#------------------------------------------------------------------------------
#$Date: 2026-04-05 14:07:20 +0200 (Sun 05 de Apr de 2026) $
#$Revision: 305371 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/06/7720666.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_7720666
loop_
_publ_author_name
'Herniman, Julie M.'
'P Keeling, George'
'King, Rhys P.'
'Light, Mark E.'
'Kandathil Sintho, Navya'
'Snowsill, Kate'
'Reid, Gillian'
_publ_section_title
;
 Transition metal complexes with phosphine oxide appended aza-macrocycles
 - effects of ring size and denticity.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5266
_journal_page_last               5275
_journal_paper_doi               10.1039/d6dt00255b
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C41 H46 N4 Ni O2 P2, 2(C24 H20 B), C2 H3 N'
_chemical_formula_sum            'C91 H89 B2 N5 Ni O2 P2'
_chemical_formula_weight         1426.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-05
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-12-15 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.020(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5349(2)
_cell_length_b                   35.3829(7)
_cell_length_c                   16.3968(3)
_cell_measurement_reflns_used    37470
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.5520
_cell_measurement_theta_min      1.8130
_cell_volume                     7547.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.44.96a (Rigaku OD, 2025)'
_computing_data_collection       'CrysAlisPro 1.171.44.96a (Rigaku OD, 2025)'
_computing_data_reduction        'CrysAlisPro 1.171.44.96a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      3.00  57.00   0.50    6.28    --   17.09-113.00  78.00  108
  2  ω    -58.00  -9.00   0.50    6.28    --  -18.50 113.00 170.00   98
  3  ω    -62.00 -22.00   0.50    6.28    --   17.09 -19.00-150.00   80
  4  ω      3.00  56.00   0.50    6.28    --   17.09  57.00-150.00  106
  5  ω    -62.00 -22.00   0.50    6.28    --   17.09 -19.00   0.00   80
  6  ω      3.00  56.00   0.50    6.28    --   17.09  57.00 150.00  106
  7  ω      3.00  56.00   0.50    6.28    --   17.09  57.00 -60.00  106
  8  ω     16.00  62.00   0.50    6.28    --  -18.50  19.00-120.00   92
  9  ω    -62.00  -4.00   0.50    6.28    --  -18.50 -57.00  60.00  116
 10  ω     16.00  62.00   0.50    6.28    --  -18.50  19.00 120.00   92
 11  ω      3.00  38.00   0.50    6.28    --   17.09  57.00  30.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, SynergyCustom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0058721000
_diffrn_orient_matrix_UB_12      -0.0111891000
_diffrn_orient_matrix_UB_13      -0.0369331000
_diffrn_orient_matrix_UB_21      0.0081294000
_diffrn_orient_matrix_UB_22      0.0162234000
_diffrn_orient_matrix_UB_23      -0.0227269000
_diffrn_orient_matrix_UB_31      0.0535899000
_diffrn_orient_matrix_UB_32      -0.0036750000
_diffrn_orient_matrix_UB_33      0.0120313000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            124747
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.375
_diffrn_reflns_theta_min         2.081
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.96a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         26475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0631P)²+4.0862P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19171
_reflns_number_total             26475
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2025rk_nibnnodpph_auto
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_database_code               7720666
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni B P O C H N'
_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.
;
_diffrn_oxdiff_ac3_digest_hkl    014f8bfd6077e0b1c6c670aaa14cb2fa8154dd
_diffrn_oxdiff_digest_hkl
;
4350b568bc6cf6f5f8fb6ed1bad4b49720a770
;
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C13(H13A,H13B), C29(H29A,H29B), C14(H14A,H14B), C38(H38A,
 H38B), C16(H16A,H16B), C30(H30A,H30B), C15(H15A,H15B), C37(H37A,H37B)
1.b Aromatic/amide H refined with riding coordinates:
 C47(H47), C53(H53), C61(H61), C43(H43), C55(H55), C45(H45), C64(H64),
 C51(H51), C63(H63), C62(H62), C24(H24), C12(H12), C49(H49), C50(H50), C59(H59),
  C32(H32), C91(H91), C46(H46), C52(H52), C33(H33), C11(H11), C72(H72),
 C44(H44), C74(H74), C87(H87), C78(H78), C8(H8), C76(H76), C75(H75), C88(H88),
 C58(H58), C36(H36), C28(H28), C34(H34), C25(H25), C84(H84), C86(H86), C2(H2),
 C56(H56), C35(H35), C57(H57), C10(H10), C73(H73), C66(H66), C22(H22), C26(H26),
  C82(H82), C70(H70), C85(H85), C80(H80), C27(H27), C6(H6), C79(H79), C18(H18),
 C3(H3), C81(H81), C69(H69), C9(H9), C21(H21), C4(H4), C68(H68), C67(H67),
 C20(H20), C19(H19), C5(H5)
1.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C90(H90A,H90B,H90C)
;
_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 1.785
_oxdiff_exptl_absorpt_empirical_full_min 0.513
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.31052(2) 0.59060(2) 0.20796(2) 0.01355(5) Uani 1 1 d . . . . .
P1 P 0.23071(3) 0.61987(2) 0.35031(3) 0.01497(8) Uani 1 1 d . . . . .
P2 P 0.28061(3) 0.64671(2) 0.06300(3) 0.01518(8) Uani 1 1 d . . . . .
O2 O 0.27740(9) 0.64457(3) 0.15438(7) 0.0172(2) Uani 1 1 d . . . . .
O1 O 0.32960(9) 0.60985(3) 0.32969(7) 0.0163(2) Uani 1 1 d . . . . .
N1 N 0.15414(10) 0.58401(4) 0.20078(9) 0.0155(3) Uani 1 1 d . . . . .
N3 N 0.26706(11) 0.57164(4) 0.08172(9) 0.0162(3) Uani 1 1 d . . . . .
N4 N 0.46298(12) 0.59976(4) 0.21081(10) 0.0200(3) Uani 1 1 d . . . . .
N2 N 0.32170(10) 0.53281(4) 0.23933(9) 0.0156(3) Uani 1 1 d . . . . .
C60 C -0.18468(12) 0.52501(5) 0.11071(10) 0.0156(3) Uani 1 1 d . . . . .
C54 C -0.21594(12) 0.53190(5) 0.26268(10) 0.0165(3) Uani 1 1 d . . . . .
C42 C -0.08023(12) 0.47986(5) 0.24080(11) 0.0163(3) Uani 1 1 d . . . . .
C7 C 0.20762(13) 0.59050(5) 0.43195(10) 0.0170(3) Uani 1 1 d . . . . .
C31 C 0.43202(13) 0.48358(5) 0.33484(11) 0.0184(3) Uani 1 1 d . . . . .
C47 C -0.04588(14) 0.44962(5) 0.19963(12) 0.0204(3) Uani 1 1 d . . . . .
H47 H -0.086782 0.442280 0.145004 0.024 Uiso 1 1 calc R U . . .
C53 C -0.37851(13) 0.47681(5) 0.11101(11) 0.0189(3) Uani 1 1 d . . . . .
H53 H -0.389536 0.501057 0.085202 0.023 Uiso 1 1 calc R U . . .
C61 C -0.11173(13) 0.51914(5) 0.06547(11) 0.0180(3) Uani 1 1 d . . . . .
H61 H -0.060082 0.500545 0.085476 0.022 Uiso 1 1 calc R U . . .
C43 C -0.01601(13) 0.48845(5) 0.32143(11) 0.0183(3) Uani 1 1 d . . . . .
H43 H -0.035399 0.508489 0.352377 0.022 Uiso 1 1 calc R U . . .
C55 C -0.29429(13) 0.52753(6) 0.30208(12) 0.0223(4) Uani 1 1 d . . . . .
H55 H -0.338290 0.506194 0.287798 0.027 Uiso 1 1 calc R U . . .
C48 C -0.28283(12) 0.46918(5) 0.16922(10) 0.0164(3) Uani 1 1 d . . . . .
C45 C 0.10632(14) 0.43972(5) 0.31506(13) 0.0237(4) Uani 1 1 d . . . . .
H45 H 0.168603 0.426552 0.339622 0.028 Uiso 1 1 calc R U . . .
C64 C -0.25719(13) 0.55341(5) 0.07681(11) 0.0200(3) Uani 1 1 d . . . . .
H64 H -0.308006 0.558897 0.105130 0.024 Uiso 1 1 calc R U . . .
C51 C -0.44486(14) 0.41474(5) 0.12592(12) 0.0223(4) Uani 1 1 d . . . . .
H51 H -0.498404 0.396526 0.111022 0.027 Uiso 1 1 calc R U . . .
C63 C -0.25848(14) 0.57383(5) 0.00425(12) 0.0230(4) Uani 1 1 d . . . . .
H63 H -0.309801 0.592502 -0.016159 0.028 Uiso 1 1 calc R U . . .
C62 C -0.18472(15) 0.56701(5) -0.03866(12) 0.0235(4) Uani 1 1 d . . . . .
H62 H -0.184559 0.580985 -0.088098 0.028 Uiso 1 1 calc R U . . .
C17 C 0.38340(13) 0.67661(5) 0.05367(12) 0.0214(3) Uani 1 1 d . . . . .
C24 C 0.10394(13) 0.68808(5) 0.03065(12) 0.0213(3) Uani 1 1 d . . . . .
H24 H 0.127014 0.694439 0.089133 0.026 Uiso 1 1 calc R U . . .
C12 C 0.10886(14) 0.58066(5) 0.43511(12) 0.0220(3) Uani 1 1 d . . . . .
H12 H 0.050596 0.589896 0.393152 0.026 Uiso 1 1 calc R U . . .
C49 C -0.27379(13) 0.43296(5) 0.20553(11) 0.0197(3) Uani 1 1 d . . . . .
H49 H -0.211333 0.426442 0.246282 0.024 Uiso 1 1 calc R U . . .
C50 C -0.35226(14) 0.40604(5) 0.18458(12) 0.0219(3) Uani 1 1 d . . . . .
H50 H -0.342230 0.381799 0.210477 0.026 Uiso 1 1 calc R U . . .
C59 C -0.15586(13) 0.56479(5) 0.28600(12) 0.0207(3) Uani 1 1 d . . . . .
H59 H -0.102825 0.569659 0.259667 0.025 Uiso 1 1 calc R U . . .
C1 C 0.22546(14) 0.66804(5) 0.38050(11) 0.0197(3) Uani 1 1 d . . . . .
C39 C 0.53564(13) 0.61163(5) 0.20087(12) 0.0214(3) Uani 1 1 d . . . . .
C23 C 0.16212(13) 0.66397(5) -0.00503(11) 0.0177(3) Uani 1 1 d . . . . .
C41 C 0.42416(13) 0.52335(5) 0.29976(11) 0.0178(3) Uani 1 1 d . . . . .
H41A H 0.438186 0.541394 0.347732 0.021 Uiso 1 1 calc R U . . .
H41B H 0.478116 0.526881 0.270164 0.021 Uiso 1 1 calc R U . . .
C13 C 0.12629(12) 0.61399(5) 0.25286(11) 0.0171(3) Uani 1 1 d . . . . .
H13A H 0.062093 0.607080 0.267027 0.021 Uiso 1 1 calc R U . . .
H13B H 0.114462 0.638030 0.220729 0.021 Uiso 1 1 calc R U . . .
C29 C 0.32065(14) 0.53441(5) 0.08663(11) 0.0194(3) Uani 1 1 d . . . . .
H29A H 0.395354 0.538575 0.096448 0.023 Uiso 1 1 calc R U . . .
H29B H 0.294710 0.520727 0.032249 0.023 Uiso 1 1 calc R U . . .
C77 C -0.24936(15) 0.79787(5) 0.02648(12) 0.0226(4) Uani 1 1 d . . . . .
C32 C 0.46594(13) 0.45382(5) 0.29296(12) 0.0203(3) Uani 1 1 d . . . . .
H32 H 0.489790 0.459036 0.244798 0.024 Uiso 1 1 calc R U . . .
C91 C -0.11171(14) 0.53942(5) -0.00761(11) 0.0218(4) Uani 1 1 d . . . . .
H91 H -0.061047 0.534199 -0.036254 0.026 Uiso 1 1 calc R U . . .
C14 C 0.09891(13) 0.58942(5) 0.10984(10) 0.0171(3) Uani 1 1 d . . . . .
H14A H 0.097290 0.616639 0.095526 0.021 Uiso 1 1 calc R U . . .
H14B H 0.027120 0.580506 0.099064 0.021 Uiso 1 1 calc R U . . .
C46 C 0.04512(14) 0.42998(5) 0.23513(13) 0.0238(4) Uani 1 1 d . . . . .
H46 H 0.065193 0.409937 0.204594 0.029 Uiso 1 1 calc R U . . .
C38 C 0.13787(13) 0.54515(5) 0.23028(11) 0.0180(3) Uani 1 1 d . . . . .
H38A H 0.105672 0.529202 0.180420 0.022 Uiso 1 1 calc R U . . .
H38B H 0.089946 0.546485 0.266175 0.022 Uiso 1 1 calc R U . . .
C16 C 0.30456(13) 0.59895(5) 0.02863(11) 0.0180(3) Uani 1 1 d . . . . .
H16A H 0.267679 0.595295 -0.031991 0.022 Uiso 1 1 calc R U . . .
H16B H 0.378975 0.595231 0.035854 0.022 Uiso 1 1 calc R U . . .
C52 C -0.45816(13) 0.45030(5) 0.08942(12) 0.0215(3) Uani 1 1 d . . . . .
H52 H -0.521451 0.456715 0.049636 0.026 Uiso 1 1 calc R U . . .
C83 C -0.16187(13) 0.73856(5) 0.12509(12) 0.0218(3) Uani 1 1 d . . . . .
C30 C 0.30193(14) 0.51077(5) 0.15871(11) 0.0187(3) Uani 1 1 d . . . . .
H30A H 0.229899 0.501744 0.142424 0.022 Uiso 1 1 calc R U . . .
H30B H 0.347453 0.488353 0.168036 0.022 Uiso 1 1 calc R U . . .
C33 C 0.46513(15) 0.41679(5) 0.32103(13) 0.0243(4) Uani 1 1 d . . . . .
H33 H 0.487354 0.396821 0.291616 0.029 Uiso 1 1 calc R U . . .
C11 C 0.09568(15) 0.55737(6) 0.49957(12) 0.0240(4) Uani 1 1 d . . . . .
H11 H 0.028433 0.550577 0.501451 0.029 Uiso 1 1 calc R U . . .
C72 C -0.27230(14) 0.77929(5) 0.23714(12) 0.0228(4) Uani 1 1 d . . . . .
H72 H -0.277828 0.752933 0.225683 0.027 Uiso 1 1 calc R U . . .
C15 C 0.15240(13) 0.56749(5) 0.05406(11) 0.0185(3) Uani 1 1 d . . . . .
H15A H 0.134684 0.540384 0.055100 0.022 Uiso 1 1 calc R U . . .
H15B H 0.126275 0.576469 -0.005194 0.022 Uiso 1 1 calc R U . . .
C44 C 0.07523(13) 0.46900(5) 0.35864(12) 0.0220(4) Uani 1 1 d . . . . .
H44 H 0.115918 0.475813 0.413713 0.026 Uiso 1 1 calc R U . . .
C74 C -0.31298(15) 0.83238(7) 0.31438(13) 0.0306(4) Uani 1 1 d . . . . .
H74 H -0.344858 0.842653 0.354292 0.037 Uiso 1 1 calc R U . . .
C87 C -0.18964(16) 0.67455(6) 0.06545(15) 0.0300(4) Uani 1 1 d . . . . .
H87 H -0.216863 0.658882 0.017440 0.036 Uiso 1 1 calc R U . . .
C37 C 0.23807(12) 0.52678(5) 0.28076(11) 0.0174(3) Uani 1 1 d . . . . .
H37A H 0.258933 0.537606 0.338670 0.021 Uiso 1 1 calc R U . . .
H37B H 0.226993 0.499326 0.285836 0.021 Uiso 1 1 calc R U . . .
C71 C -0.21759(13) 0.80164(5) 0.19380(11) 0.0204(3) Uani 1 1 d . . . . .
C78 C -0.34855(15) 0.81180(6) 0.01819(13) 0.0278(4) Uani 1 1 d . . . . .
H78 H -0.370265 0.815081 0.068111 0.033 Uiso 1 1 calc R U . . .
C8 C 0.29265(14) 0.57699(6) 0.49405(12) 0.0249(4) Uani 1 1 d . . . . .
H8 H 0.360097 0.583659 0.492512 0.030 Uiso 1 1 calc R U . . .
C76 C -0.21284(14) 0.84030(5) 0.21459(12) 0.0244(4) Uani 1 1 d . . . . .
H76 H -0.176187 0.856775 0.187632 0.029 Uiso 1 1 calc R U . . .
C75 C -0.25947(15) 0.85540(6) 0.27289(13) 0.0283(4) Uani 1 1 d . . . . .
H75 H -0.254649 0.881751 0.284430 0.034 Uiso 1 1 calc R U . . .
C88 C -0.20026(14) 0.71373(5) 0.05757(13) 0.0246(4) Uani 1 1 d . . . . .
H88 H -0.235205 0.723976 0.003788 0.029 Uiso 1 1 calc R U . . .
C58 C -0.17078(14) 0.59036(6) 0.34572(13) 0.0254(4) Uani 1 1 d . . . . .
H58 H -0.127384 0.611844 0.360239 0.030 Uiso 1 1 calc R U . . .
C36 C 0.40252(14) 0.47525(6) 0.40786(12) 0.0233(4) Uani 1 1 d . . . . .
H36 H 0.382531 0.495126 0.438894 0.028 Uiso 1 1 calc R U . . .
C28 C 0.12886(14) 0.65501(5) -0.09146(12) 0.0226(4) Uani 1 1 d . . . . .
H28 H 0.169027 0.638914 -0.115980 0.027 Uiso 1 1 calc R U . . .
C65 C -0.05648(15) 0.80362(6) 0.12623(12) 0.0247(4) Uani 1 1 d . . . . .
C34 C 0.43183(15) 0.40903(6) 0.39205(13) 0.0268(4) Uani 1 1 d . . . . .
H34 H 0.429542 0.383678 0.410519 0.032 Uiso 1 1 calc R U . . .
C25 C 0.01210(15) 0.70276(6) -0.01967(14) 0.0289(4) Uani 1 1 d . . . . .
H25 H -0.027593 0.719292 0.004325 0.035 Uiso 1 1 calc R U . . .
C84 C -0.11199(15) 0.72111(6) 0.20288(13) 0.0273(4) Uani 1 1 d . . . . .
H84 H -0.084683 0.736554 0.251248 0.033 Uiso 1 1 calc R U . . .
C86 C -0.13988(16) 0.65839(6) 0.14246(16) 0.0321(5) Uani 1 1 d . . . . .
H86 H -0.132309 0.631748 0.148052 0.038 Uiso 1 1 calc R U . . .
C2 C 0.27832(17) 0.69477(6) 0.34622(14) 0.0288(4) Uani 1 1 d . . . . .
H2 H 0.318484 0.687022 0.309966 0.035 Uiso 1 1 calc R U . . .
C56 C -0.31075(15) 0.55319(6) 0.36163(13) 0.0297(4) Uani 1 1 d . . . . .
H56 H -0.365101 0.549005 0.386869 0.036 Uiso 1 1 calc R U . . .
C35 C 0.40208(15) 0.43817(6) 0.43571(12) 0.0269(4) Uani 1 1 d . . . . .
H35 H 0.381094 0.432886 0.485240 0.032 Uiso 1 1 calc R U . . .
C57 C -0.24866(15) 0.58466(6) 0.38421(13) 0.0290(4) Uani 1 1 d . . . . .
H57 H -0.259193 0.601996 0.425253 0.035 Uiso 1 1 calc R U . . .
C10 C 0.18032(16) 0.54408(6) 0.56089(13) 0.0292(4) Uani 1 1 d . . . . .
H10 H 0.171196 0.528269 0.605073 0.035 Uiso 1 1 calc R U . . .
C40 C 0.62848(14) 0.62761(6) 0.18495(14) 0.0294(4) Uani 1 1 d . . . . .
H40A H 0.650944 0.649631 0.221633 0.044 Uiso 1 1 calc R U . . .
H40B H 0.613483 0.635352 0.125389 0.044 Uiso 1 1 calc R U . . .
H40C H 0.683102 0.608536 0.197164 0.044 Uiso 1 1 calc R U . . .
C73 C -0.31893(15) 0.79398(6) 0.29628(13) 0.0285(4) Uani 1 1 d . . . . .
H73 H -0.354842 0.777664 0.324229 0.034 Uiso 1 1 calc R U . . .
C66 C 0.03707(15) 0.78499(6) 0.16166(14) 0.0294(4) Uani 1 1 d . . . . .
H66 H 0.035696 0.759273 0.177943 0.035 Uiso 1 1 calc R U . . .
C22 C 0.41402(17) 0.67912(6) -0.01990(15) 0.0331(5) Uani 1 1 d . . . . .
H22 H 0.380303 0.664803 -0.068648 0.040 Uiso 1 1 calc R U . . .
C26 C -0.02167(15) 0.69327(6) -0.10502(14) 0.0319(5) Uani 1 1 d . . . . .
H26 H -0.085270 0.702909 -0.138952 0.038 Uiso 1 1 calc R U . . .
C82 C -0.22155(18) 0.79507(6) -0.04988(13) 0.0307(4) Uani 1 1 d . . . . .
H82 H -0.154315 0.786583 -0.047829 0.037 Uiso 1 1 calc R U . . .
C70 C -0.04728(17) 0.84127(6) 0.10168(14) 0.0313(4) Uani 1 1 d . . . . .
H70 H -0.108038 0.854837 0.074591 0.038 Uiso 1 1 calc R U . . .
C85 C -0.10128(16) 0.68191(6) 0.21135(15) 0.0325(5) Uani 1 1 d . . . . .
H85 H -0.067164 0.671293 0.264940 0.039 Uiso 1 1 calc R U . . .
C80 C -0.38748(19) 0.81691(7) -0.13326(14) 0.0373(5) Uani 1 1 d . . . . .
H80 H -0.434058 0.822620 -0.186764 0.045 Uiso 1 1 calc R U . . .
C27 C 0.03692(15) 0.66977(6) -0.14113(13) 0.0290(4) Uani 1 1 d . . . . .
H27 H 0.014044 0.663811 -0.199841 0.035 Uiso 1 1 calc R U . . .
C6 C 0.16667(18) 0.67933(6) 0.43382(14) 0.0323(5) Uani 1 1 d . . . . .
H6 H 0.131686 0.661055 0.457969 0.039 Uiso 1 1 calc R U . . .
C79 C -0.41712(17) 0.82112(7) -0.05987(15) 0.0352(5) Uani 1 1 d . . . . .
H79 H -0.483832 0.830303 -0.062319 0.042 Uiso 1 1 calc R U . . .
C18 C 0.43107(16) 0.69837(6) 0.12487(15) 0.0323(5) Uani 1 1 d . . . . .
H18 H 0.408523 0.696822 0.174737 0.039 Uiso 1 1 calc R U . . .
C3 C 0.2720(2) 0.73262(6) 0.36528(16) 0.0386(5) Uani 1 1 d . . . . .
H3 H 0.308791 0.750954 0.343024 0.046 Uiso 1 1 calc R U . . .
C81 C -0.2885(2) 0.80421(6) -0.12829(14) 0.0362(5) Uani 1 1 d . . . . .
H81 H -0.266820 0.801793 -0.178419 0.043 Uiso 1 1 calc R U . . .
C69 C 0.04742(19) 0.85956(7) 0.11543(16) 0.0387(5) Uani 1 1 d . . . . .
H69 H 0.049817 0.885290 0.099550 0.046 Uiso 1 1 calc R U . . .
B1 B -0.18994(14) 0.50132(5) 0.19602(12) 0.0152(3) Uani 1 1 d . . . . .
C9 C 0.27860(16) 0.55380(7) 0.55804(14) 0.0341(5) Uani 1 1 d . . . . .
H9 H 0.336591 0.544505 0.600194 0.041 Uiso 1 1 calc R U . . .
B2 B -0.17062(16) 0.78493(6) 0.11797(13) 0.0219(4) Uani 1 1 d . . . . .
C21 C 0.49623(18) 0.70332(7) -0.02114(19) 0.0439(6) Uani 1 1 d . . . . .
H21 H 0.518955 0.705368 -0.070845 0.053 Uiso 1 1 calc R U . . .
C4 C 0.2117(2) 0.74366(6) 0.41697(17) 0.0445(6) Uani 1 1 d . . . . .
H4 H 0.206184 0.769731 0.428859 0.053 Uiso 1 1 calc R U . . .
C68 C 0.13738(18) 0.84035(8) 0.15200(16) 0.0404(6) Uani 1 1 d . . . . .
H68 H 0.201918 0.852715 0.161971 0.048 Uiso 1 1 calc R U . . .
C67 C 0.13224(17) 0.80284(7) 0.17392(16) 0.0376(5) Uani 1 1 d . . . . .
H67 H 0.193788 0.789080 0.197481 0.045 Uiso 1 1 calc R U . . .
C20 C 0.54358(17) 0.72406(7) 0.0503(2) 0.0443(6) Uani 1 1 d . . . . .
H20 H 0.599804 0.739973 0.049397 0.053 Uiso 1 1 calc R U . . .
C89 C 0.40850(18) 0.68970(8) 0.6962(2) 0.0473(6) Uani 1 1 d . . . . .
C19 C 0.51141(17) 0.72221(7) 0.12222(19) 0.0430(6) Uani 1 1 d . . . . .
H19 H 0.543965 0.737188 0.170191 0.052 Uiso 1 1 calc R U . . .
C5 C 0.1596(2) 0.71742(7) 0.45144(18) 0.0463(6) Uani 1 1 d . . . . .
H5 H 0.118891 0.725383 0.487123 0.056 Uiso 1 1 calc R U . . .
N5 N 0.4056(2) 0.69379(10) 0.7642(2) 0.0783(9) Uani 1 1 d . . . . .
C90 C 0.4111(3) 0.68338(9) 0.6101(2) 0.0626(8) Uani 1 1 d . . . . .
H90A H 0.482367 0.684392 0.607176 0.094 Uiso 1 1 calc R U . . .
H90B H 0.370704 0.702965 0.573347 0.094 Uiso 1 1 calc R U . . .
H90C H 0.381907 0.658486 0.591203 0.094 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
O2 Ni1 N1 88.97(5) . . ?
O2 Ni1 N3 84.76(5) . . ?
O2 Ni1 N2 168.43(5) . . ?
O1 Ni1 O2 93.44(5) . . ?
O1 Ni1 N1 86.89(5) . . ?
O1 Ni1 N3 171.31(5) . . ?
O1 Ni1 N4 93.93(5) . . ?
O1 Ni1 N2 95.93(5) . . ?
N1 Ni1 N2 84.79(5) . . ?
N3 Ni1 N1 84.58(5) . . ?
N3 Ni1 N2 84.96(5) . . ?
N4 Ni1 O2 87.91(5) . . ?
N4 Ni1 N1 176.81(6) . . ?
N4 Ni1 N3 94.50(6) . . ?
N4 Ni1 N2 98.17(6) . . ?
O1 P1 C7 112.32(7) . . ?
O1 P1 C1 113.11(8) . . ?
O1 P1 C13 107.24(7) . . ?
C7 P1 C13 109.58(8) . . ?
C1 P1 C7 108.62(8) . . ?
C1 P1 C13 105.72(8) . . ?
O2 P2 C17 110.49(8) . . ?
O2 P2 C23 111.64(8) . . ?
O2 P2 C16 108.26(7) . . ?
C17 P2 C23 109.24(8) . . ?
C17 P2 C16 108.10(8) . . ?
C23 P2 C16 109.04(8) . . ?
P2 O2 Ni1 113.52(7) . . ?
P1 O1 Ni1 114.41(6) . . ?
C13 N1 Ni1 107.61(10) . . ?
C13 N1 C14 110.53(13) . . ?
C13 N1 C38 112.98(13) . . ?
C14 N1 Ni1 105.21(10) . . ?
C14 N1 C38 111.44(13) . . ?
C38 N1 Ni1 108.68(10) . . ?
C29 N3 Ni1 103.21(10) . . ?
C29 N3 C15 112.11(13) . . ?
C16 N3 Ni1 108.83(10) . . ?
C16 N3 C29 111.52(13) . . ?
C16 N3 C15 112.34(13) . . ?
C15 N3 Ni1 108.33(10) . . ?
C39 N4 Ni1 163.87(15) . . ?
C41 N2 Ni1 111.64(10) . . ?
C30 N2 Ni1 107.93(10) . . ?
C30 N2 C41 112.00(13) . . ?
C37 N2 Ni1 103.80(10) . . ?
C37 N2 C41 110.30(13) . . ?
C37 N2 C30 110.87(13) . . ?
C61 C60 C64 114.35(15) . . ?
C61 C60 B1 125.04(15) . . ?
C64 C60 B1 120.61(15) . . ?
C55 C54 C59 114.91(16) . . ?
C55 C54 B1 124.39(15) . . ?
C59 C54 B1 120.68(15) . . ?
C47 C42 B1 120.76(15) . . ?
C43 C42 C47 114.57(15) . . ?
C43 C42 B1 124.63(15) . . ?
C12 C7 P1 122.64(13) . . ?
C8 C7 P1 117.80(13) . . ?
C8 C7 C12 119.55(16) . . ?
C32 C31 C41 120.70(16) . . ?
C36 C31 C41 121.09(16) . . ?
C36 C31 C32 118.18(17) . . ?
C42 C47 H47 118.4 . . ?
C46 C47 C42 123.25(17) . . ?
C46 C47 H47 118.4 . . ?
C48 C53 H53 118.5 . . ?
C52 C53 H53 118.5 . . ?
C52 C53 C48 122.95(17) . . ?
C60 C61 H61 118.5 . . ?
C91 C61 C60 122.94(17) . . ?
C91 C61 H61 118.5 . . ?
C42 C43 H43 118.4 . . ?
C44 C43 C42 123.25(17) . . ?
C44 C43 H43 118.4 . . ?
C54 C55 H55 118.6 . . ?
C54 C55 C56 122.73(18) . . ?
C56 C55 H55 118.6 . . ?
C53 C48 B1 122.39(15) . . ?
C49 C48 C53 114.77(15) . . ?
C49 C48 B1 122.78(15) . . ?
C46 C45 H45 120.5 . . ?
C46 C45 C44 119.02(17) . . ?
C44 C45 H45 120.5 . . ?
C60 C64 H64 118.2 . . ?
C63 C64 C60 123.55(17) . . ?
C63 C64 H64 118.2 . . ?
C50 C51 H51 120.4 . . ?
C52 C51 H51 120.4 . . ?
C52 C51 C50 119.11(16) . . ?
C64 C63 H63 119.9 . . ?
C64 C63 C62 120.13(17) . . ?
C62 C63 H63 119.9 . . ?
C63 C62 H62 120.8 . . ?
C91 C62 C63 118.41(17) . . ?
C91 C62 H62 120.8 . . ?
C22 C17 P2 122.71(16) . . ?
C22 C17 C18 120.85(18) . . ?
C18 C17 P2 116.42(15) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C25 C24 C23 119.73(18) . . ?
C7 C12 H12 120.0 . . ?
C11 C12 C7 120.08(17) . . ?
C11 C12 H12 120.0 . . ?
C48 C49 H49 118.4 . . ?
C50 C49 C48 123.14(16) . . ?
C50 C49 H49 118.4 . . ?
C51 C50 C49 119.94(17) . . ?
C51 C50 H50 120.0 . . ?
C49 C50 H50 120.0 . . ?
C54 C59 H59 118.5 . . ?
C58 C59 C54 122.93(17) . . ?
C58 C59 H59 118.5 . . ?
C2 C1 P1 118.21(14) . . ?
C6 C1 P1 121.46(15) . . ?
C6 C1 C2 120.27(18) . . ?
N4 C39 C40 178.0(2) . . ?
C24 C23 P2 117.39(13) . . ?
C24 C23 C28 120.14(16) . . ?
C28 C23 P2 122.44(14) . . ?
N2 C41 C31 114.40(13) . . ?
N2 C41 H41A 108.7 . . ?
N2 C41 H41B 108.7 . . ?
C31 C41 H41A 108.7 . . ?
C31 C41 H41B 108.7 . . ?
H41A C41 H41B 107.6 . . ?
P1 C13 H13A 109.8 . . ?
P1 C13 H13B 109.8 . . ?
N1 C13 P1 109.16(11) . . ?
N1 C13 H13A 109.8 . . ?
N1 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
N3 C29 H29A 109.6 . . ?
N3 C29 H29B 109.6 . . ?
N3 C29 C30 110.07(14) . . ?
H29A C29 H29B 108.2 . . ?
C30 C29 H29A 109.6 . . ?
C30 C29 H29B 109.6 . . ?
C78 C77 C82 115.03(18) . . ?
C78 C77 B2 123.23(17) . . ?
C82 C77 B2 121.74(17) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 C31 120.81(17) . . ?
C33 C32 H32 119.6 . . ?
C61 C91 H91 119.7 . . ?
C62 C91 C61 120.62(17) . . ?
C62 C91 H91 119.7 . . ?
N1 C14 H14A 109.6 . . ?
N1 C14 H14B 109.6 . . ?
N1 C14 C15 110.23(14) . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 H14A 109.6 . . ?
C15 C14 H14B 109.6 . . ?
C47 C46 H46 120.0 . . ?
C45 C46 C47 119.95(17) . . ?
C45 C46 H46 120.0 . . ?
N1 C38 H38A 109.1 . . ?
N1 C38 H38B 109.1 . . ?
N1 C38 C37 112.29(13) . . ?
H38A C38 H38B 107.9 . . ?
C37 C38 H38A 109.1 . . ?
C37 C38 H38B 109.1 . . ?
P2 C16 H16A 110.2 . . ?
P2 C16 H16B 110.2 . . ?
N3 C16 P2 107.56(11) . . ?
N3 C16 H16A 110.2 . . ?
N3 C16 H16B 110.2 . . ?
H16A C16 H16B 108.5 . . ?
C53 C52 H52 120.0 . . ?
C51 C52 C53 120.08(17) . . ?
C51 C52 H52 120.0 . . ?
C88 C83 C84 114.97(18) . . ?
C88 C83 B2 124.53(17) . . ?
C84 C83 B2 120.50(17) . . ?
N2 C30 C29 111.83(14) . . ?
N2 C30 H30A 109.3 . . ?
N2 C30 H30B 109.3 . . ?
C29 C30 H30A 109.3 . . ?
C29 C30 H30B 109.3 . . ?
H30A C30 H30B 107.9 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 119.92(18) . . ?
C34 C33 H33 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 C12 120.03(18) . . ?
C10 C11 H11 120.0 . . ?
C71 C72 H72 118.5 . . ?
C73 C72 H72 118.5 . . ?
C73 C72 C71 123.02(18) . . ?
N3 C15 C14 113.06(13) . . ?
N3 C15 H15A 109.0 . . ?
N3 C15 H15B 109.0 . . ?
C14 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C43 C44 H44 120.0 . . ?
C45 C44 C43 119.97(17) . . ?
C45 C44 H44 120.0 . . ?
C75 C74 H74 120.7 . . ?
C75 C74 C73 118.51(19) . . ?
C73 C74 H74 120.7 . . ?
C88 C87 H87 119.7 . . ?
C86 C87 H87 119.7 . . ?
C86 C87 C88 120.5(2) . . ?
N2 C37 C38 111.46(14) . . ?
N2 C37 H37A 109.3 . . ?
N2 C37 H37B 109.3 . . ?
C38 C37 H37A 109.3 . . ?
C38 C37 H37B 109.3 . . ?
H37A C37 H37B 108.0 . . ?
C72 C71 C76 114.87(17) . . ?
C72 C71 B2 123.02(16) . . ?
C76 C71 B2 121.90(17) . . ?
C77 C78 H78 118.4 . . ?
C79 C78 C77 123.2(2) . . ?
C79 C78 H78 118.4 . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.87(17) . . ?
C9 C8 H8 120.1 . . ?
C71 C76 H76 118.6 . . ?
C75 C76 C71 122.79(19) . . ?
C75 C76 H76 118.6 . . ?
C74 C75 C76 120.63(19) . . ?
C74 C75 H75 119.7 . . ?
C76 C75 H75 119.7 . . ?
C83 C88 H88 118.5 . . ?
C87 C88 C83 123.0(2) . . ?
C87 C88 H88 118.5 . . ?
C59 C58 H58 119.9 . . ?
C57 C58 C59 120.25(18) . . ?
C57 C58 H58 119.9 . . ?
C31 C36 H36 119.7 . . ?
C35 C36 C31 120.65(17) . . ?
C35 C36 H36 119.7 . . ?
C23 C28 H28 120.2 . . ?
C27 C28 C23 119.67(19) . . ?
C27 C28 H28 120.2 . . ?
C66 C65 C70 114.97(18) . . ?
C66 C65 B2 124.23(18) . . ?
C70 C65 B2 120.70(18) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 C33 119.83(18) . . ?
C35 C34 H34 120.1 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 120.01(19) . . ?
C26 C25 H25 120.0 . . ?
C83 C84 H84 118.8 . . ?
C85 C84 C83 122.4(2) . . ?
C85 C84 H84 118.8 . . ?
C87 C86 H86 120.8 . . ?
C87 C86 C85 118.47(19) . . ?
C85 C86 H86 120.8 . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.67(19) . . ?
C3 C2 H2 120.2 . . ?
C55 C56 H56 119.7 . . ?
C57 C56 C55 120.58(18) . . ?
C57 C56 H56 119.7 . . ?
C36 C35 H35 119.7 . . ?
C34 C35 C36 120.50(18) . . ?
C34 C35 H35 119.7 . . ?
C58 C57 H57 120.7 . . ?
C56 C57 C58 118.57(18) . . ?
C56 C57 H57 120.7 . . ?
C11 C10 H10 119.9 . . ?
C11 C10 C9 120.10(18) . . ?
C9 C10 H10 119.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C72 C73 H73 119.9 . . ?
C74 C73 C72 120.17(19) . . ?
C74 C73 H73 119.9 . . ?
C65 C66 H66 118.7 . . ?
C67 C66 C65 122.5(2) . . ?
C67 C66 H66 118.7 . . ?
C17 C22 H22 120.7 . . ?
C17 C22 C21 118.7(2) . . ?
C21 C22 H22 120.7 . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.43(18) . . ?
C27 C26 H26 119.8 . . ?
C77 C82 H82 118.7 . . ?
C81 C82 C77 122.7(2) . . ?
C81 C82 H82 118.7 . . ?
C65 C70 H70 118.6 . . ?
C69 C70 C65 122.8(2) . . ?
C69 C70 H70 118.6 . . ?
C84 C85 H85 119.7 . . ?
C86 C85 C84 120.7(2) . . ?
C86 C85 H85 119.7 . . ?
C79 C80 H80 120.3 . . ?
C79 C80 C81 119.4(2) . . ?
C81 C80 H80 120.3 . . ?
C28 C27 C26 120.00(19) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C1 C6 H6 120.2 . . ?
C5 C6 C1 119.6(2) . . ?
C5 C6 H6 120.2 . . ?
C78 C79 H79 120.2 . . ?
C80 C79 C78 119.7(2) . . ?
C80 C79 H79 120.2 . . ?
C17 C18 H18 120.2 . . ?
C19 C18 C17 119.6(2) . . ?
C19 C18 H18 120.2 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.7(2) . . ?
C4 C3 H3 120.2 . . ?
C82 C81 C80 120.0(2) . . ?
C82 C81 H81 120.0 . . ?
C80 C81 H81 120.0 . . ?
C70 C69 H69 119.9 . . ?
C68 C69 C70 120.2(2) . . ?
C68 C69 H69 119.9 . . ?
C60 B1 C42 111.55(13) . . ?
C60 B1 C48 109.28(13) . . ?
C54 B1 C60 107.26(13) . . ?
C54 B1 C42 109.81(13) . . ?
C54 B1 C48 109.95(13) . . ?
C42 B1 C48 108.98(13) . . ?
C8 C9 C10 120.36(19) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C77 B2 C71 107.38(15) . . ?
C77 B2 C65 108.59(15) . . ?
C83 B2 C77 110.94(15) . . ?
C83 B2 C71 109.75(15) . . ?
C83 B2 C65 110.25(15) . . ?
C65 B2 C71 109.88(15) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 C22 119.6(2) . . ?
C20 C21 H21 120.2 . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 121.0(2) . . ?
C5 C4 H4 119.5 . . ?
C69 C68 H68 120.5 . . ?
C69 C68 C67 119.0(2) . . ?
C67 C68 H68 120.5 . . ?
C66 C67 H67 119.8 . . ?
C68 C67 C66 120.4(2) . . ?
C68 C67 H67 119.8 . . ?
C21 C20 H20 119.2 . . ?
C19 C20 C21 121.5(2) . . ?
C19 C20 H20 119.2 . . ?
N5 C89 C90 178.3(3) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.7(2) . . ?
C20 C19 H19 120.1 . . ?
C6 C5 H5 120.1 . . ?
C4 C5 C6 119.8(2) . . ?
C4 C5 H5 120.1 . . ?
C89 C90 H90A 109.5 . . ?
C89 C90 H90B 109.5 . . ?
C89 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 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 O2 2.0981(12) . ?
Ni1 O1 2.0567(12) . ?
Ni1 N1 2.1002(14) . ?
Ni1 N3 2.0997(14) . ?
Ni1 N4 2.0765(16) . ?
Ni1 N2 2.1038(14) . ?
P1 O1 1.5105(12) . ?
P1 C7 1.7888(17) . ?
P1 C1 1.7818(18) . ?
P1 C13 1.8297(17) . ?
P2 O2 1.5128(13) . ?
P2 C17 1.7877(18) . ?
P2 C23 1.7893(17) . ?
P2 C16 1.8381(18) . ?
N1 C13 1.474(2) . ?
N1 C14 1.484(2) . ?
N1 C38 1.494(2) . ?
N3 C29 1.495(2) . ?
N3 C16 1.481(2) . ?
N3 C15 1.499(2) . ?
N4 C39 1.122(2) . ?
N2 C41 1.503(2) . ?
N2 C30 1.494(2) . ?
N2 C37 1.487(2) . ?
C60 C61 1.405(2) . ?
C60 C64 1.407(2) . ?
C60 B1 1.649(2) . ?
C54 C55 1.394(2) . ?
C54 C59 1.411(2) . ?
C54 B1 1.644(2) . ?
C42 C47 1.411(2) . ?
C42 C43 1.401(2) . ?
C42 B1 1.649(2) . ?
C7 C12 1.396(2) . ?
C7 C8 1.394(2) . ?
C31 C41 1.513(2) . ?
C31 C32 1.402(2) . ?
C31 C36 1.394(2) . ?
C47 H47 0.9500 . ?
C47 C46 1.394(3) . ?
C53 H53 0.9500 . ?
C53 C48 1.407(2) . ?
C53 C52 1.399(2) . ?
C61 H61 0.9500 . ?
C61 C91 1.397(2) . ?
C43 H43 0.9500 . ?
C43 C44 1.398(2) . ?
C55 H55 0.9500 . ?
C55 C56 1.396(3) . ?
C48 C49 1.404(2) . ?
C48 B1 1.662(2) . ?
C45 H45 0.9500 . ?
C45 C46 1.387(3) . ?
C45 C44 1.388(3) . ?
C64 H64 0.9500 . ?
C64 C63 1.388(3) . ?
C51 H51 0.9500 . ?
C51 C50 1.388(3) . ?
C51 C52 1.383(3) . ?
C63 H63 0.9500 . ?
C63 C62 1.392(3) . ?
C62 H62 0.9500 . ?
C62 C91 1.383(3) . ?
C17 C22 1.382(3) . ?
C17 C18 1.399(3) . ?
C24 H24 0.9500 . ?
C24 C23 1.394(3) . ?
C24 C25 1.389(3) . ?
C12 H12 0.9500 . ?
C12 C11 1.390(3) . ?
C49 H49 0.9500 . ?
C49 C50 1.397(2) . ?
C50 H50 0.9500 . ?
C59 H59 0.9500 . ?
C59 C58 1.388(3) . ?
C1 C2 1.394(3) . ?
C1 C6 1.393(3) . ?
C39 C40 1.466(3) . ?
C23 C28 1.400(2) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.525(2) . ?
C77 C78 1.401(3) . ?
C77 C82 1.407(3) . ?
C77 B2 1.647(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.390(3) . ?
C91 H91 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.526(2) . ?
C46 H46 0.9500 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C37 1.526(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C52 H52 0.9500 . ?
C83 C88 1.396(3) . ?
C83 C84 1.410(3) . ?
C83 B2 1.647(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C33 H33 0.9500 . ?
C33 C34 1.387(3) . ?
C11 H11 0.9500 . ?
C11 C10 1.381(3) . ?
C72 H72 0.9500 . ?
C72 C71 1.403(3) . ?
C72 C73 1.395(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C44 H44 0.9500 . ?
C74 H74 0.9500 . ?
C74 C75 1.387(3) . ?
C74 C73 1.388(3) . ?
C87 H87 0.9500 . ?
C87 C88 1.396(3) . ?
C87 C86 1.380(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C71 C76 1.407(3) . ?
C71 B2 1.654(3) . ?
C78 H78 0.9500 . ?
C78 C79 1.397(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.386(3) . ?
C76 H76 0.9500 . ?
C76 C75 1.389(3) . ?
C75 H75 0.9500 . ?
C88 H88 0.9500 . ?
C58 H58 0.9500 . ?
C58 C57 1.385(3) . ?
C36 H36 0.9500 . ?
C36 C35 1.390(3) . ?
C28 H28 0.9500 . ?
C28 C27 1.387(3) . ?
C65 C66 1.403(3) . ?
C65 C70 1.407(3) . ?
C65 B2 1.651(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.377(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.388(3) . ?
C84 H84 0.9500 . ?
C84 C85 1.398(3) . ?
C86 H86 0.9500 . ?
C86 C85 1.384(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.383(3) . ?
C56 H56 0.9500 . ?
C56 C57 1.382(3) . ?
C35 H35 0.9500 . ?
C57 H57 0.9500 . ?
C10 H10 0.9500 . ?
C10 C9 1.387(3) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C73 H73 0.9500 . ?
C66 H66 0.9500 . ?
C66 C67 1.398(3) . ?
C22 H22 0.9500 . ?
C22 C21 1.409(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.389(3) . ?
C82 H82 0.9500 . ?
C82 C81 1.391(3) . ?
C70 H70 0.9500 . ?
C70 C69 1.397(3) . ?
C85 H85 0.9500 . ?
C80 H80 0.9500 . ?
C80 C79 1.378(3) . ?
C80 C81 1.394(4) . ?
C27 H27 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.387(3) . ?
C79 H79 0.9500 . ?
C18 H18 0.9500 . ?
C18 C19 1.386(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.385(3) . ?
C81 H81 0.9500 . ?
C69 H69 0.9500 . ?
C69 C68 1.379(4) . ?
C9 H9 0.9500 . ?
C21 H21 0.9500 . ?
C21 C20 1.380(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.378(4) . ?
C68 H68 0.9500 . ?
C68 C67 1.382(4) . ?
C67 H67 0.9500 . ?
C20 H20 0.9500 . ?
C20 C19 1.367(4) . ?
C89 N5 1.135(4) . ?
C89 C90 1.439(4) . ?
C19 H19 0.9500 . ?
C5 H5 0.9500 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N1 C13 P1 -40.51(12) . . . . ?
Ni1 N1 C14 C15 45.17(14) . . . . ?
Ni1 N1 C38 C37 17.49(16) . . . . ?
Ni1 N3 C29 C30 48.50(14) . . . . ?
Ni1 N3 C16 P2 -42.23(12) . . . . ?
Ni1 N3 C15 C14 18.87(16) . . . . ?
Ni1 N2 C41 C31 171.64(11) . . . . ?
Ni1 N2 C30 C29 21.65(16) . . . . ?
Ni1 N2 C37 C38 46.06(15) . . . . ?
P1 C7 C12 C11 179.24(14) . . . . ?
P1 C7 C8 C9 -179.29(17) . . . . ?
P1 C1 C2 C3 177.05(18) . . . . ?
P1 C1 C6 C5 -175.9(2) . . . . ?
P2 C17 C22 C21 -179.67(17) . . . . ?
P2 C17 C18 C19 179.98(17) . . . . ?
P2 C23 C28 C27 -179.01(15) . . . . ?
O2 P2 C17 C22 169.86(16) . . . . ?
O2 P2 C17 C18 -11.42(17) . . . . ?
O2 P2 C23 C24 28.04(16) . . . . ?
O2 P2 C23 C28 -153.91(14) . . . . ?
O2 P2 C16 N3 25.45(13) . . . . ?
O1 P1 C7 C12 -148.14(14) . . . . ?
O1 P1 C7 C8 31.45(17) . . . . ?
O1 P1 C1 C2 30.05(18) . . . . ?
O1 P1 C1 C6 -152.80(16) . . . . ?
O1 P1 C13 N1 30.18(13) . . . . ?
N1 C14 C15 N3 -44.18(18) . . . . ?
N1 C38 C37 N2 -44.21(19) . . . . ?
N3 C29 C30 N2 -48.83(19) . . . . ?
C60 C61 C91 C62 0.6(3) . . . . ?
C60 C64 C63 C62 -0.7(3) . . . . ?
C54 C55 C56 C57 0.1(3) . . . . ?
C54 C59 C58 C57 -1.3(3) . . . . ?
C42 C47 C46 C45 0.5(3) . . . . ?
C42 C43 C44 C45 0.4(3) . . . . ?
C7 P1 O1 Ni1 116.49(8) . . . . ?
C7 P1 C1 C2 155.47(15) . . . . ?
C7 P1 C1 C6 -27.39(19) . . . . ?
C7 P1 C13 N1 -91.99(12) . . . . ?
C7 C12 C11 C10 0.4(3) . . . . ?
C7 C8 C9 C10 -0.3(3) . . . . ?
C31 C32 C33 C34 -0.9(3) . . . . ?
C31 C36 C35 C34 0.7(3) . . . . ?
C47 C42 C43 C44 0.3(2) . . . . ?
C47 C42 B1 C60 -67.5(2) . . . . ?
C47 C42 B1 C54 173.70(15) . . . . ?
C47 C42 B1 C48 53.2(2) . . . . ?
C53 C48 C49 C50 1.4(2) . . . . ?
C53 C48 B1 C60 -40.9(2) . . . . ?
C53 C48 B1 C54 76.61(19) . . . . ?
C53 C48 B1 C42 -162.99(15) . . . . ?
C61 C60 C64 C63 0.8(2) . . . . ?
C61 C60 B1 C54 138.86(16) . . . . ?
C61 C60 B1 C42 18.6(2) . . . . ?
C61 C60 B1 C48 -101.99(18) . . . . ?
C43 C42 C47 C46 -0.8(3) . . . . ?
C43 C42 B1 C60 114.78(17) . . . . ?
C43 C42 B1 C54 -4.0(2) . . . . ?
C43 C42 B1 C48 -124.48(17) . . . . ?
C55 C54 C59 C58 2.1(3) . . . . ?
C55 C54 B1 C60 129.22(17) . . . . ?
C55 C54 B1 C42 -109.39(18) . . . . ?
C55 C54 B1 C48 10.5(2) . . . . ?
C55 C56 C57 C58 0.8(3) . . . . ?
C48 C53 C52 C51 0.1(3) . . . . ?
C48 C49 C50 C51 -0.6(3) . . . . ?
C64 C60 C61 C91 -0.7(2) . . . . ?
C64 C60 B1 C54 -41.82(19) . . . . ?
C64 C60 B1 C42 -162.10(15) . . . . ?
C64 C60 B1 C48 77.33(19) . . . . ?
C64 C63 C62 C91 0.6(3) . . . . ?
C63 C62 C91 C61 -0.5(3) . . . . ?
C17 P2 O2 Ni1 -114.30(8) . . . . ?
C17 P2 C23 C24 -94.46(15) . . . . ?
C17 P2 C23 C28 83.59(16) . . . . ?
C17 P2 C16 N3 145.16(11) . . . . ?
C17 C22 C21 C20 -0.5(3) . . . . ?
C17 C18 C19 C20 -0.3(3) . . . . ?
C24 C23 C28 C27 -1.0(3) . . . . ?
C24 C25 C26 C27 -1.4(3) . . . . ?
C12 C7 C8 C9 0.3(3) . . . . ?
C12 C11 C10 C9 -0.3(3) . . . . ?
C49 C48 B1 C60 142.03(16) . . . . ?
C49 C48 B1 C54 -100.49(18) . . . . ?
C49 C48 B1 C42 19.9(2) . . . . ?
C50 C51 C52 C53 0.7(3) . . . . ?
C59 C54 C55 C56 -1.5(3) . . . . ?
C59 C54 B1 C60 -52.74(19) . . . . ?
C59 C54 B1 C42 68.65(19) . . . . ?
C59 C54 B1 C48 -171.46(15) . . . . ?
C59 C58 C57 C56 -0.2(3) . . . . ?
C1 P1 O1 Ni1 -120.11(8) . . . . ?
C1 P1 C7 C12 85.99(16) . . . . ?
C1 P1 C7 C8 -94.42(16) . . . . ?
C1 P1 C13 N1 151.13(11) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
C1 C6 C5 C4 -0.8(4) . . . . ?
C23 P2 O2 Ni1 123.92(8) . . . . ?
C23 P2 C17 C22 -66.95(19) . . . . ?
C23 P2 C17 C18 111.76(16) . . . . ?
C23 P2 C16 N3 -96.19(12) . . . . ?
C23 C24 C25 C26 0.3(3) . . . . ?
C23 C28 C27 C26 -0.1(3) . . . . ?
C41 N2 C30 C29 -101.63(16) . . . . ?
C41 N2 C37 C38 165.77(13) . . . . ?
C41 C31 C32 C33 -174.60(16) . . . . ?
C41 C31 C36 C35 174.72(17) . . . . ?
C13 P1 O1 Ni1 -3.96(10) . . . . ?
C13 P1 C7 C12 -29.05(17) . . . . ?
C13 P1 C7 C8 150.54(15) . . . . ?
C13 P1 C1 C2 -87.00(17) . . . . ?
C13 P1 C1 C6 90.14(18) . . . . ?
C13 N1 C14 C15 161.06(13) . . . . ?
C13 N1 C38 C37 -101.87(16) . . . . ?
C29 N3 C16 P2 -155.44(11) . . . . ?
C29 N3 C15 C14 132.11(15) . . . . ?
C77 C78 C79 C80 -0.5(3) . . . . ?
C77 C82 C81 C80 0.3(3) . . . . ?
C32 C31 C41 N2 90.06(19) . . . . ?
C32 C31 C36 C35 -3.1(3) . . . . ?
C32 C33 C34 C35 -1.6(3) . . . . ?
C14 N1 C13 P1 -154.89(11) . . . . ?
C14 N1 C38 C37 132.98(15) . . . . ?
C46 C45 C44 C43 -0.7(3) . . . . ?
C38 N1 C13 P1 79.47(14) . . . . ?
C38 N1 C14 C15 -72.43(17) . . . . ?
C16 P2 O2 Ni1 3.90(9) . . . . ?
C16 P2 C17 C22 51.57(19) . . . . ?
C16 P2 C17 C18 -129.72(15) . . . . ?
C16 P2 C23 C24 147.61(13) . . . . ?
C16 P2 C23 C28 -34.34(17) . . . . ?
C16 N3 C29 C30 165.18(14) . . . . ?
C16 N3 C15 C14 -101.37(16) . . . . ?
C52 C53 C48 C49 -1.2(2) . . . . ?
C52 C53 C48 B1 -178.47(16) . . . . ?
C52 C51 C50 C49 -0.5(3) . . . . ?
C83 C84 C85 C86 0.0(3) . . . . ?
C30 N2 C41 C31 -67.20(18) . . . . ?
C30 N2 C37 C38 -69.59(17) . . . . ?
C33 C34 C35 C36 1.7(3) . . . . ?
C11 C10 C9 C8 0.3(4) . . . . ?
C72 C71 C76 C75 -0.6(3) . . . . ?
C72 C71 B2 C77 101.24(19) . . . . ?
C72 C71 B2 C83 -19.4(2) . . . . ?
C72 C71 B2 C65 -140.84(18) . . . . ?
C15 N3 C29 C30 -67.86(17) . . . . ?
C15 N3 C16 P2 77.73(14) . . . . ?
C44 C45 C46 C47 0.3(3) . . . . ?
C87 C86 C85 C84 -0.4(3) . . . . ?
C37 N2 C41 C31 56.79(18) . . . . ?
C37 N2 C30 C29 134.70(15) . . . . ?
C71 C72 C73 C74 0.3(3) . . . . ?
C71 C76 C75 C74 0.6(3) . . . . ?
C78 C77 C82 C81 -2.1(3) . . . . ?
C78 C77 B2 C83 105.6(2) . . . . ?
C78 C77 B2 C71 -14.4(2) . . . . ?
C78 C77 B2 C65 -133.12(19) . . . . ?
C8 C7 C12 C11 -0.3(3) . . . . ?
C76 C71 B2 C77 -73.3(2) . . . . ?
C76 C71 B2 C83 166.01(16) . . . . ?
C76 C71 B2 C65 44.6(2) . . . . ?
C75 C74 C73 C72 -0.4(3) . . . . ?
C88 C83 C84 C85 0.4(3) . . . . ?
C88 C83 B2 C77 11.0(2) . . . . ?
C88 C83 B2 C71 129.51(18) . . . . ?
C88 C83 B2 C65 -109.3(2) . . . . ?
C88 C87 C86 C85 0.2(3) . . . . ?
C36 C31 C41 N2 -87.7(2) . . . . ?
C36 C31 C32 C33 3.3(3) . . . . ?
C65 C66 C67 C68 0.8(3) . . . . ?
C65 C70 C69 C68 2.2(3) . . . . ?
C25 C24 C23 P2 179.00(14) . . . . ?
C25 C24 C23 C28 0.9(3) . . . . ?
C25 C26 C27 C28 1.3(3) . . . . ?
C84 C83 C88 C87 -0.6(3) . . . . ?
C84 C83 B2 C77 -169.78(17) . . . . ?
C84 C83 B2 C71 -51.3(2) . . . . ?
C84 C83 B2 C65 69.9(2) . . . . ?
C86 C87 C88 C83 0.3(3) . . . . ?
C2 C1 C6 C5 1.1(3) . . . . ?
C2 C3 C4 C5 1.5(4) . . . . ?
C73 C72 C71 C76 0.2(3) . . . . ?
C73 C72 C71 B2 -174.73(17) . . . . ?
C73 C74 C75 C76 -0.1(3) . . . . ?
C66 C65 C70 C69 -3.2(3) . . . . ?
C66 C65 B2 C77 -141.28(19) . . . . ?
C66 C65 B2 C83 -19.5(3) . . . . ?
C66 C65 B2 C71 101.5(2) . . . . ?
C22 C17 C18 C19 -1.3(3) . . . . ?
C22 C21 C20 C19 -1.2(4) . . . . ?
C82 C77 C78 C79 2.1(3) . . . . ?
C82 C77 B2 C83 -73.4(2) . . . . ?
C82 C77 B2 C71 166.66(17) . . . . ?
C82 C77 B2 C65 47.9(2) . . . . ?
C70 C65 C66 C67 1.8(3) . . . . ?
C70 C65 B2 C77 42.5(2) . . . . ?
C70 C65 B2 C83 164.28(18) . . . . ?
C70 C65 B2 C71 -74.6(2) . . . . ?
C70 C69 C68 C67 0.6(4) . . . . ?
C6 C1 C2 C3 -0.1(3) . . . . ?
C79 C80 C81 C82 1.5(3) . . . . ?
C18 C17 C22 C21 1.7(3) . . . . ?
C3 C4 C5 C6 -0.5(4) . . . . ?
C81 C80 C79 C78 -1.4(3) . . . . ?
C69 C68 C67 C66 -2.0(4) . . . . ?
B1 C60 C61 C91 178.61(15) . . . . ?
B1 C60 C64 C63 -178.58(16) . . . . ?
B1 C54 C55 C56 176.67(17) . . . . ?
B1 C54 C59 C58 -176.12(17) . . . . ?
B1 C42 C47 C46 -178.72(16) . . . . ?
B1 C42 C43 C44 178.15(16) . . . . ?
B1 C48 C49 C50 178.70(16) . . . . ?
B2 C77 C78 C79 -176.89(19) . . . . ?
B2 C77 C82 C81 176.99(19) . . . . ?
B2 C83 C88 C87 178.64(17) . . . . ?
B2 C83 C84 C85 -178.86(18) . . . . ?
B2 C71 C76 C75 174.33(17) . . . . ?
B2 C65 C66 C67 -174.60(19) . . . . ?
B2 C65 C70 C69 173.3(2) . . . . ?
C21 C20 C19 C18 1.6(4) . . . . ?
