7) Uani 1 1 d . . . . .
H1 H 0.294702 0.827312 0.558104 0.051 Uiso 1 1 calc R . . . .
C2 C 0.22730(15) 0.8445(3) 0.59579(17) 0.0501(8) Uani 1 1 d . . . . .
H2 H 0.189675 0.849886 0.551726 0.060 Uiso 1 1 calc R . . . .
C3 C 0.21992(15) 0.8487(3) 0.65581(18) 0.0477(7) Uani 1 1 d . . . . .
H3A H 0.177072 0.854927 0.653809 0.057 Uiso 1 1 calc R . . . .
C4 C 0.27600(14) 0.8439(3) 0.71968(16) 0.0393(6) Uani 1 1 d . . . . .
H4A H 0.272240 0.846954 0.762034 0.047 Uiso 1 1 calc R . . . .
C5 C 0.33749(13) 0.8344(2) 0.72011(14) 0.0316(5) Uani 1 1 d . . . . .
C6 C 0.40316(12) 0.8364(2) 0.78795(13) 0.0294(5) Uani 1 1 d . . . . .
C7 C 0.39917(12) 0.7654(2) 0.84575(13) 0.0323(5) Uani 1 1 d . . . . .
C8 C 0.38109(17) 0.8093(3) 0.89429(16) 0.0468(7) Uani 1 1 d . . . . .
H8 H 0.371582 0.887256 0.893968 0.056 Uiso 1 1 calc R . . . .
C9 C 0.37687(19) 0.7382(3) 0.94386(17) 0.0535(9) Uani 1 1 d . . . . .
H9 H 0.362847 0.766537 0.976553 0.064 Uiso 1 1 calc R . . . .
C10 C 0.39336(19) 0.6260(3) 0.94481(17) 0.0504(8) Uani 1 1 d . . . . .
H10 H 0.391011 0.575848 0.978139 0.060 Uiso 1 1 calc R . . . .
C11 C 0.41340(16) 0.5883(3) 0.89609(14) 0.0415(6) Uani 1 1 d . . . . .
H11 H 0.426083 0.511681 0.897452 0.050 Uiso 1 1 calc R . . . .
C12 C 0.44221(19) 0.3561(2) 0.79486(16) 0.0445(7) Uani 1 1 d . . . . .
H12 H 0.396261 0.360256 0.763950 0.053 Uiso 1 1 calc R . . . .
C13 C 0.4693(2) 0.2534(3) 0.8240(2) 0.0597(10) Uani 1 1 d . . . . .
H13 H 0.441901 0.188465 0.814109 0.072 Uiso 1 1 calc R . . . .
C14 C 0.5359(2) 0.2458(3) 0.8671(2) 0.0610(10) Uani 1 1 d . . . . .
H14 H 0.555096 0.175639 0.887293 0.073 Uiso 1 1 calc R . . . .
C15 C 0.5750(2) 0.3416(3) 0.88117(16) 0.0481(8) Uani 1 1 d . . . . .
H15 H 0.621359 0.338139 0.910362 0.058 Uiso 1 1 calc R . . . .
C16 C 0.54442(15) 0.4433(2) 0.85126(12) 0.0342(6) Uani 1 1 d . . . . .
C17 C 0.58281(13) 0.5548(2) 0.86806(12) 0.0319(5) Uani 1 1 d . . . . .
C18 C 0.64949(14) 0.5440(2) 0.86616(13) 0.0366(6) Uani 1 1 d . . . . .
C19 C 0.70776(16) 0.5150(3) 0.92383(15) 0.0467(7) Uani 1 1 d . . . . .
H19 H 0.707613 0.498152 0.967057 0.056 Uiso 1 1 calc R . . . .
C20 C 0.76580(16) 0.5111(3) 0.91727(18) 0.0532(8) Uani 1 1 d . . . . .
H20 H 0.806109 0.490372 0.955947 0.064 Uiso 1 1 calc R . . . .
C21 C 0.76525(16) 0.5374(3) 0.85445(19) 0.0495(8) Uani 1 1 d . . . . .
H21 H 0.805113 0.538198 0.849527 0.059 Uiso 1 1 calc R . . . .
C22 C 0.70461(14) 0.5628(2) 0.79837(16) 0.0403(6) Uani 1 1 d . . . . .
H22 H 0.703573 0.578476 0.754470 0.048 Uiso 1 1 calc R . . . .
C23A C 0.4335(3) 0.8811(4) 0.5357(2) 0.0342(11) Uani 0.711(10) 1 d D U P A 1
C23B C 0.4480(9) 0.8751(10) 0.5424(6) 0.0338(13) Uani 0.289(10) 1 d D U P A 2
C24A C 0.4360(6) 0.8418(5) 0.4710(3) 0.0409(19) Uani 0.711(10) 1 d D U P A 1
H24A H 0.467427 0.779215 0.482145 0.061 Uiso 0.711(10) 1 calc GR . P A 1
H24B H 0.450437 0.903905 0.450866 0.061 Uiso 0.711(10) 1 calc GR . P A 1
H24C H 0.391866 0.816576 0.437382 0.061 Uiso 0.711(10) 1 calc GR . P A 1
C24B C 0.4428(18) 0.8376(16) 0.4736(8) 0.070(10) Uani 0.289(10) 1 d D U P A 2
H24D H 0.436863 0.755714 0.469415 0.104 Uiso 0.289(10) 1 calc GR . P A 2
H24E H 0.483473 0.857977 0.470286 0.104 Uiso 0.289(10) 1 calc GR . P A 2
H24F H 0.404783 0.874413 0.436062 0.104 Uiso 0.289(10) 1 calc GR . 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 6 0 0.0375
-1 -1 13 0.0538
7 -7 -1 0.0650
6 6 -8 0.0409
8 -6 -8 0.0565
10 -6 -3 0.0675
-5 7 1 0.0582
-3 -4 11 0.0501
-11 0 13 0.0667
-6 -7 0 0.0253
-5 -6 7 0.0421
-12 -4 9 0.0589
6 -7 2 0.0644
11 -5 -1 0.0761
7 -5 -11 0.0627
-1 3 -11 0.0664
11 -4 -11 0.0585
11 -5 -6 0.0669
-9 -6 0 0.0380
6 0 -14 0.0693
12 0 -12 0.0574
9 5 -8 0.0450
5 7 -5 0.0327
14 -1 -5 0.0803
-5 7 7 0.0679
7 1 8 0.0727
-13 2 11 0.0705
1 1 12 0.0572
9 6 -6 0.0412
11 5 -6 0.0514
-4 0 -10 0.0671
4 4 9 0.0561
-10 4 10 0.0739
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
O1 Ni1 O1 81.68(7) . 2_656
O1 Ni1 O2 76.14(7) 2_656 2_656
O1 Ni1 O2 81.51(7) . 2_656
O1 Ni1 O7 94.27(9) . .
O1 Ni1 N1 77.34(8) . .
O5A Ni1 O1 169.08(15) . .
O5A Ni1 O1 101.69(19) . 2_656
O5A Ni1 O2 89.18(17) . 2_656
O5A Ni1 O7 95.88(17) . .
O5A Ni1 N1 98.84(19) . .
O5B Ni1 O1 167.2(5) . .
O5B Ni1 O7 97.9(4) . .
O5B Ni1 N1 106.6(5) . .
O7 Ni1 O1 93.32(8) . 2_656
O7 Ni1 O2 169.07(9) . 2_656
O7 Ni1 N1 88.84(9) . .
N1 Ni1 O1 159.01(8) . 2_656
N1 Ni1 O2 99.98(8) . 2_656
O2 Ni2 O1 78.78(7) . .
O2 Ni2 O1 81.00(7) 2_656 .
O2 Ni2 O2 83.87(7) . 2_656
O2 Ni2 N2 105.63(8) . .
O2 Ni2 N3 78.37(8) . .
O2 Ni2 N3 106.81(8) 2_656 .
O2 Ni2 N4 157.67(8) . 2_656
N2 Ni2 O1 78.63(8) . .
N2 Ni2 O2 155.24(8) . 2_656
N2 Ni2 N3 97.57(9) . .
N2 Ni2 N4 96.54(9) . 2_656
N3 Ni2 O1 154.83(8) . .
N4 Ni2 O1 108.82(8) 2_656 .
N4 Ni2 O2 76.89(8) 2_656 2_656
N4 Ni2 N3 96.32(9) 2_656 .
Ni1 O1 Ni1 96.33(7) . 2_656
Ni1 O1 Ni2 98.91(7) . .
Ni2 O1 Ni1 101.32(7) . 2_656
C6 O1 Ni1 116.41(14) . .
C6 O1 Ni1 130.62(15) . 2_656
C6 O1 Ni2 108.25(14) . .
Ni2 O2 Ni1 96.59(7) 2_656 2_656
Ni2 O2 Ni1 103.70(7) . 2_656
Ni2 O2 Ni2 94.37(7) . 2_656
C17 O2 Ni1 128.41(15) . 2_656
C17 O2 Ni2 110.40(14) . 2_656
C17 O2 Ni2 116.50(16) . .
C6 O3 H3 109.5 . .
C17 O4 H4 109.5 . .
C23A O5A Ni1 130.5(3) . .
C23B O5B Ni1 128.8(8) . .
Ni1 O7 H7A 114.9 . .
Ni1 O7 H7B 115.0 . .
H7A O7 H7B 103.7 . .
C1 N1 Ni1 125.8(2) . .
C1 N1 C5 118.6(2) . .
C5 N1 Ni1 115.55(17) . .
C7 N2 Ni2 113.78(17) . .
C11 N2 Ni2 127.0(2) . .
C11 N2 C7 119.2(2) . .
C12 N3 Ni2 127.0(2) . .
C12 N3 C16 118.6(3) . .
C16 N3 Ni2 114.35(18) . .
C18 N4 Ni2 113.96(18) . 2_656
C22 N4 Ni2 127.2(2) . 2_656
C22 N4 C18 118.7(2) . .
O9A N5A O8A 120.2(4) . .
O9A N5A O10A 121.3(4) . .
O10A N5A O8A 118.4(4) . .
O9B N5B O8B 120.0(4) . .
O9B N5B O10B 120.2(4) . .
O10B N5B O8B 119.8(4) . .
N1 C1 H1 119.0 . .
N1 C1 C2 122.0(3) . .
C2 C1 H1 119.0 . .
C1 C2 H2 120.3 . .
C3 C2 C1 119.5(3) . .
C3 C2 H2 120.3 . .
C2 C3 H3A 120.4 . .
C2 C3 C4 119.1(3) . .
C4 C3 H3A 120.4 . .
C3 C4 H4A 120.8 . .
C5 C4 C3 118.5(3) . .
C5 C4 H4A 120.8 . .
N1 C5 C4 122.3(2) . .
N1 C5 C6 115.0(2) . .
C4 C5 C6 122.7(2) . .
O1 C6 O3 112.6(2) . .
O1 C6 C5 108.3(2) . .
O1 C6 C7 108.12(19) . .
O3 C6 C5 107.6(2) . .
O3 C6 C7 108.2(2) . .
C7 C6 C5 112.1(2) . .
N2 C7 C6 115.6(2) . .
N2 C7 C8 121.3(3) . .
C8 C7 C6 123.1(3) . .
C7 C8 H8 120.3 . .
C7 C8 C9 119.4(3) . .
C9 C8 H8 120.3 . .
C8 C9 H9 120.4 . .
C10 C9 C8 119.1(3) . .
C10 C9 H9 120.4 . .
C9 C10 H10 120.8 . .
C9 C10 C11 118.5(3) . .
C11 C10 H10 120.8 . .
N2 C11 C10 122.4(3) . .
N2 C11 H11 118.8 . .
C10 C11 H11 118.8 . .
N3 C12 H12 119.0 . .
N3 C12 C13 122.0(4) . .
C13 C12 H12 119.0 . .
C12 C13 H13 120.3 . .
C14 C13 C12 119.5(3) . .
C14 C13 H13 120.3 . .
C13 C14 H14 120.3 . .
C13 C14 C15 119.4(3) . .
C15 C14 H14 120.3 . .
C14 C15 H15 120.9 . .
C14 C15 C16 118.3(3) . .
C16 C15 H15 120.9 . .
N3 C16 C15 122.2(3) . .
N3 C16 C17 115.9(2) . .
C15 C16 C17 121.8(3) . .
O2 C17 O4 111.63(19) . .
O2 C17 C16 109.2(2) . .
O2 C17 C18 108.0(2) . .
O4 C17 C16 105.3(2) . .
O4 C17 C18 110.4(2) . .
C18 C17 C16 112.3(2) . .
N4 C18 C17 114.9(2) . .
N4 C18 C19 121.9(3) . .
C19 C18 C17 123.3(3) . .
C18 C19 H19 120.6 . .
C20 C19 C18 118.8(3) . .
C20 C19 H19 120.6 . .
C19 C20 H20 120.1 . .
C19 C20 C21 119.8(3) . .
C21 C20 H20 120.1 . .
C20 C21 H21 120.9 . .
C20 C21 C22 118.1(3) . .
C22 C21 H21 120.9 . .
N4 C22 C21 122.6(3) . .
N4 C22 H22 118.7 . .
C21 C22 H22 118.7 . .
O5A C23A C24A 118.2(3) . .
O6A C23A O5A 122.0(4) . .
O6A C23A C24A 119.4(4) . .
O5B C23B C24B 116.3(6) . .
O6B C23B O5B 121.5(10) . .
O6B C23B C24B 118.2(6) . .
C23A C24A H24A 109.5 . .
C23A C24A H24B 109.5 . .
C23A C24A H24C 109.5 . .
H24A C24A H24B 109.5 . .
H24A C24A H24C 109.5 . .
H24B C24A H24C 109.5 . .
C23B C24B H24D 109.5 . .
C23B C24B H24E 109.5 . .
C23B C24B H24F 109.5 . .
H24D C24B H24E 109.5 . .
H24D C24B H24F 109.5 . .
H24E C24B H24F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.0478(17) .
Ni1 O1 2.1325(17) 2_656
Ni1 O2 2.1464(17) 2_656
Ni1 O5A 2.019(2) .
Ni1 O5B 2.021(4) .
Ni1 O7 2.076(2) .
Ni1 N1 2.097(2) .
Ni2 O1 2.1210(18) .
Ni2 O2 2.0968(17) 2_656
Ni2 O2 2.0359(18) .
Ni2 N2 2.042(2) .
Ni2 N3 2.097(2) .
Ni2 N4 2.095(2) 2_656
O1 C6 1.390(3) .
O2 C17 1.388(3) .
O3 H3 0.8400 .
O3 C6 1.407(3) .
O4 H4 0.8400 .
O4 C17 1.416(3) .
O5A C23A 1.269(4) .
O5B C23B 1.269(5) .
O6A C23A 1.232(5) .
O6B C23B 1.234(6) .
O7 H7A 0.9566 .
O7 H7B 0.9603 .
O8A N5A 1.254(3) .
O8B N5B 1.248(3) .
O9A N5A 1.242(3) .
O9B N5B 1.243(3) .
O10A N5A 1.242(3) .
O10B N5B 1.245(3) .
N1 C1 1.342(3) .
N1 C5 1.344(4) .
N2 C7 1.350(4) .
N2 C11 1.342(4) .
N3 C12 1.345(4) .
N3 C16 1.346(4) .
N4 C18 1.348(4) .
N4 C22 1.332(4) .
C1 H1 0.9500 .
C1 C2 1.385(5) .
C2 H2 0.9500 .
C2 C3 1.371(5) .
C3 H3A 0.9500 .
C3 C4 1.391(4) .
C4 H4A 0.9500 .
C4 C5 1.386(4) .
C5 C6 1.546(3) .
C6 C7 1.534(4) .
C7 C8 1.378(4) .
C8 H8 0.9500 .
C8 C9 1.394(5) .
C9 H9 0.9500 .
C9 C10 1.381(5) .
C10 H10 0.9500 .
C10 C11 1.385(4) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C12 C13 1.383(5) .
C13 H13 0.9500 .
C13 C14 1.371(6) .
C14 H14 0.9500 .
C14 C15 1.387(6) .
C15 H15 0.9500 .
C15 C16 1.397(4) .
C16 C17 1.534(4) .
C17 C18 1.527(4) .
C18 C19 1.388(4) .
C19 H19 0.9500 .
C19 C20 1.377(5) .
C20 H20 0.9500 .
C20 C21 1.378(5) .
C21 H21 0.9500 .
C21 C22 1.393(4) .
C22 H22 0.9500 .
C23A C24A 1.490(4) .
C23B C24B 1.496(5) .
C24A H24A 0.9800 .
C24A H24B 0.9800 .
C24A H24C 0.9800 .
C24B H24D 0.9800 .
C24B H24E 0.9800 .
C24B H24F 0.9800 .
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
Ni1 O1 C6 O3 -88.5(2) .
Ni1 O1 C6 O3 37.5(3) 2_656
Ni1 O1 C6 C5 156.38(16) 2_656
Ni1 O1 C6 C5 30.3(2) .
Ni1 O1 C6 C7 -81.9(2) 2_656
Ni1 O1 C6 C7 152.02(16) .
Ni1 O2 C17 O4 47.6(3) 2_656
Ni1 O2 C17 C16 163.66(15) 2_656
Ni1 O2 C17 C18 -73.9(2) 2_656
Ni1 O5A C23A O6A -27.5(6) .
Ni1 O5A C23A C24A 160.3(7) .
Ni1 O5B C23B O6B 20.4(16) .
Ni1 O5B C23B C24B 177(2) .
Ni1 N1 C1 C2 -177.4(2) .
Ni1 N1 C5 C4 179.4(2) .
Ni1 N1 C5 C6 1.7(3) .
Ni2 O1 C6 O3 161.27(16) .
Ni2 O1 C6 C5 -79.90(19) .
Ni2 O1 C6 C7 41.8(2) .
Ni2 O2 C17 O4 -89.6(2) .
Ni2 O2 C17 O4 164.40(18) 2_656
Ni2 O2 C17 C16 -79.5(2) 2_656
Ni2 O2 C17 C16 26.5(2) .
Ni2 O2 C17 C18 148.94(16) .
Ni2 O2 C17 C18 42.9(2) 2_656
Ni2 N2 C7 C6 2.4(3) .
Ni2 N2 C7 C8 -176.7(2) .
Ni2 N2 C11 C10 178.7(3) .
Ni2 N3 C12 C13 -177.1(2) .
Ni2 N3 C16 C15 178.6(2) .
Ni2 N3 C16 C17 2.0(3) .
Ni2 N4 C18 C17 1.7(3) 2_656
Ni2 N4 C18 C19 -177.7(2) 2_656
Ni2 N4 C22 C21 175.3(2) 2_656
O1 C6 C7 N2 -30.7(3) .
O1 C6 C7 C8 148.4(3) .
O2 C17 C18 N4 -29.7(3) .
O2 C17 C18 C19 149.7(3) .
O3 C6 C7 N2 -152.9(2) .
O3 C6 C7 C8 26.2(4) .
O4 C17 C18 N4 -151.9(2) .
O4 C17 C18 C19 27.4(4) .
N1 C1 C2 C3 -1.6(5) .
N1 C5 C6 O1 -20.2(3) .
N1 C5 C6 O3 101.8(3) .
N1 C5 C6 C7 -139.4(2) .
N2 C7 C8 C9 -2.8(5) .
N3 C12 C13 C14 -1.8(5) .
N3 C16 C17 O2 -18.1(3) .
N3 C16 C17 O4 101.9(2) .
N3 C16 C17 C18 -137.9(2) .
N4 C18 C19 C20 1.5(5) .
C1 N1 C5 C4 2.0(4) .
C1 N1 C5 C6 -175.7(2) .
C1 C2 C3 C4 1.8(5) .
C2 C3 C4 C5 -0.2(5) .
C3 C4 C5 N1 -1.8(4) .
C3 C4 C5 C6 175.8(3) .
C4 C5 C6 O1 162.1(2) .
C4 C5 C6 O3 -75.9(3) .
C4 C5 C6 C7 42.9(3) .
C5 N1 C1 C2 -0.3(5) .
C5 C6 C7 N2 88.7(3) .
C5 C6 C7 C8 -92.2(3) .
C6 C7 C8 C9 178.2(3) .
C7 N2 C11 C10 1.6(5) .
C7 C8 C9 C10 2.4(5) .
C8 C9 C10 C11 -0.2(6) .
C9 C10 C11 N2 -1.9(5) .
C11 N2 C7 C6 179.9(2) .
C11 N2 C7 C8 0.8(4) .
C12 N3 C16 C15 -0.5(4) .
C12 N3 C16 C17 -177.1(2) .
C12 C13 C14 C15 0.3(5) .
C13 C14 C15 C16 1.0(5) .
C14 C15 C16 N3 -0.9(4) .
C14 C15 C16 C17 175.5(3) .
C15 C16 C17 O2 165.3(2) .
C15 C16 C17 O4 -74.6(3) .
C15 C16 C17 C18 45.5(3) .
C16 N3 C12 C13 1.9(4) .
C16 C17 C18 N4 90.8(3) .
C16 C17 C18 C19 -89.8(3) .
C17 C18 C19 C20 -177.9(3) .
C18 N4 C22 C21 0.2(4) .
C18 C19 C20 C21 0.9(5) .
C19 C20 C21 C22 -2.6(5) .
C20 C21 C22 N4 2.1(5) .
C22 N4 C18 C17 177.4(2) .
C22 N4 C18 C19 -2.0(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
7.0066 6.0026 -0.0059 0.8909 -0.2859 -0.1284
-0.9963 -0.9981 13.0030 0.4418 0.8618 0.3190
6.9937 -7.0034 -0.9883 -0.3249 0.0871 0.9830
6.0036 6.0012 -8.0074 0.4828 -0.7760 -0.3621
7.9922 -6.0042 -7.9904 -0.4981 -0.3980 0.7970
9.9943 -6.0033 -2.9890 -0.1742 -0.1083 1.0207
-4.9934 7.0033 0.9889 0.4250 -0.1114 -0.8702
-3.0002 -3.9998 11.0061 -0.0181 0.8610 0.4235
-10.9965 0.0024 12.9984 0.0313 0.9493 -0.3322
-6.0075 -7.0031 0.0076 -0.9310 0.3073 0.2720
-5.0038 -6.0014 7.0076 -0.4775 0.7011 0.3964
-12.0019 -4.0001 9.0029 -0.5582 0.8444 -0.1285
5.9947 -7.0028 2.0118 -0.2407 0.2876 0.9931
10.9961 -5.0025 -0.9897 0.0555 -0.0283 1.0342
6.9919 -5.0042 -10.9925 -0.5924 -0.6077 0.5869
-1.0012 2.9994 -11.0061 -0.2722 -0.7790 -0.5619
10.9934 -4.0038 -10.9926 -0.3021 -0.6897 0.7253
10.9942 -5.0034 -5.9905 -0.1683 -0.3422 0.9234
-9.0068 -6.0026 0.0052 -0.9911 0.3101 0.0155
5.9956 -0.0025 -14.0001 -0.3263 -0.9516 0.0280
11.9970 -0.0022 -11.9979 0.0636 -0.8987 0.4108
9.0029 5.0007 -8.0051 0.5429 -0.7788 -0.1057
5.0055 7.0022 -5.0087 0.6571 -0.6091 -0.4392
13.9988 -1.0014 -4.9948 0.3870 -0.4499 0.7660
-4.9912 7.0044 6.9899 0.6936 0.2653 -0.7372
7.0047 1.0018 8.0022 0.7986 0.3840 0.4850
-12.9955 2.0029 10.9946 0.0218 0.7809 -0.6637
1.0055 1.0026 12.0008 0.6773 0.7077 0.2353
9.0046 6.0016 -6.0061 0.7225 -0.6868 -0.1486
11.0039 5.0011 -6.0041 0.7325 -0.6775 0.0514
-4.0041 -0.0018 -10.0029 -0.6479 -0.5794 -0.4473
4.0076 4.0034 8.9972 0.9635 0.3825 0.0764
-9.9936 4.0036 9.9928 0.3074 0.6148 -0.6911
