#------------------------------------------------------------------------------
#$Date: 2022-05-17 00:55:14 +0300 (Tue, 17 May 2022) $
#$Revision: 275455 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/00/7130095.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_7130095
loop_
_publ_author_name
'Li, Sha'
'Sun, Yahan'
'Li, Xiaofang'
'Smaga, Oskar'
'Koniarz, Sebastian'
'Stępień, Marcin'
'Chmielewski, Piotr J.'
_publ_section_title
;
 1,3-Dipolar cycloaddition of polycyclic azomethine ylide to norcorroles:
 towards dibenzoullazine-fused derivatives
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02071H
_journal_year                    2022
_chemical_formula_moiety         'C84 H71 N7 Ni O2, C6 H14'
_chemical_formula_sum            'C90 H85 N7 Ni O2'
_chemical_formula_weight         1355.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-20 deposited with the CCDC.	2022-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                109.234(2)
_cell_angle_beta                 102.943(2)
_cell_angle_gamma                103.838(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3458(2)
_cell_length_b                   12.9810(2)
_cell_length_c                   16.1260(3)
_cell_measurement_reflns_used    19648
_cell_measurement_temperature    169.99(16)
_cell_measurement_theta_max      75.0430
_cell_measurement_theta_min      3.8010
_cell_volume                     2236.35(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00 -57.00   0.50    0.05    --  -46.95 132.00 -68.00   50
  2  ω   -118.00 -93.00   0.50    0.05    --  -46.95-132.00-138.00   50
  3  ω   -105.00 -80.00   0.50    0.05    --  -46.95-138.00  45.00   50
  4  ω    -85.00 -60.00   0.50    0.05    --  -46.95 138.00 107.00   50
  5  ω     72.00  97.00   0.50    0.05    --   46.95 138.00 107.00   50
  6  ω     49.00  99.00   0.50    0.05    --   46.95-138.00  45.00  100
  7  ω     24.00  95.00   0.50    0.05    --   46.95-132.00-138.00  142
  8  ω   -116.00 -28.00   0.50    0.10    --  -99.00 132.00 -68.00  176
  9  ω    -83.00 -29.00   0.50    0.10    --  -99.00 138.00 107.00  108
 10  ω   -121.00 -88.00   0.50    0.10    --  -99.00 138.00 107.00   66
 11  ω   -141.00-116.00   0.50    0.10    --  -99.00-138.00  45.00   50
 12  ω    116.00 144.00   0.50    0.10    --  103.25 138.00 107.00   56
 13  ω     96.00 121.00   0.50    0.10    --  103.25-138.00  45.00   50
 14  ω     50.00  75.00   0.50    0.10    --  103.25-132.00-138.00   50
 15  ω     81.00 123.00   0.50    0.10    --  103.25 132.00 -68.00   84
 16  ω   -110.00 -74.00   0.50    0.05    --  -46.95-125.00  60.00   72
 17  ω    -19.00  25.00   0.50    0.05    --  -46.95  19.00-180.00   88
 18  ω    -22.00  28.00   0.50    0.05    --  -46.95  19.00 -60.00  100
 19  ω    -11.00  27.00   0.50    0.05    --   46.95 -19.00   0.00   76
 20  ω    -26.00  18.00   0.50    0.05    --   46.95 -19.00 -30.00   88
 21  ω     25.00 119.00   0.50    0.05    --   46.95  77.00 -60.00  188
 22  ω   -110.00 -29.00   0.50    0.10    --  -99.00 125.00 -90.00  162
 23  ω    -54.00 -27.00   0.50    0.10    --  -99.00 125.00-180.00   54
 24  ω   -168.00 -85.00   0.50    0.10    --  -99.00 -15.00 -90.00  166
 25  ω   -161.00-111.00   0.50    0.10    --  -99.00 -94.00 -30.00  100
 26  ω    -79.00 -27.00   0.50    0.10    --  -99.00  77.00  60.00  104
 27  ω   -167.00 -93.00   0.50    0.10    --  -99.00 -69.00-145.04  148
 28  ω   -126.00-100.00   0.50    0.10    --  -99.00 147.00  42.84   52
 29  ω   -126.00 -63.00   0.50    0.10    --  -99.00 144.00 128.90  126
 30  ω   -143.00-118.00   0.50    0.10    --  -99.00-132.00-138.00   50
 31  ω   -168.00 -99.00   0.50    0.10    --  -99.00 -30.00  90.00  138
 32  ω   -111.00 -43.00   0.50    0.10    --  -99.00 125.00 -30.00  136
 33  ω   -164.00 -85.00   0.50    0.10    --  -99.00 -94.00-180.00  158
 34  ω    -56.00 -28.00   0.50    0.10    --  -99.00 147.00  42.84   56
 35  ω    -68.00 -40.00   0.50    0.10    --  -99.00  61.00 150.00   56
 36  ω   -112.00 -59.00   0.50    0.10    --  -99.00 125.00-180.00  106
 37  ω     33.00  59.00   0.50    0.10    --  103.25-125.00  90.00   52
 38  ω     50.00  76.00   0.50    0.10    --  103.25-125.00 120.00   52
 39  ω     34.00  73.00   0.50    0.10    --  103.25 -94.00  60.00   78
 40  ω     31.00  75.00   0.50    0.10    --  103.25 -61.00-180.00   88
 41  ω     36.00  75.00   0.50    0.10    --  103.25 -61.00-120.00   78
 42  ω     34.00 109.00   0.50    0.10    --  103.25 -77.00  60.00  150
 43  ω     77.00 110.00   0.50    0.10    --  103.25-125.00 120.00   66
 44  ω     71.00  97.00   0.50    0.10    --  103.25 -94.00-120.00   52
 45  ω     35.00  87.00   0.50    0.10    --  103.25 -77.00-120.00  104
 46  ω     32.00  70.00   0.50    0.10    --  103.25 -61.00  90.00   76
 47  ω     35.00  74.00   0.50    0.10    --  103.25 -61.00 120.00   78
 48  ω     66.00 100.00   0.50    0.10    --  103.25-125.00  90.00   68
 49  ω     82.00 169.00   0.50    0.10    --  103.25  77.00   0.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0261995000
_diffrn_orient_matrix_UB_12      -0.0975409000
_diffrn_orient_matrix_UB_13      0.0261943000
_diffrn_orient_matrix_UB_21      0.0428431000
_diffrn_orient_matrix_UB_22      0.0813970000
_diffrn_orient_matrix_UB_23      0.1039150000
_diffrn_orient_matrix_UB_31      -0.1265538000
_diffrn_orient_matrix_UB_32      -0.0415441000
_diffrn_orient_matrix_UB_33      0.0025139000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33345
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.441
_diffrn_reflns_theta_min         3.824
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_description       rod
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0666
_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)+(0.1233P)²+0.7657P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1933
_refine_ls_wR_factor_ref         0.1966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8055
_reflns_number_total             8863
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc02071h3.cif
_cod_data_source_block           tx2499_sq
_cod_original_cell_volume        2236.35(7)
_cod_database_code               7130095
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNO
_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 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Others
 Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32A)=Sof(H32D)=Sof(H32E)=
 Sof(H32F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Fixed Sof: O1(0.5) O2(0.5) N3(0.5) H2(0.5)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C27(H27)
3.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25), C36(H36), C38(H38)
3.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F), C30A(H30D,H30E,H30F)
;
_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 1.539
_oxdiff_exptl_absorpt_empirical_full_min 0.678
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.500000 1.000000 0.500000 0.03988(16) Uani 1 2 d S T P . .
O1 O 0.0682(3) 0.9448(3) 0.2404(3) 0.0609(9) Uani 0.5 1 d . . . A 1
O2 O 0.0945(3) 0.8186(3) 0.1278(2) 0.0637(9) Uani 0.5 1 d . . . A 1
N1 N 0.39825(15) 0.95798(14) 0.38723(11) 0.0394(4) Uani 1 1 d . . . . .
N2 N 0.53206(14) 0.86900(14) 0.44976(11) 0.0383(4) Uani 1 1 d . . . . .
N3 N 0.1290(3) 0.8918(3) 0.2089(2) 0.0432(8) Uani 0.5 1 d . . . A 1
N4 N 0.46703(13) 0.51246(12) 0.33437(11) 0.0336(3) Uani 1 1 d . . . . .
C1 C 0.31688(15) 1.00035(15) 0.35800(12) 0.0330(4) Uani 1 1 d . . . . .
C2 C 0.24722(17) 0.91659(18) 0.26576(14) 0.0413(4) Uani 1 1 d . . . . .
H2 H 0.182886 0.922077 0.226725 0.050 Uiso 0.5 1 calc R . . A 2
C3 C 0.29142(17) 0.82556(17) 0.24397(13) 0.0387(4) Uani 1 1 d . . . . .
H3 H 0.263135 0.760230 0.188210 0.046 Uiso 1 1 calc R . . . .
C4 C 0.38657(17) 0.85154(15) 0.32222(13) 0.0359(4) Uani 1 1 d . . . . .
C5 C 0.46797(16) 0.80438(15) 0.36131(12) 0.0347(4) Uani 1 1 d . . . . .
C6 C 0.49528(15) 0.69521(15) 0.32880(12) 0.0322(4) Uani 1 1 d . . . . .
H6 H 0.517349 0.683656 0.272548 0.039 Uiso 1 1 calc R . . . .
C7 C 0.60035(15) 0.71120(15) 0.41288(12) 0.0322(4) Uani 1 1 d . . . . .
H7 H 0.672912 0.720361 0.396602 0.039 Uiso 1 1 calc R . . . .
C8 C 0.61185(16) 0.82548(15) 0.49050(13) 0.0335(4) Uani 1 1 d . . . . .
C9 C 0.39748(16) 0.58454(15) 0.31698(13) 0.0340(4) Uani 1 1 d . . . . .
H9 H 0.363609 0.606159 0.366925 0.041 Uiso 1 1 calc R . . . .
C10 C 0.29815(16) 0.52167(16) 0.22567(14) 0.0369(4) Uani 1 1 d . . . . .
C11 C 0.19132(17) 0.54126(18) 0.21456(15) 0.0435(4) Uani 1 1 d . . . . .
H11 H 0.180355 0.594797 0.263982 0.052 Uiso 1 1 calc R . . . .
C12 C 0.10034(18) 0.4808(2) 0.12936(17) 0.0512(5) Uani 1 1 d . . . . .
H12 H 0.029236 0.495098 0.121270 0.061 Uiso 1 1 calc R . . . .
C13 C 0.11637(19) 0.3994(2) 0.05700(17) 0.0521(5) Uani 1 1 d . . . . .
H13 H 0.055197 0.357932 0.000476 0.063 Uiso 1 1 calc R . . . .
C14 C 0.22250(18) 0.37910(19) 0.06785(15) 0.0457(5) Uani 1 1 d . . . . .
H14 H 0.231738 0.323227 0.018897 0.055 Uiso 1 1 calc R . . . .
C15 C 0.31624(17) 0.44197(16) 0.15197(14) 0.0379(4) Uani 1 1 d . . . . .
C16 C 0.43348(16) 0.42855(15) 0.16738(13) 0.0360(4) Uani 1 1 d . . . . .
C17 C 0.47319(18) 0.38153(17) 0.09392(14) 0.0400(4) Uani 1 1 d . . . . .
H17 H 0.423787 0.357524 0.033346 0.048 Uiso 1 1 calc R . . . .
C18 C 0.58396(19) 0.36910(18) 0.10773(15) 0.0421(4) Uani 1 1 d . . . . .
C19 C 0.65379(18) 0.40345(18) 0.19884(14) 0.0411(4) Uani 1 1 d . . . . .
H19 H 0.727602 0.394718 0.209742 0.049 Uiso 1 1 calc R . . . .
C20 C 0.61833(17) 0.45070(16) 0.27524(14) 0.0368(4) Uani 1 1 d . . . . .
C21 C 0.68895(17) 0.47838(16) 0.37133(14) 0.0380(4) Uani 1 1 d . . . . .
C22 C 0.7817(2) 0.4370(2) 0.39215(16) 0.0484(5) Uani 1 1 d . . . . .
H22 H 0.805683 0.396819 0.344407 0.058 Uiso 1 1 calc R . . . .
C23 C 0.8381(2) 0.4549(2) 0.48231(18) 0.0525(5) Uani 1 1 d . . . . .
H23 H 0.901917 0.429784 0.495442 0.063 Uiso 1 1 calc R . . . .
C24 C 0.7996(2) 0.51027(19) 0.55332(16) 0.0474(5) Uani 1 1 d . . . . .
H24 H 0.834865 0.518979 0.613716 0.057 Uiso 1 1 calc R . . . .
C25 C 0.70848(19) 0.55259(16) 0.53415(14) 0.0414(4) Uani 1 1 d . . . . .
H25 H 0.682459 0.589426 0.581825 0.050 Uiso 1 1 calc R . . . .
C26 C 0.65571(17) 0.54056(15) 0.44451(14) 0.0362(4) Uani 1 1 d . . . . .
C27 C 0.56097(16) 0.59186(15) 0.42384(13) 0.0342(4) Uani 1 1 d . . . . .
H27 H 0.525669 0.602878 0.473423 0.041 Uiso 1 1 calc R . . . .
C28 C 0.50757(16) 0.46554(15) 0.25942(13) 0.0336(4) Uani 1 1 d . . . . .
C29 C 0.6254(2) 0.3171(2) 0.02520(16) 0.0498(5) Uani 1 1 d . . . . .
C30 C 0.6043(11) 0.3783(10) -0.0392(8) 0.073(3) Uani 0.494(14) 1 d . . . B 1
H30A H 0.525314 0.380548 -0.051138 0.109 Uiso 0.494(14) 1 calc GR . . B 1
H30B H 0.614423 0.337108 -0.096842 0.109 Uiso 0.494(14) 1 calc GR . . B 1
H30C H 0.659792 0.456062 -0.010480 0.109 Uiso 0.494(14) 1 calc GR . . B 1
C31 C 0.5452(11) 0.1861(6) -0.0294(7) 0.078(3) Uani 0.494(14) 1 d . . . B 1
H31A H 0.558516 0.144971 0.009480 0.117 Uiso 0.494(14) 1 calc GR . . B 1
H31B H 0.564466 0.152908 -0.084414 0.117 Uiso 0.494(14) 1 calc GR . . B 1
H31C H 0.463698 0.180464 -0.046556 0.117 Uiso 0.494(14) 1 calc GR . . B 1
C32 C 0.7478(8) 0.3179(12) 0.0519(5) 0.078(3) Uani 0.494(14) 1 d . . . B 1
H32A H 0.800508 0.396269 0.088510 0.118 Uiso 0.494(14) 1 calc GR . . B 1
H32B H 0.767577 0.285859 -0.003049 0.118 Uiso 0.494(14) 1 calc GR . . B 1
H32C H 0.755142 0.272278 0.087773 0.118 Uiso 0.494(14) 1 calc GR . . B 1
C33 C 0.68466(15) 0.88494(15) 0.58142(12) 0.0326(4) Uani 1 1 d . . . . .
C34 C 0.77038(15) 0.84081(15) 0.62723(13) 0.0336(4) Uani 1 1 d . . . . .
C35 C 0.87647(17) 0.84568(17) 0.60826(15) 0.0408(4) Uani 1 1 d . . . . .
C36 C 0.95829(19) 0.8121(2) 0.65764(18) 0.0506(5) Uani 1 1 d . . . . .
H36 H 1.027557 0.813365 0.643641 0.061 Uiso 1 1 calc R . . . .
C37 C 0.9401(2) 0.7767(2) 0.72739(17) 0.0500(5) Uani 1 1 d . . . . .
C38 C 0.8349(2) 0.77242(18) 0.74552(15) 0.0453(5) Uani 1 1 d . . . . .
H38 H 0.821112 0.748053 0.791525 0.054 Uiso 1 1 calc R . . . .
C39 C 0.74942(17) 0.80359(16) 0.69679(13) 0.0378(4) Uani 1 1 d . . . . .
C40 C 0.9060(2) 0.8921(2) 0.53875(17) 0.0509(5) Uani 1 1 d . . . . .
H40A H 0.877487 0.829589 0.478277 0.076 Uiso 1 1 calc GR . . . .
H40B H 0.990103 0.927309 0.556952 0.076 Uiso 1 1 calc GR . . . .
H40C H 0.869145 0.948930 0.536788 0.076 Uiso 1 1 calc GR . . . .
C41 C 0.63515(19) 0.79404(19) 0.71700(15) 0.0455(5) Uani 1 1 d . . . . .
H41A H 0.628895 0.869786 0.741021 0.068 Uiso 1 1 calc GR . . . .
H41B H 0.633508 0.761069 0.762152 0.068 Uiso 1 1 calc GR . . . .
H41C H 0.570091 0.745170 0.660721 0.068 Uiso 1 1 calc GR . . . .
C42 C 1.0310(3) 0.7414(3) 0.7805(2) 0.0693(7) Uani 1 1 d . . . . .
H42A H 1.035502 0.670807 0.739596 0.104 Uiso 1 1 calc GR . . . .
H42B H 1.008602 0.729483 0.830855 0.104 Uiso 1 1 calc GR . . . .
H42C H 1.106698 0.801569 0.804990 0.104 Uiso 1 1 calc GR . . . .
C43 C 0.2714(4) 1.0530(4) 0.0113(3) 0.0974(11) Uani 1 1 d . . . . .
H43A H 0.255347 1.026528 -0.054645 0.146 Uiso 1 1 calc GR . . . .
H43B H 0.335057 1.030832 0.037849 0.146 Uiso 1 1 calc GR . . . .
H43C H 0.293297 1.135982 0.038599 0.146 Uiso 1 1 calc GR . . . .
C44 C 0.1616(3) 0.9988(3) 0.0307(2) 0.0773(8) Uani 1 1 d . . . . .
H44A H 0.142341 0.915244 0.005124 0.093 Uiso 1 1 calc R . . . .
H44B H 0.179253 1.025371 0.097497 0.093 Uiso 1 1 calc R . . . .
C45 C 0.0546(3) 1.0265(3) -0.0092(2) 0.0726(8) Uani 1 1 d . . . . .
H45A H 0.074031 1.110116 0.016473 0.087 Uiso 1 1 calc R . . . .
H45B H 0.037287 1.000195 -0.075934 0.087 Uiso 1 1 calc R . . . .
C31A C 0.6250(12) 0.1986(7) 0.0165(7) 0.085(3) Uani 0.506(14) 1 d . . . B 2
H31D H 0.686179 0.205168 0.068588 0.128 Uiso 0.506(14) 1 calc GR . . B 2
H31E H 0.638875 0.160027 -0.040102 0.128 Uiso 0.506(14) 1 calc GR . . B 2
H31F H 0.549749 0.154473 0.015264 0.128 Uiso 0.506(14) 1 calc GR . . B 2
C32A C 0.7596(8) 0.3916(12) 0.0500(6) 0.100(4) Uani 0.506(14) 1 d . . . B 2
H32D H 0.765146 0.468373 0.054517 0.151 Uiso 0.506(14) 1 calc GR . . B 2
H32E H 0.789322 0.355453 0.002139 0.151 Uiso 0.506(14) 1 calc GR . . B 2
H32F H 0.805426 0.395888 0.108429 0.151 Uiso 0.506(14) 1 calc GR . . B 2
C30A C 0.5578(14) 0.3182(15) -0.0626(7) 0.098(4) Uani 0.506(14) 1 d . . . B 2
H30D H 0.480411 0.260684 -0.086943 0.146 Uiso 0.506(14) 1 calc GR . . B 2
H30E H 0.598304 0.301354 -0.107000 0.146 Uiso 0.506(14) 1 calc GR . . B 2
H30F H 0.550724 0.393417 -0.050689 0.146 Uiso 0.506(14) 1 calc GR . . B 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_
_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
N1 Ni1 N1 180.0 . 2_676 ?
N1 Ni1 N2 86.20(7) 2_676 2_676 ?
N1 Ni1 N2 93.80(7) 2_676 . ?
N1 Ni1 N2 93.80(7) . 2_676 ?
N1 Ni1 N2 86.20(7) . . ?
N2 Ni1 N2 180.0 2_676 . ?
C1 N1 Ni1 131.20(13) . . ?
C1 N1 C4 112.79(16) . . ?
C4 N1 Ni1 114.89(13) . . ?
C5 N2 Ni1 114.36(14) . . ?
C5 N2 C8 115.86(16) . . ?
C8 N2 Ni1 129.77(13) . . ?
O1 N3 O2 122.7(4) . . ?
O1 N3 C2 119.7(3) . . ?
O2 N3 C2 117.5(3) . . ?
C9 N4 C27 102.90(14) . . ?
C28 N4 C9 112.13(15) . . ?
C28 N4 C27 115.19(14) . . ?
N1 C1 C2 105.09(16) . . ?
N1 C1 C33 120.63(16) . 2_676 ?
C2 C1 C33 134.25(17) . 2_676 ?
C1 C2 N3 132.0(2) . . ?
C3 C2 N3 115.6(2) . . ?
C3 C2 C1 108.93(17) . . ?
C2 C3 C4 106.59(17) . . ?
N1 C4 C3 106.57(17) . . ?
N1 C4 C5 110.20(16) . . ?
C3 C4 C5 142.93(17) . . ?
N2 C5 C4 114.17(16) . . ?
N2 C5 C6 109.98(16) . . ?
C4 C5 C6 135.74(16) . . ?
C5 C6 C7 104.24(14) . . ?
C5 C6 C9 114.66(15) . . ?
C9 C6 C7 102.73(14) . . ?
C6 C7 C27 103.17(13) . . ?
C8 C7 C6 103.53(14) . . ?
C8 C7 C27 120.29(15) . . ?
N2 C8 C7 105.96(15) . . ?
C33 C8 N2 121.59(16) . . ?
C33 C8 C7 132.38(17) . . ?
N4 C9 C6 101.74(14) . . ?
N4 C9 C10 112.10(15) . . ?
C10 C9 C6 117.31(15) . . ?
C11 C10 C9 121.29(17) . . ?
C11 C10 C15 120.69(18) . . ?
C15 C10 C9 118.02(17) . . ?
C10 C11 C12 120.03(19) . . ?
C13 C12 C11 119.6(2) . . ?
C12 C13 C14 120.6(2) . . ?
C13 C14 C15 120.5(2) . . ?
C10 C15 C14 118.49(18) . . ?
C10 C15 C16 117.92(17) . . ?
C14 C15 C16 123.59(18) . . ?
C17 C16 C15 122.09(18) . . ?
C17 C16 C28 119.29(18) . . ?
C28 C16 C15 118.62(16) . . ?
C18 C17 C16 122.54(19) . . ?
C17 C18 C29 121.31(19) . . ?
C19 C18 C17 116.95(18) . . ?
C19 C18 C29 121.72(19) . . ?
C18 C19 C20 122.98(19) . . ?
C19 C20 C21 122.60(18) . . ?
C19 C20 C28 118.86(18) . . ?
C28 C20 C21 118.42(16) . . ?
C22 C21 C20 122.67(18) . . ?
C22 C21 C26 118.48(19) . . ?
C26 C21 C20 118.63(17) . . ?
C23 C22 C21 121.1(2) . . ?
C22 C23 C24 119.9(2) . . ?
C25 C24 C23 119.8(2) . . ?
C24 C25 C26 120.5(2) . . ?
C21 C26 C27 119.05(17) . . ?
C25 C26 C21 120.00(18) . . ?
C25 C26 C27 120.94(17) . . ?
N4 C27 C7 104.00(14) . . ?
N4 C27 C26 110.67(15) . . ?
C26 C27 C7 116.74(14) . . ?
C16 C28 N4 119.46(16) . . ?
C20 C28 N4 121.16(17) . . ?
C20 C28 C16 119.33(16) . . ?
C18 C29 C31 107.5(3) . . ?
C18 C29 C32A 108.4(3) . . ?
C30 C29 C18 108.3(4) . . ?
C30 C29 C31 107.9(5) . . ?
C32 C29 C18 114.4(3) . . ?
C32 C29 C30 112.4(6) . . ?
C32 C29 C31 106.1(5) . . ?
C31A C29 C18 108.3(3) . . ?
C31A C29 C32A 105.6(6) . . ?
C30A C29 C18 113.7(5) . . ?
C30A C29 C31A 113.2(6) . . ?
C30A C29 C32A 107.3(7) . . ?
C8 C33 C1 122.07(17) . 2_676 ?
C8 C33 C34 123.01(16) . . ?
C34 C33 C1 114.92(15) . 2_676 ?
C35 C34 C33 120.86(17) . . ?
C35 C34 C39 119.61(18) . . ?
C39 C34 C33 119.26(16) . . ?
C34 C35 C40 121.41(18) . . ?
C36 C35 C34 119.18(19) . . ?
C36 C35 C40 119.35(19) . . ?
C35 C36 C37 122.1(2) . . ?
C36 C37 C42 121.0(2) . . ?
C38 C37 C36 118.1(2) . . ?
C38 C37 C42 120.9(2) . . ?
C37 C38 C39 121.8(2) . . ?
C34 C39 C41 120.98(18) . . ?
C38 C39 C34 119.15(18) . . ?
C38 C39 C41 119.85(18) . . ?
C45 C44 C43 114.2(3) . . ?
C45 C45 C44 114.8(3) 2_575 . ?
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 N1 1.7827(17) . ?
Ni1 N1 1.7827(17) 2_676 ?
Ni1 N2 1.8062(16) 2_676 ?
Ni1 N2 1.8063(16) . ?
O1 N3 1.217(5) . ?
O2 N3 1.238(5) . ?
N1 C1 1.325(2) . ?
N1 C4 1.383(2) . ?
N2 C5 1.324(2) . ?
N2 C8 1.393(2) . ?
N3 C2 1.434(4) . ?
N4 C9 1.463(2) . ?
N4 C27 1.479(2) . ?
N4 C28 1.419(2) . ?
C1 C2 1.431(3) . ?
C1 C33 1.495(2) 2_676 ?
C2 C3 1.392(3) . ?
C3 C4 1.397(3) . ?
C4 C5 1.431(3) . ?
C5 C6 1.488(2) . ?
C6 C7 1.569(3) . ?
C6 C9 1.564(2) . ?
C7 C8 1.544(2) . ?
C7 C27 1.589(2) . ?
C8 C33 1.373(3) . ?
C9 C10 1.503(3) . ?
C10 C11 1.386(3) . ?
C10 C15 1.397(3) . ?
C11 C12 1.394(3) . ?
C12 C13 1.381(3) . ?
C13 C14 1.382(3) . ?
C14 C15 1.400(3) . ?
C15 C16 1.475(3) . ?
C16 C17 1.394(3) . ?
C16 C28 1.408(3) . ?
C17 C18 1.392(3) . ?
C18 C19 1.385(3) . ?
C18 C29 1.538(3) . ?
C19 C20 1.399(3) . ?
C20 C21 1.473(3) . ?
C20 C28 1.405(3) . ?
C21 C22 1.397(3) . ?
C21 C26 1.400(3) . ?
C22 C23 1.379(3) . ?
C23 C24 1.386(3) . ?
C24 C25 1.384(3) . ?
C25 C26 1.385(3) . ?
C26 C27 1.506(3) . ?
C29 C30 1.517(11) . ?
C29 C31 1.569(8) . ?
C29 C32 1.472(8) . ?
C29 C31A 1.497(8) . ?
C29 C32A 1.588(8) . ?
C29 C30A 1.480(11) . ?
C33 C34 1.488(3) . ?
C34 C35 1.402(3) . ?
C34 C39 1.409(3) . ?
C35 C36 1.387(3) . ?
C35 C40 1.508(3) . ?
C36 C37 1.390(4) . ?
C37 C38 1.386(3) . ?
C37 C42 1.509(3) . ?
C38 C39 1.392(3) . ?
C39 C41 1.504(3) . ?
C43 C44 1.520(5) . ?
C44 C45 1.513(5) . ?
C45 C45 1.499(7) 2_575 ?
