#------------------------------------------------------------------------------
#$Date: 2024-03-04 22:14:42 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290167 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/49/7714920.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_7714920
loop_
_publ_author_name
'Pavun, Anna'
'Niess, Raffael'
'Scheibel, Lucas A.'
'Seidl, Michael'
'Hohloch, Stephan'
_publ_section_title
;
 A mesoionic carbene stabilized nickel(II) hydroxide complex: a facile
 precursor for C-H activation chemistry.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2749
_journal_page_last               2761
_journal_paper_doi               10.1039/d3dt03746k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C39.92 H47.28 Cl0.12 N7 Ni O6.16'
_chemical_formula_sum            'C39.92 H47.28 Cl0.12 N7 Ni O6.16'
_chemical_formula_weight         786.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-07 deposited with the CCDC.	2024-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2879(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.26757(15)
_cell_length_b                   13.99843(13)
_cell_length_c                   22.5929(2)
_cell_measurement_reflns_used    19755
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.8240
_cell_measurement_theta_min      3.1460
_cell_volume                     3848.46(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.91a 64-bit (release 29-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     30.00 106.00   0.50   10.00    --   62.92   9.00  43.00  152
  2  ω     30.00 106.00   0.50   10.00    --   62.92   9.00  43.00  152
  3  ω   -107.00 -30.00   0.50   10.00    --  -63.82  -9.00-130.00  154
  4  ω     43.00 119.00   0.50   10.00    --   75.87   9.00  43.00  152
  5  ω   -119.00 -43.00   0.50   10.00    --  -76.65  -9.00-130.00  152
  6  ω    -90.00 -58.00   0.50   10.00    --  -50.00 -65.00  80.24   64
  7  ω     25.00  71.00   0.50   10.00    --   62.92 -95.00-150.00   92
  8  ω     25.00  71.00   0.50   10.00    --   62.92 -95.00 150.00   92
  9  ω   -106.00 -75.00   0.50   10.00    --  -70.00 -74.00-109.13   62
 10  ω   -113.00 -80.00   0.50   10.00    --  -70.00 -54.00-173.72   66
 11  ω   -100.00 -32.00   0.50   10.00    --  -73.68 125.00  90.00  136
 12  ω   -116.00 -40.00   0.50   10.00    --  -73.68  -9.00-130.00  152
 13  ω   -100.00 -32.00   0.50   10.00    --  -73.68 125.00  90.00  136
 14  ω   -120.00 -87.00   0.50   10.00    --  -74.00 -41.00-151.06   66
 15  ω   -110.00 -79.00   0.50   10.00    --  -74.00 -74.00 -20.75   62
 16  ω     38.00  84.00   0.50   10.00    --   75.87 -95.00-180.00   92
 17  ω   -117.00 -86.00   0.50   10.00    --  -78.25 -67.00 108.08   62
 18  ω   -114.00 -79.00   0.50   10.00    --  -78.25 -90.00-145.15   70
 19  ω   -112.00 -36.00   0.50   10.00    --  -78.25 135.00  79.99  152
 20  ω    -91.00 -39.00   0.50   10.00    --  -78.25 102.00 144.73  104
 21  ω     68.00 127.00   0.50   10.00    --   79.75  24.00-155.94  118
 22  ω     90.00 127.00   0.50   10.00    --   79.75  36.00-121.52   74
 23  ω     38.00 105.00   0.50   10.00    --   79.75-122.00  50.60  134
 24  ω     48.00 124.00   0.50   10.00    --   79.75  13.00  28.95  152
 25  ω     68.00 127.00   0.50   10.00    --   79.75  24.00 162.11  118
 26  ω     37.00 108.00   0.50   10.00    --   79.75-126.00 135.61  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0356826000
_diffrn_orient_matrix_UB_12      0.0100496000
_diffrn_orient_matrix_UB_13      0.0675898000
_diffrn_orient_matrix_UB_21      -0.1206777000
_diffrn_orient_matrix_UB_22      -0.0084267000
_diffrn_orient_matrix_UB_23      0.0114022000
_diffrn_orient_matrix_UB_31      0.0127880000
_diffrn_orient_matrix_UB_32      -0.1093464000
_diffrn_orient_matrix_UB_33      0.0054048000
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47663
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.440
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.94a (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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       plate
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7565
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0638
_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)+(0.0560P)²+6.9852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6505
_reflns_number_total             7565
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03746k2.cif
_cod_data_source_block           ni_malon4_abs
_cod_depositor_comments
'Adding full bibliography for 7714908--7714920.cif.'
_cod_database_code               7714920
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C102  H0  N66  O62  Cl0  Ni4  '
_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   0.981
_shelx_estimated_absorpt_t_min   0.905
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29-C28A \\sim C29-C28 \\sim C28A-C27 \\sim C28-C27
 with sigma of 0.02
 C19A-C17 \\sim C19-C17 \\sim C20A-C17 \\sim C20-C17 \\sim C18A-C17 \\sim
C18-C17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C28A \\sim C28: within 1.9A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.9A
C20 \\sim C20A \\sim C19 \\sim C19A \\sim C17 \\sim C18A \\sim C18: within 1.9A
with sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.9A
4. Rigid body (RIGU) restrains
 C19, C19A, C17, C20, C20A, C18A, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Ni1(0.88) O1(0.88) O3(0.88) O2(0.88) O5(0.88) O7(0.88) O4(0.88)
 O6(0.88) H27A(0.8) H27B(0.8) H27C(0.2) H27D(0.2) C34(0.88) C39(0.88)
 H39A(0.88) H39B(0.88) C33(0.88) C35(0.88) C38(0.88) H38A(0.88) H38B(0.88)
 H38C(0.88) C40(0.88) C18(0.86) H18A(0.86) H18B(0.86) H18C(0.86) C37(0.88)
 C28(0.8) H28A(0.8) H28B(0.8) H29A(0.8) H29B(0.8) C36(0.88) H36A(0.88)
 H36B(0.88) H36C(0.88) C20(0.86) H20A(0.86) H20B(0.86) H20C(0.86) C19(0.86)
 H19A(0.86) H19B(0.86) H19C(0.86) C41(0.88) H41A(0.88) H41B(0.88) H41C(0.88)
 Ni1A(0.12) Cl1A(0.12) C20A(0.14) H20D(0.14) H20E(0.14) H20F(0.14) C18A(0.14)
 H18D(0.14) H18E(0.14) H18F(0.14) C19A(0.14) H19D(0.14) H19E(0.14) H19F(0.14)
 C28A(0.2) H28C(0.2) H28D(0.2)
6.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C27(H27C,H27D), C30(H30A,H30B), C39(H39A,H39B), C21(H21A,
 H21B), C24(H24A,H24B), C22(H22A,H22B), C28(H28A,H28B), C23(H23A,H23B),
 C29(H29A,H29B), C28A(H28C,H28D)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C3(H3), C10(H10)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C38(H38A,H38B,H38C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C36(H36A,H36B,H36C), C20(H20A,H20B,H20C), C19(H19A,
 H19B,H19C), C41(H41A,H41B,H41C), C20A(H20D,H20E,H20F), C18A(H18D,H18E,H18F),
 C19A(H19D,H19E,H19F)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems, Cryostream 700'
_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 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.781
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.57858(6) 0.27898(4) 0.22400(3) 0.02724(17) Uani 0.88 1 d . . P A 1
O1 O 0.49479(19) 0.28925(16) 0.28958(10) 0.0289(5) Uani 0.88 1 d . . P A 1
N10 N 0.6386(2) 0.26610(17) 0.15256(11) 0.0283(5) Uani 1 1 d . . . . .
N1 N 0.6115(2) 0.07215(18) 0.19683(11) 0.0331(6) Uani 1 1 d . . . . .
O43 O 0.1763(2) 0.2949(2) 0.38139(11) 0.0421(6) Uani 0.88 1 d . . P A 1
N2 N 0.6258(2) 0.47087(18) 0.17704(11) 0.0310(5) Uani 1 1 d . . . . .
N5 N 0.5751(2) -0.00823(18) 0.26856(12) 0.0362(6) Uani 1 1 d . . . . .
O42 O 0.1499(2) 0.2770(2) 0.28264(11) 0.0419(6) Uani 0.88 1 d . . P A 1
O45 O 0.3834(2) 0.21980(19) 0.42790(11) 0.0410(6) Uani 0.88 1 d . . P A 1
N4 N 0.6297(2) 0.56516(18) 0.18700(12) 0.0351(6) Uani 1 1 d . . . . .
O41 O 0.3154(2) 0.13209(19) 0.22536(12) 0.0442(6) Uani 0.88 1 d . . P A 1
N6 N 0.6007(2) 0.57131(18) 0.24112(11) 0.0332(6) Uani 1 1 d . . . . .
N3 N 0.6045(2) -0.01875(19) 0.21481(12) 0.0362(6) Uani 1 1 d . . . . .
O44 O 0.4533(3) 0.3608(2) 0.41360(13) 0.0613(9) Uani 0.88 1 d . . P A 1
C14 C 0.6422(3) 0.0893(2) 0.13939(14) 0.0325(7) Uani 1 1 d . . . . .
C24 C 0.6555(2) 0.3382(2) 0.11330(13) 0.0285(6) Uani 1 1 d . . . . .
C1 C 0.5854(3) 0.1411(2) 0.23644(14) 0.0381(7) Uani 1 1 d . . . . .
C20 C 0.6926(2) 0.3657(2) 0.01055(13) 0.0326(7) Uani 1 1 d . . . . .
H5 H 0.707833 0.341048 -0.026714 0.039 Uiso 1 1 calc R U . . .
C13 C 0.6516(2) 0.1829(2) 0.12121(13) 0.0289(6) Uani 1 1 d . . . . .
C23 C 0.6503(2) 0.4366(2) 0.12091(13) 0.0311(6) Uani 1 1 d . . . . .
O40 O 0.2281(3) 0.2071(2) 0.14542(15) 0.0689(10) Uani 0.88 1 d . . P A 1
C19 C 0.6793(2) 0.3032(2) 0.05720(13) 0.0308(6) Uani 1 1 d . . . . .
C2 C 0.5932(3) 0.4168(2) 0.22235(14) 0.0362(7) Uani 1 1 d . . . . .
C17 C 0.6981(2) 0.1246(2) 0.02555(14) 0.0327(7) Uani 1 1 d . . . . .
H8 H 0.715559 0.137285 -0.013466 0.039 Uiso 1 1 calc R U . . .
C4 C 0.5790(3) 0.4862(2) 0.26498(14) 0.0354(7) Uani 1 1 d . . . . .
C18 C 0.6789(2) 0.2004(2) 0.06301(14) 0.0311(6) Uani 1 1 d . . . . .
C22 C 0.6639(3) 0.4988(2) 0.07439(14) 0.0342(7) Uani 1 1 d . . . . .
H3 H 0.659760 0.565738 0.080599 0.041 Uiso 1 1 calc R U . . .
C15 C 0.6623(3) 0.0137(2) 0.10178(14) 0.0355(7) Uani 1 1 d . . . . .
H10 H 0.655637 -0.050121 0.115185 0.043 Uiso 1 1 calc R U . . .
C16 C 0.6918(3) 0.0299(2) 0.04505(14) 0.0345(7) Uani 1 1 d . . . . .
C21 C 0.6837(3) 0.4640(2) 0.01824(14) 0.0338(7) Uani 1 1 d . . . . .
C11 C 0.5544(3) -0.0953(2) 0.30222(15) 0.0391(8) Uani 1 1 d D . . . .
H27A H 0.624953 -0.123597 0.320047 0.047 Uiso 0.8 1 calc R U P B 1
H27B H 0.515066 -0.143061 0.275078 0.047 Uiso 0.8 1 calc R U P B 1
H27C H 0.611120 -0.143680 0.296739 0.047 Uiso 0.2 1 calc R U P C 2
H27D H 0.481919 -0.122127 0.286202 0.047 Uiso 0.2 1 calc R U P C 2
C5 C 0.5295(4) 0.1053(2) 0.34465(15) 0.0473(9) Uani 1 1 d . . . . .
H30A H 0.579331 0.154148 0.364898 0.057 Uiso 1 1 calc R U . . .
H30B H 0.454367 0.132522 0.338914 0.057 Uiso 1 1 calc R U . . .
C29 C 0.6943(3) 0.5354(2) -0.03249(14) 0.0380(7) Uani 1 1 d . . . . .
C41 C 0.3321(3) 0.2908(2) 0.33359(15) 0.0305(7) Uani 0.88 1 d . . P A 1
C42 C 0.3294(3) 0.3002(3) 0.22105(15) 0.0342(8) Uani 0.88 1 d . . P A 1
H39A H 0.268110 0.346065 0.221595 0.041 Uiso 0.88 1 calc R U P A 1
H39B H 0.380907 0.327659 0.195210 0.041 Uiso 0.88 1 calc R U P A 1
C31 C 0.6079(3) 0.6141(3) -0.03389(16) 0.0440(8) Uani 1 1 d . . . . .
H14A H 0.620889 0.651788 0.002876 0.066 Uiso 1 1 calc R U . . .
H14B H 0.534566 0.585281 -0.037095 0.066 Uiso 1 1 calc R U . . .
H14C H 0.612745 0.655678 -0.068341 0.066 Uiso 1 1 calc R U . . .
C40 C 0.3890(3) 0.2922(2) 0.28390(15) 0.0293(7) Uani 0.88 1 d . . P A 1
C12 C 0.5952(3) 0.6666(2) 0.26869(15) 0.0434(8) Uani 1 1 d . . . . .
H21A H 0.564815 0.713553 0.238219 0.052 Uiso 1 1 calc R U . . .
H21B H 0.669848 0.687665 0.285300 0.052 Uiso 1 1 calc R U . . .
C3 C 0.5641(3) 0.0841(2) 0.28500(15) 0.0392(8) Uani 1 1 d . . . . .
C45 C 0.2123(3) 0.2861(3) 0.32822(16) 0.0331(7) Uani 0.88 1 d . . P A 1
C25 C 0.7137(3) -0.0537(2) 0.00396(16) 0.0419(8) Uani 1 1 d D U . . .
C6 C 0.5415(3) 0.4820(2) 0.32527(14) 0.0401(8) Uani 1 1 d . . . . .
H24A H 0.585396 0.433393 0.349588 0.048 Uiso 1 1 calc R U . . .
H24B H 0.463704 0.461467 0.320886 0.048 Uiso 1 1 calc R U . . .
C30 C 0.8083(3) 0.5828(3) -0.02242(18) 0.0513(9) Uani 1 1 d . . . . .
H15A H 0.815457 0.627788 -0.054928 0.077 Uiso 1 1 calc R U . . .
H15B H 0.865325 0.533648 -0.021598 0.077 Uiso 1 1 calc R U . . .
H15C H 0.816580 0.617160 0.015673 0.077 Uiso 1 1 calc R U . . .
C10 C 0.5229(4) 0.6611(3) 0.31762(17) 0.0515(10) Uani 1 1 d . . . . .
H22A H 0.530453 0.720866 0.341251 0.062 Uiso 1 1 calc R U . . .
H22B H 0.445227 0.655444 0.299706 0.062 Uiso 1 1 calc R U . . .
C47 C 0.4414(3) 0.2243(3) 0.48816(18) 0.0456(10) Uani 0.88 1 d . . P A 1
H38A H 0.519794 0.235097 0.486327 0.068 Uiso 0.88 1 calc R U P A 1
H38B H 0.431567 0.163961 0.508828 0.068 Uiso 0.88 1 calc R U P A 1
H38C H 0.411788 0.276915 0.509904 0.068 Uiso 0.88 1 calc R U P A 1
C43 C 0.2837(3) 0.2086(3) 0.19299(16) 0.0383(8) Uani 0.88 1 d . . P A 1
C32 C 0.6805(4) 0.4857(3) -0.09374(16) 0.0643(13) Uani 1 1 d . . . . .
H16A H 0.607951 0.455512 -0.100716 0.096 Uiso 1 1 calc R U . . .
H16B H 0.737602 0.436836 -0.094484 0.096 Uiso 1 1 calc R U . . .
H16C H 0.687288 0.532994 -0.125030 0.096 Uiso 1 1 calc R U . . .
C27 C 0.8213(3) -0.0382(3) -0.0217(2) 0.0441(10) Uani 0.86 1 d D U P D 1
H18A H 0.835445 -0.092911 -0.046700 0.066 Uiso 0.86 1 calc R U P D 1
H18B H 0.881531 -0.031791 0.010946 0.066 Uiso 0.86 1 calc R U P D 1
H18C H 0.816146 0.020123 -0.045927 0.066 Uiso 0.86 1 calc R U P D 1
C46 C 0.3949(3) 0.2957(3) 0.39466(16) 0.0348(8) Uani 0.88 1 d . . P A 1
C9 C 0.4851(4) -0.0690(3) 0.35122(19) 0.0390(9) Uani 0.8 1 d D U P E 1
H28A H 0.408245 -0.057535 0.333472 0.047 Uiso 0.8 1 calc R U P E 1
H28B H 0.485363 -0.122612 0.379822 0.047 Uiso 0.8 1 calc R U P E 1
C8 C 0.5521(3) 0.5775(3) 0.35822(15) 0.0455(8) Uani 1 1 d . . . . .
H23A H 0.503397 0.577194 0.389950 0.055 Uiso 1 1 calc R U . . .
H23B H 0.628663 0.585103 0.377612 0.055 Uiso 1 1 calc R U . . .
C7 C 0.5304(4) 0.0197(3) 0.38368(16) 0.0497(9) Uani 1 1 d D . . . .
H29A H 0.486474 0.033536 0.416536 0.060 Uiso 0.8 1 calc R U P E 1
H29B H 0.606855 0.007079 0.401685 0.060 Uiso 0.8 1 calc R U P E 1
C48 C 0.0582(3) 0.2875(3) 0.38127(18) 0.0446(9) Uani 0.88 1 d . . P A 1
H36A H 0.021521 0.337526 0.355759 0.067 Uiso 0.88 1 calc R U P A 1
H36B H 0.040279 0.295139 0.422056 0.067 Uiso 0.88 1 calc R U P A 1
H36C H 0.033141 0.224659 0.365926 0.067 Uiso 0.88 1 calc R U P A 1
C28 C 0.7292(4) -0.1501(3) 0.0391(2) 0.0531(11) Uani 0.86 1 d D U P D 1
H20A H 0.661042 -0.166257 0.055202 0.080 Uiso 0.86 1 calc R U P D 1
H20B H 0.789078 -0.143434 0.071889 0.080 Uiso 0.86 1 calc R U P D 1
H20C H 0.747148 -0.200890 0.012080 0.080 Uiso 0.86 1 calc R U P D 1
C26 C 0.6182(4) -0.0651(4) -0.0434(2) 0.0594(13) Uani 0.86 1 d D U P D 1
H19A H 0.629419 -0.121550 -0.067576 0.089 Uiso 0.86 1 calc R U P D 1
H19B H 0.611828 -0.008256 -0.068997 0.089 Uiso 0.86 1 calc R U P D 1
H19C H 0.550780 -0.072866 -0.024893 0.089 Uiso 0.86 1 calc R U P D 1
C44 C 0.2812(4) 0.0399(3) 0.2026(2) 0.0648(14) Uani 0.88 1 d . . P A 1
H41A H 0.222269 0.047273 0.169363 0.097 Uiso 0.88 1 calc R U P A 1
H41B H 0.254221 0.002210 0.234346 0.097 Uiso 0.88 1 calc R U P A 1
H41C H 0.343656 0.006973 0.188656 0.097 Uiso 0.88 1 calc R U P A 1
Ni1A Ni 0.6503(4) 0.2679(3) 0.23492(19) 0.0281(9) Uani 0.12 1 d . . P A 2
Cl1A Cl 0.7189(7) 0.2782(5) 0.3281(3) 0.0481(17) Uani 0.12 1 d . . P A 2
C28A C 0.631(2) -0.1342(16) 0.0084(14) 0.055(4) Uani 0.14 1 d D U P D 2
H20D H 0.556794 -0.110786 -0.004618 0.083 Uiso 0.14 1 calc R U P D 2
H20E H 0.636136 -0.156036 0.049889 0.083 Uiso 0.14 1 calc R U P D 2
H20F H 0.647940 -0.187430 -0.017111 0.083 Uiso 0.14 1 calc R U P D 2
C27A C 0.8325(14) -0.081(3) 0.0047(17) 0.062(5) Uani 0.14 1 d D U P D 2
H18D H 0.838450 -0.133987 -0.022744 0.093 Uiso 0.14 1 calc R U P D 2
H18E H 0.863027 -0.099595 0.045192 0.093 Uiso 0.14 1 calc R U P D 2
H18F H 0.873583 -0.025683 -0.007819 0.093 Uiso 0.14 1 calc R U P D 2
C26A C 0.664(3) -0.0198(19) -0.0603(8) 0.058(5) Uani 0.14 1 d D U P D 2
H19D H 0.642032 -0.075686 -0.085083 0.087 Uiso 0.14 1 calc R U P D 2
H19E H 0.720055 0.016321 -0.078399 0.087 Uiso 0.14 1 calc R U P D 2
H19F H 0.600285 0.020962 -0.057530 0.087 Uiso 0.14 1 calc R U P D 2
C9A C 0.5560(18) -0.0752(10) 0.3672(6) 0.052(4) Uani 0.2 1 d D U P E 2
H28C H 0.503297 -0.119114 0.382984 0.062 Uiso 0.2 1 calc R U P E 2
H28D H 0.630064 -0.091180 0.387487 0.062 Uiso 0.2 1 calc R U P E 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'
Cl Cl 0.3639 0.7018 '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
0 1 -2 0.0323
0 -1 2 0.0189
0 1 1 0.0422
0 -1 -1 0.0306
-1 0 1 0.0022
1 0 -1 0.0132
0 1 2 0.0308
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 C1 88.86(12) . . ?
O1 Ni1 C2 90.01(12) . . ?
N10 Ni1 O1 170.80(11) . . ?
N10 Ni1 C1 90.84(12) . . ?
N10 Ni1 C2 91.83(12) . . ?
C2 Ni1 C1 170.12(15) . . ?
C40 O1 Ni1 124.0(2) . . ?
C24 N10 Ni1 126.5(2) . . ?
C24 N10 C13 104.5(2) . . ?
C24 N10 Ni1A 129.8(2) . . ?
C13 N10 Ni1 127.5(2) . . ?
C13 N10 Ni1A 121.9(2) . . ?
N3 N1 C14 118.2(2) . . ?
N3 N1 C1 115.9(2) . . ?
C1 N1 C14 125.9(3) . . ?
C45 O43 C48 115.8(3) . . ?
N4 N2 C23 118.4(2) . . ?
N4 N2 C2 115.2(2) . . ?
C2 N2 C23 126.3(3) . . ?
N3 N5 C11 117.9(2) . . ?
N3 N5 C3 114.0(3) . . ?
C3 N5 C11 128.0(3) . . ?
C46 O45 C47 115.0(3) . . ?
N6 N4 N2 102.2(2) . . ?
C43 O41 C44 118.6(3) . . ?
N4 N6 C4 113.8(3) . . ?
N4 N6 C12 118.8(3) . . ?
C4 N6 C12 127.4(3) . . ?
N5 N3 N1 102.0(2) . . ?
C13 C14 N1 118.3(3) . . ?
C13 C14 C15 120.6(3) . . ?
C15 C14 N1 121.1(3) . . ?
N10 C24 C23 129.3(3) . . ?
N10 C24 C19 112.7(3) . . ?
C23 C24 C19 118.0(3) . . ?
N1 C1 Ni1 127.4(2) . . ?
N1 C1 C3 101.0(3) . . ?
N1 C1 Ni1A 119.8(3) . . ?
C3 C1 Ni1 131.6(2) . . ?
C3 C1 Ni1A 130.3(3) . . ?
C19 C20 H5 119.8 . . ?
C21 C20 H5 119.8 . . ?
C21 C20 C19 120.4(3) . . ?
N10 C13 C14 128.8(3) . . ?
N10 C13 C18 112.7(3) . . ?
C14 C13 C18 118.5(3) . . ?
C24 C23 N2 117.6(3) . . ?
C24 C23 C22 121.0(3) . . ?
C22 C23 N2 121.4(3) . . ?
C24 C19 C18 105.0(3) . . ?
C20 C19 C24 120.9(3) . . ?
C20 C19 C18 134.0(3) . . ?
N2 C2 Ni1 126.8(2) . . ?
N2 C2 C4 101.8(3) . . ?
N2 C2 Ni1A 120.0(2) . . ?
C4 C2 Ni1 131.3(2) . . ?
C4 C2 Ni1A 129.4(3) . . ?
C18 C17 H8 119.7 . . ?
C18 C17 C16 120.5(3) . . ?
C16 C17 H8 119.7 . . ?
N6 C4 C2 106.9(3) . . ?
N6 C4 C6 119.9(3) . . ?
C2 C4 C6 133.1(3) . . ?
C13 C18 C19 105.0(3) . . ?
C17 C18 C13 120.6(3) . . ?
C17 C18 C19 134.4(3) . . ?
C23 C22 H3 119.5 . . ?
C23 C22 C21 121.0(3) . . ?
C21 C22 H3 119.5 . . ?
C14 C15 H10 119.3 . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 H10 119.3 . . ?
C17 C16 C25 120.6(3) . . ?
C15 C16 C17 118.3(3) . . ?
C15 C16 C25 121.1(3) . . ?
C20 C21 C22 118.6(3) . . ?
C20 C21 C29 122.2(3) . . ?
C22 C21 C29 119.2(3) . . ?
N5 C11 H27A 109.9 . . ?
N5 C11 H27B 109.9 . . ?
N5 C11 H27C 109.3 . . ?
N5 C11 H27D 109.3 . . ?
N5 C11 C9 108.9(3) . . ?
N5 C11 C9A 111.7(6) . . ?
H27A C11 H27B 108.3 . . ?
H27C C11 H27D 107.9 . . ?
C9 C11 H27A 109.9 . . ?
C9 C11 H27B 109.9 . . ?
C9A C11 H27C 109.3 . . ?
C9A C11 H27D 109.3 . . ?
H30A C5 H30B 107.8 . . ?
C3 C5 H30A 108.9 . . ?
C3 C5 H30B 108.9 . . ?
C7 C5 H30A 108.9 . . ?
C7 C5 H30B 108.9 . . ?
C7 C5 C3 113.1(3) . . ?
C21 C29 C32 111.5(3) . . ?
C31 C29 C21 111.1(3) . . ?
C31 C29 C30 107.9(3) . . ?
C31 C29 C32 108.1(3) . . ?
C30 C29 C21 109.4(3) . . ?
C30 C29 C32 108.8(3) . . ?
C40 C41 C45 122.3(3) . . ?
C40 C41 C46 119.4(3) . . ?
C45 C41 C46 118.3(3) . . ?
H39A C42 H39B 107.4 . . ?
C40 C42 H39A 108.3 . . ?
C40 C42 H39B 108.3 . . ?
C43 C42 H39A 108.3 . . ?
C43 C42 H39B 108.3 . . ?
C43 C42 C40 116.1(3) . . ?
C29 C31 H14A 109.5 . . ?
C29 C31 H14B 109.5 . . ?
C29 C31 H14C 109.5 . . ?
H14A C31 H14B 109.5 . . ?
H14A C31 H14C 109.5 . . ?
H14B C31 H14C 109.5 . . ?
O1 C40 C41 121.3(3) . . ?
O1 C40 C42 117.1(3) . . ?
C41 C40 C42 121.6(3) . . ?
N6 C12 H21A 109.9 . . ?
N6 C12 H21B 109.9 . . ?
N6 C12 C10 109.1(3) . . ?
H21A C12 H21B 108.3 . . ?
C10 C12 H21A 109.9 . . ?
C10 C12 H21B 109.9 . . ?
N5 C3 C1 107.0(3) . . ?
N5 C3 C5 119.1(3) . . ?
C1 C3 C5 133.8(3) . . ?
O43 C45 C41 111.4(3) . . ?
O42 C45 O43 121.9(3) . . ?
O42 C45 C41 126.7(3) . . ?
C16 C25 C28 111.7(3) . . ?
C16 C25 C26A 104.6(10) . . ?
C27 C25 C16 110.3(3) . . ?
C27 C25 C28 105.1(3) . . ?
C26 C25 C16 109.5(3) . . ?
C26 C25 C27 112.4(4) . . ?
C26 C25 C28 107.8(4) . . ?
C28A C25 C16 110.8(10) . . ?
C28A C25 C26A 95.9(18) . . ?
C27A C25 C16 115.2(13) . . ?
C27A C25 C28A 117.6(19) . . ?
C27A C25 C26A 110(2) . . ?
C4 C6 H24A 108.9 . . ?
C4 C6 H24B 108.9 . . ?
C4 C6 C8 113.2(3) . . ?
H24A C6 H24B 107.8 . . ?
C8 C6 H24A 108.9 . . ?
C8 C6 H24B 108.9 . . ?
C29 C30 H15A 109.5 . . ?
C29 C30 H15B 109.5 . . ?
C29 C30 H15C 109.5 . . ?
H15A C30 H15B 109.5 . . ?
H15A C30 H15C 109.5 . . ?
H15B C30 H15C 109.5 . . ?
C12 C10 H22A 109.3 . . ?
C12 C10 H22B 109.3 . . ?
H22A C10 H22B 107.9 . . ?
C8 C10 C12 111.8(3) . . ?
C8 C10 H22A 109.3 . . ?
C8 C10 H22B 109.3 . . ?
O45 C47 H38A 109.5 . . ?
O45 C47 H38B 109.5 . . ?
O45 C47 H38C 109.5 . . ?
H38A C47 H38B 109.5 . . ?
H38A C47 H38C 109.5 . . ?
H38B C47 H38C 109.5 . . ?
O41 C43 C42 112.8(3) . . ?
O40 C43 O41 125.0(4) . . ?
O40 C43 C42 122.2(4) . . ?
C29 C32 H16A 109.5 . . ?
C29 C32 H16B 109.5 . . ?
C29 C32 H16C 109.5 . . ?
H16A C32 H16B 109.5 . . ?
H16A C32 H16C 109.5 . . ?
H16B C32 H16C 109.5 . . ?
C25 C27 H18A 109.5 . . ?
C25 C27 H18B 109.5 . . ?
C25 C27 H18C 109.5 . . ?
H18A C27 H18B 109.5 . . ?
H18A C27 H18C 109.5 . . ?
H18B C27 H18C 109.5 . . ?
O45 C46 C41 114.1(3) . . ?
O44 C46 O45 120.6(4) . . ?
O44 C46 C41 125.3(3) . . ?
C11 C9 H28A 109.6 . . ?
C11 C9 H28B 109.6 . . ?
H28A C9 H28B 108.1 . . ?
C7 C9 C11 110.3(3) . . ?
C7 C9 H28A 109.6 . . ?
C7 C9 H28B 109.6 . . ?
C6 C8 H23A 109.1 . . ?
C6 C8 H23B 109.1 . . ?
C10 C8 C6 112.7(3) . . ?
C10 C8 H23A 109.1 . . ?
C10 C8 H23B 109.1 . . ?
H23A C8 H23B 107.8 . . ?
C5 C7 C9 113.6(3) . . ?
C5 C7 H29A 108.9 . . ?
C5 C7 H29B 108.9 . . ?
C9 C7 H29A 108.9 . . ?
C9 C7 H29B 108.9 . . ?
H29A C7 H29B 107.7 . . ?
C9A C7 C5 125.6(6) . . ?
O43 C48 H36A 109.5 . . ?
O43 C48 H36B 109.5 . . ?
O43 C48 H36C 109.5 . . ?
H36A C48 H36B 109.5 . . ?
H36A C48 H36C 109.5 . . ?
H36B C48 H36C 109.5 . . ?
C25 C28 H20A 109.5 . . ?
C25 C28 H20B 109.5 . . ?
C25 C28 H20C 109.5 . . ?
H20A C28 H20B 109.5 . . ?
H20A C28 H20C 109.5 . . ?
H20B C28 H20C 109.5 . . ?
C25 C26 H19A 109.5 . . ?
C25 C26 H19B 109.5 . . ?
C25 C26 H19C 109.5 . . ?
H19A C26 H19B 109.5 . . ?
H19A C26 H19C 109.5 . . ?
H19B C26 H19C 109.5 . . ?
O41 C44 H41A 109.5 . . ?
O41 C44 H41B 109.5 . . ?
O41 C44 H41C 109.5 . . ?
H41A C44 H41B 109.5 . . ?
H41A C44 H41C 109.5 . . ?
H41B C44 H41C 109.5 . . ?
N10 Ni1A C1 91.5(2) . . ?
N10 Ni1A C2 84.3(2) . . ?
N10 Ni1A Cl1A 161.5(4) . . ?
C1 Ni1A C2 137.7(3) . . ?
C1 Ni1A Cl1A 98.8(3) . . ?
Cl1A Ni1A C2 98.0(3) . . ?
C25 C28A H20D 109.5 . . ?
C25 C28A H20E 109.5 . . ?
C25 C28A H20F 109.5 . . ?
H20D C28A H20E 109.5 . . ?
H20D C28A H20F 109.5 . . ?
H20E C28A H20F 109.5 . . ?
C25 C27A H18D 109.5 . . ?
C25 C27A H18E 109.5 . . ?
C25 C27A H18F 109.5 . . ?
H18D C27A H18E 109.5 . . ?
H18D C27A H18F 109.5 . . ?
H18E C27A H18F 109.5 . . ?
C25 C26A H19D 109.5 . . ?
C25 C26A H19E 109.5 . . ?
C25 C26A H19F 109.5 . . ?
H19D C26A H19E 109.5 . . ?
H19D C26A H19F 109.5 . . ?
H19E C26A H19F 109.5 . . ?
C11 C9A H28C 108.0 . . ?
C11 C9A H28D 108.0 . . ?
C7 C9A C11 117.1(10) . . ?
C7 C9A H28C 108.0 . . ?
C7 C9A H28D 108.0 . . ?
H28C C9A H28D 107.3 . . ?
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 1.913(2) . ?
Ni1 N10 1.866(2) . ?
Ni1 C1 1.951(3) . ?
Ni1 C2 1.938(3) . ?
O1 C40 1.288(4) . ?
N10 C24 1.377(4) . ?
N10 C13 1.382(4) . ?
N10 Ni1A 1.848(5) . ?
N1 N3 1.342(4) . ?
N1 C14 1.417(4) . ?
N1 C1 1.381(4) . ?
O43 C45 1.337(4) . ?
O43 C48 1.452(4) . ?
N2 N4 1.339(4) . ?
N2 C23 1.423(4) . ?
N2 C2 1.373(4) . ?
N5 N3 1.318(4) . ?
N5 C11 1.476(4) . ?
N5 C3 1.356(4) . ?
O42 C45 1.210(4) . ?
O45 C47 1.455(5) . ?
O45 C46 1.320(4) . ?
N4 N6 1.319(3) . ?
O41 C43 1.327(5) . ?
O41 C44 1.433(5) . ?
N6 C4 1.348(4) . ?
N6 C12 1.477(4) . ?
O44 C46 1.203(5) . ?
C14 C13 1.383(4) . ?
C14 C15 1.398(4) . ?
C24 C23 1.390(4) . ?
C24 C19 1.423(4) . ?
C1 C3 1.408(4) . ?
C1 Ni1A 1.947(5) . ?
C20 H5 0.9500 . ?
C20 C19 1.395(4) . ?
C20 C21 1.393(4) . ?
C13 C18 1.419(4) . ?
C23 C22 1.391(4) . ?
O40 C43 1.197(5) . ?
C19 C18 1.446(4) . ?
C2 C4 1.395(4) . ?
C2 Ni1A 2.206(5) . ?
C17 H8 0.9500 . ?
C17 C18 1.396(4) . ?
C17 C16 1.402(5) . ?
C4 C6 1.493(4) . ?
C22 H3 0.9500 . ?
C22 C21 1.408(4) . ?
C15 H10 0.9500 . ?
C15 C16 1.394(4) . ?
C16 C25 1.538(4) . ?
C21 C29 1.538(4) . ?
C11 H27A 0.9900 . ?
C11 H27B 0.9900 . ?
C11 H27C 0.9900 . ?
C11 H27D 0.9900 . ?
C11 C9 1.523(5) . ?
C11 C9A 1.493(12) . ?
C5 H30A 0.9900 . ?
C5 H30B 0.9900 . ?
C5 C3 1.493(4) . ?
C5 C7 1.487(5) . ?
C29 C31 1.527(5) . ?
C29 C30 1.538(5) . ?
C29 C32 1.539(5) . ?
C41 C40 1.395(5) . ?
C41 C45 1.461(5) . ?
C41 C46 1.494(5) . ?
C42 H39A 0.9900 . ?
C42 H39B 0.9900 . ?
C42 C40 1.517(5) . ?
C42 C43 1.507(5) . ?
C31 H14A 0.9800 . ?
C31 H14B 0.9800 . ?
C31 H14C 0.9800 . ?
C12 H21A 0.9900 . ?
C12 H21B 0.9900 . ?
C12 C10 1.504(5) . ?
C25 C27 1.524(5) . ?
C25 C28 1.565(5) . ?
C25 C26 1.491(5) . ?
C25 C28A 1.526(14) . ?
C25 C27A 1.504(15) . ?
C25 C26A 1.574(15) . ?
C6 H24A 0.9900 . ?
C6 H24B 0.9900 . ?
C6 C8 1.528(5) . ?
C30 H15A 0.9800 . ?
C30 H15B 0.9800 . ?
C30 H15C 0.9800 . ?
C10 H22A 0.9900 . ?
C10 H22B 0.9900 . ?
C10 C8 1.502(5) . ?
C47 H38A 0.9800 . ?
C47 H38B 0.9800 . ?
C47 H38C 0.9800 . ?
C32 H16A 0.9800 . ?
C32 H16B 0.9800 . ?
C32 H16C 0.9800 . ?
C27 H18A 0.9800 . ?
C27 H18B 0.9800 . ?
C27 H18C 0.9800 . ?
C9 H28A 0.9900 . ?
C9 H28B 0.9900 . ?
C9 C7 1.512(5) . ?
C8 H23A 0.9900 . ?
C8 H23B 0.9900 . ?
C7 H29A 0.9900 . ?
C7 H29B 0.9900 . ?
C7 C9A 1.426(12) . ?
C48 H36A 0.9800 . ?
C48 H36B 0.9800 . ?
C48 H36C 0.9800 . ?
C28 H20A 0.9800 . ?
C28 H20B 0.9800 . ?
C28 H20C 0.9800 . ?
C26 H19A 0.9800 . ?
C26 H19B 0.9800 . ?
C26 H19C 0.9800 . ?
C44 H41A 0.9800 . ?
C44 H41B 0.9800 . ?
C44 H41C 0.9800 . ?
Ni1A Cl1A 2.171(8) . ?
C28A H20D 0.9800 . ?
C28A H20E 0.9800 . ?
C28A H20F 0.9800 . ?
C27A H18D 0.9800 . ?
C27A H18E 0.9800 . ?
C27A H18F 0.9800 . ?
C26A H19D 0.9800 . ?
C26A H19E 0.9800 . ?
C26A H19F 0.9800 . ?
C9A H28C 0.9900 . ?
C9A H28D 0.9900 . ?
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 O1 C40 C41 174.0(2) . . . . ?
Ni1 O1 C40 C42 -7.8(4) . . . . ?
Ni1 N10 C24 C23 11.8(5) . . . . ?
Ni1 N10 C24 C19 -166.8(2) . . . . ?
Ni1 N10 C13 C14 -12.5(5) . . . . ?
Ni1 N10 C13 C18 167.9(2) . . . . ?
Ni1 C1 C3 N5 176.4(3) . . . . ?
Ni1 C1 C3 C5 -0.4(7) . . . . ?
Ni1 C2 C4 N6 179.4(3) . . . . ?
Ni1 C2 C4 C6 -4.2(6) . . . . ?
N10 C24 C23 N2 1.1(5) . . . . ?
N10 C24 C23 C22 -176.2(3) . . . . ?
N10 C24 C19 C20 176.3(3) . . . . ?
N10 C24 C19 C18 -1.1(3) . . . . ?
N10 C13 C18 C19 -1.9(3) . . . . ?
N10 C13 C18 C17 178.2(3) . . . . ?
N1 C14 C13 N10 2.4(5) . . . . ?
N1 C14 C13 C18 -178.0(3) . . . . ?
N1 C14 C15 C16 179.6(3) . . . . ?
N1 C1 C3 N5 -2.3(4) . . . . ?
N1 C1 C3 C5 -179.1(4) . . . . ?
N2 N4 N6 C4 0.0(3) . . . . ?
N2 N4 N6 C12 179.9(3) . . . . ?
N2 C23 C22 C21 -177.4(3) . . . . ?
N2 C2 C4 N6 1.6(4) . . . . ?
N2 C2 C4 C6 178.0(4) . . . . ?
N5 C11 C9 C7 -45.9(4) . . . . ?
N5 C11 C9A C7 25.5(18) . . . . ?
N4 N2 C23 C24 174.3(3) . . . . ?
N4 N2 C23 C22 -8.3(4) . . . . ?
N4 N2 C2 Ni1 -179.7(2) . . . . ?
N4 N2 C2 C4 -1.8(4) . . . . ?
N4 N2 C2 Ni1A -152.2(3) . . . . ?
N4 N6 C4 C2 -1.1(4) . . . . ?
N4 N6 C4 C6 -178.0(3) . . . . ?
N4 N6 C12 C10 159.2(3) . . . . ?
N6 C4 C6 C8 -10.5(5) . . . . ?
N6 C12 C10 C8 48.0(4) . . . . ?
N3 N1 C14 C13 -178.7(3) . . . . ?
N3 N1 C14 C15 1.4(4) . . . . ?
N3 N1 C1 Ni1 -176.4(2) . . . . ?
N3 N1 C1 C3 2.3(4) . . . . ?
N3 N1 C1 Ni1A 152.8(3) . . . . ?
N3 N5 C11 C9 -160.4(3) . . . . ?
N3 N5 C11 C9A 162.5(9) . . . . ?
N3 N5 C3 C1 1.8(4) . . . . ?
N3 N5 C3 C5 179.1(3) . . . . ?
C14 N1 N3 N5 180.0(3) . . . . ?
C14 N1 C1 Ni1 2.1(5) . . . . ?
C14 N1 C1 C3 -179.1(3) . . . . ?
C14 N1 C1 Ni1A -28.6(5) . . . . ?
C14 C13 C18 C19 178.4(3) . . . . ?
C14 C13 C18 C17 -1.4(4) . . . . ?
C14 C15 C16 C17 -1.8(5) . . . . ?
C14 C15 C16 C25 -179.9(3) . . . . ?
C24 N10 C13 C14 -179.1(3) . . . . ?
C24 N10 C13 C18 1.3(3) . . . . ?
C24 N10 Ni1A C1 170.9(3) . . . . ?
C24 N10 Ni1A C2 33.1(3) . . . . ?
C24 N10 Ni1A Cl1A -65.1(11) . . . . ?
C24 C23 C22 C21 -0.2(5) . . . . ?
C24 C19 C18 C13 1.7(3) . . . . ?
C24 C19 C18 C17 -178.5(3) . . . . ?
C1 Ni1 N10 C24 176.5(3) . . . . ?
C1 Ni1 N10 C13 12.7(3) . . . . ?
C1 N1 N3 N5 -1.4(4) . . . . ?
C1 N1 C14 C13 2.7(5) . . . . ?
C1 N1 C14 C15 -177.1(3) . . . . ?
C20 C19 C18 C13 -175.1(3) . . . . ?
C20 C19 C18 C17 4.7(6) . . . . ?
C20 C21 C29 C31 137.7(3) . . . . ?
C20 C21 C29 C30 -103.3(4) . . . . ?
C20 C21 C29 C32 17.1(5) . . . . ?
C13 N10 C24 C23 178.5(3) . . . . ?
C13 N10 C24 C19 -0.1(3) . . . . ?
C13 N10 Ni1A C1 -34.7(3) . . . . ?
C13 N10 Ni1A C2 -172.5(2) . . . . ?
C13 N10 Ni1A Cl1A 89.4(10) . . . . ?
C13 C14 C15 C16 -0.3(5) . . . . ?
C23 N2 N4 N6 178.5(2) . . . . ?
C23 N2 C2 Ni1 3.3(5) . . . . ?
C23 N2 C2 C4 -178.8(3) . . . . ?
C23 N2 C2 Ni1A 30.8(4) . . . . ?
C23 C24 C19 C20 -2.5(4) . . . . ?
C23 C24 C19 C18 -179.9(3) . . . . ?
C23 C22 C21 C20 -1.8(5) . . . . ?
C23 C22 C21 C29 177.9(3) . . . . ?
C19 C24 C23 N2 179.7(3) . . . . ?
C19 C24 C23 C22 2.3(4) . . . . ?
C19 C20 C21 C22 1.6(5) . . . . ?
C19 C20 C21 C29 -178.2(3) . . . . ?
C2 Ni1 N10 C24 -13.0(3) . . . . ?
C2 Ni1 N10 C13 -176.8(3) . . . . ?
C2 N2 N4 N6 1.2(4) . . . . ?
C2 N2 C23 C24 -8.7(5) . . . . ?
C2 N2 C23 C22 168.6(3) . . . . ?
C2 C4 C6 C8 173.4(4) . . . . ?
C17 C16 C25 C27 50.3(4) . . . . ?
C17 C16 C25 C28 166.8(3) . . . . ?
C17 C16 C25 C26 -73.9(4) . . . . ?
C17 C16 C25 C28A -138.4(15) . . . . ?
C17 C16 C25 C27A 84.9(17) . . . . ?
C17 C16 C25 C26A -36.1(15) . . . . ?
C4 N6 C12 C10 -20.8(5) . . . . ?
C4 C6 C8 C10 38.7(5) . . . . ?
C18 C17 C16 C15 2.2(5) . . . . ?
C18 C17 C16 C25 -179.6(3) . . . . ?
C22 C21 C29 C31 -42.1(4) . . . . ?
C22 C21 C29 C30 76.9(4) . . . . ?
C22 C21 C29 C32 -162.7(3) . . . . ?
C15 C14 C13 N10 -177.7(3) . . . . ?
C15 C14 C13 C18 1.8(5) . . . . ?
C15 C16 C25 C27 -131.6(4) . . . . ?
C15 C16 C25 C28 -15.1(5) . . . . ?
C15 C16 C25 C26 104.2(4) . . . . ?
C15 C16 C25 C28A 39.7(15) . . . . ?
C15 C16 C25 C27A -96.9(17) . . . . ?
C15 C16 C25 C26A 142.0(14) . . . . ?
C16 C17 C18 C13 -0.6(5) . . . . ?
C16 C17 C18 C19 179.6(3) . . . . ?
C21 C20 C19 C24 0.6(5) . . . . ?
C21 C20 C19 C18 177.0(3) . . . . ?
C11 N5 N3 N1 177.4(3) . . . . ?
C11 N5 C3 C1 -175.7(3) . . . . ?
C11 N5 C3 C5 1.7(6) . . . . ?
C11 C9 C7 C5 61.4(5) . . . . ?
C5 C7 C9A C11 -16(2) . . . . ?
C40 C41 C45 O43 -173.9(3) . . . . ?
C40 C41 C45 O42 4.9(6) . . . . ?
C40 C41 C46 O45 -117.7(4) . . . . ?
C40 C41 C46 O44 61.1(5) . . . . ?
C40 C42 C43 O41 -8.2(5) . . . . ?
C40 C42 C43 O40 174.4(4) . . . . ?
C12 N6 C4 C2 179.0(3) . . . . ?
C12 N6 C4 C6 2.0(5) . . . . ?
C12 C10 C8 C6 -59.5(4) . . . . ?
C3 N5 N3 N1 -0.3(4) . . . . ?
C3 N5 C11 C9 17.0(5) . . . . ?
C3 N5 C11 C9A -20.1(10) . . . . ?
C3 C5 C7 C9 -41.7(5) . . . . ?
C3 C5 C7 C9A -2.8(13) . . . . ?
C45 C41 C40 O1 -174.8(3) . . . . ?
C45 C41 C40 C42 7.0(5) . . . . ?
C45 C41 C46 O45 63.2(4) . . . . ?
C45 C41 C46 O44 -118.0(4) . . . . ?
C47 O45 C46 O44 2.8(5) . . . . ?
C47 O45 C46 C41 -178.4(3) . . . . ?
C43 C42 C40 O1 99.4(4) . . . . ?
C43 C42 C40 C41 -82.3(4) . . . . ?
C46 C41 C40 O1 6.2(5) . . . . ?
C46 C41 C40 C42 -172.0(3) . . . . ?
C46 C41 C45 O43 5.1(4) . . . . ?
C46 C41 C45 O42 -176.1(4) . . . . ?
C7 C5 C3 N5 10.3(5) . . . . ?
C7 C5 C3 C1 -173.2(4) . . . . ?
C48 O43 C45 O42 3.4(5) . . . . ?
C48 O43 C45 C41 -177.7(3) . . . . ?
C44 O41 C43 O40 -0.3(6) . . . . ?
C44 O41 C43 C42 -177.6(4) . . . . ?
Ni1A N10 C24 C23 -23.7(5) . . . . ?
Ni1A N10 C24 C19 157.7(3) . . . . ?
Ni1A N10 C13 C14 20.9(5) . . . . ?
Ni1A N10 C13 C18 -158.7(3) . . . . ?
Ni1A C1 C3 N5 -148.2(3) . . . . ?
Ni1A C1 C3 C5 35.0(7) . . . . ?
Ni1A C2 C4 N6 147.9(3) . . . . ?
Ni1A C2 C4 C6 -35.6(6) . . . . ?
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
0.0000 1.0000 -2.0000 -0.1251 -0.0312 -0.1202
-0.0000 -1.0000 2.0000 0.1251 0.0312 0.1202
0.0000 1.0000 1.0000 0.0776 0.0030 -0.1039
-0.0000 -1.0000 -1.0000 -0.0776 -0.0030 0.1039
-1.0000 0.0001 0.9999 0.0319 0.1321 -0.0074
1.0000 -0.0001 -0.9999 -0.0319 -0.1321 0.0074
0.0000 1.0000 2.0000 0.1452 0.0144 -0.0985
