#------------------------------------------------------------------------------
#$Date: 2022-02-12 01:54:55 +0200 (Sat, 12 Feb 2022) $
#$Revision: 272941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/94/7709474.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_7709474
loop_
_publ_author_name
'Cui, Xiaoxiao'
'Hao, Xiujia'
'Guo, Fang'
_publ_section_title
;
 Stepwise synthesis and catalysis in C-S cross-coupling of
 pyridine-functionalized N-heterocyclic carbene nickel (II) complexes by
 mechanochemistry
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03651C
_journal_year                    2022
_chemical_formula_moiety         '2(C27 H22 N6 Ni), 8(F3 P0.5), C2 H3 N'
_chemical_formula_sum            'C56 H47 F24 N13 Ni2 P4'
_chemical_formula_weight         1599.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-26 deposited with the CCDC.	2022-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.261(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.2054(15)
_cell_length_b                   12.4113(6)
_cell_length_c                   17.2760(9)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    273
_cell_measurement_theta_max      28.332
_cell_measurement_theta_min      2.984
_cell_volume                     6147.1(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      273
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49237
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         28.364
_diffrn_reflns_theta_min         2.889
_exptl_absorpt_coefficient_mu    0.842
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       block
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.414(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         14027
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0511
_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)+(0.0566P)²+17.7115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                12360
_reflns_number_total             14027
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03651c2.cif
_cod_data_source_block           2020_12_18_gf_cxx_2a_0m
_cod_database_code               7709474
_shelx_shelxl_version_number     2014/7
_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   0.906
_shelx_estimated_absorpt_t_min   0.780
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.586(18)
 0.414(18)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C49(H49A,H49B), C14(H14A,H14B), C41(H41A,H41B), C22(H22A,H22B),
 C33(H33A,H33B)
3.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C44(H44), C54(H54), C12(H12), C18(H18), C29(H29), C46(H46),
 C26(H26), C24(H24), C3(H3), C9(H9), C31(H31), C4(H4), C10(H10), C1(H1),
 C36(H36), C27(H27), C30(H30), C51(H51), C25(H25), C47(H47), C20(H20), C2(H2),
 C53(H53), C11(H11), C38(H38), C19(H19), C45(H45), C52(H52), C39(H39), C37(H37),
  C17(H17)
3.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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 0.63097(3) 0.70829(5) 0.92165(4) 0.02900(17) Uani 1 1 d . . . . .
Ni2 Ni 0.36763(3) 0.26203(5) 0.56882(4) 0.03028(18) Uani 1 1 d . . . . .
P4 P 0.5000 0.9698(2) 1.0000 0.0389(5) Uani 1 2 d S T P . .
P5 P 0.5000 0.0295(2) 0.5000 0.0420(6) Uani 1 2 d S T P . .
P1 P 0.78136(7) 0.62656(19) 1.03114(13) 0.0509(5) Uani 1 1 d . . . . .
P2 P 0.48794(7) 0.61568(19) 0.76994(12) 0.0516(4) Uani 1 1 d . . . . .
P3 P 0.21899(8) 0.33605(19) 0.47436(14) 0.0525(5) Uani 1 1 d . . . . .
F20 F 0.44461(16) 0.9715(4) 0.9699(3) 0.0606(12) Uani 1 1 d . . . . .
F24 F 0.49976(18) -0.0605(4) 0.4346(3) 0.0609(12) Uani 1 1 d . . . . .
N7 N 0.35537(18) 0.1901(4) 0.4628(3) 0.0322(11) Uani 1 1 d . . . . .
F23 F 0.44419(16) 0.0310(5) 0.4598(3) 0.0663(14) Uani 1 1 d . . . . .
F21 F 0.4961(2) 0.8798(4) 0.9321(3) 0.0672(14) Uani 1 1 d . . . . .
N3 N 0.62657(17) 0.4758(4) 0.9404(3) 0.0309(10) Uani 1 1 d . . . . .
N6 N 0.61626(19) 0.8418(4) 0.8584(3) 0.0316(11) Uani 1 1 d . . . . .
N8 N 0.40053(18) 0.3930(4) 0.4713(3) 0.0318(11) Uani 1 1 d . . . . .
F22 F 0.49975(19) 0.1212(4) 0.5650(3) 0.0652(13) Uani 1 1 d . . . . .
F19 F 0.50401(17) 1.0611(4) 1.0677(3) 0.0581(12) Uani 1 1 d . . . . .
N4 N 0.65423(18) 0.5293(5) 0.8359(3) 0.0316(11) Uani 1 1 d . . . . .
N5 N 0.65954(19) 0.6848(4) 0.7852(3) 0.0332(12) Uani 1 1 d . . . . .
N1 N 0.63743(19) 0.7764(4) 1.0260(3) 0.0337(11) Uani 1 1 d . . . . .
N12 N 0.38216(19) 0.1267(5) 0.6328(3) 0.0338(11) Uani 1 1 d . . . . .
N10 N 0.35158(18) 0.4454(5) 0.6582(3) 0.0323(11) Uani 1 1 d . . . . .
N2 N 0.59546(19) 0.5699(4) 1.0099(3) 0.0336(11) Uani 1 1 d . . . . .
C32 C 0.3734(2) 0.2192(5) 0.4067(4) 0.0356(13) Uani 1 1 d . . . . .
C23 C 0.6244(2) 0.8634(5) 0.7885(4) 0.0365(14) Uani 1 1 d . . . . .
C7 C 0.6201(2) 0.5778(5) 0.9613(3) 0.0293(12) Uani 1 1 d . . . . .
C28 C 0.3210(2) 0.1176(6) 0.4404(4) 0.0385(14) Uani 1 1 d . . . . .
H28 H 0.3087 0.0978 0.4793 0.046 Uiso 1 1 calc R . . . .
C44 C 0.3202(3) 0.5628(7) 0.7443(4) 0.0468(17) Uani 1 1 d . . . . .
H44 H 0.3232 0.6288 0.7215 0.056 Uiso 1 1 calc R . . . .
C15 C 0.6458(2) 0.6359(5) 0.8418(3) 0.0303(12) Uani 1 1 d . . . . .
N11 N 0.3451(2) 0.2916(5) 0.7109(3) 0.0368(12) Uani 1 1 d . . . . .
C6 C 0.5787(3) 0.6629(6) 1.0416(4) 0.0408(15) Uani 1 1 d . . . . .
H6A H 0.5687 0.6397 1.0854 0.049 Uiso 1 1 calc R . . . .
H6B H 0.5520 0.6940 0.9963 0.049 Uiso 1 1 calc R . . . .
C54 C 0.4101(3) 0.0585(6) 0.6149(4) 0.0439(16) Uani 1 1 d . . . . .
H54 H 0.4138 0.0676 0.5645 0.053 Uiso 1 1 calc R . . . .
F1 F 0.7531(3) 0.5528(9) 0.9529(5) 0.135(3) Uani 1 1 d . . . . .
N9 N 0.37639(18) 0.4929(4) 0.5481(3) 0.0319(11) Uani 1 1 d . . . . .
C13 C 0.6065(2) 0.4022(6) 0.9766(4) 0.0340(13) Uani 1 1 d . . . . .
C12 C 0.6048(3) 0.2908(6) 0.9748(5) 0.0438(16) Uani 1 1 d . . . . .
H12 H 0.6187 0.2507 0.9456 0.053 Uiso 1 1 calc R . . . .
F13 F 0.2038(3) 0.4382(7) 0.4156(6) 0.123(3) Uani 1 1 d . . . . .
C18 C 0.7067(3) 0.4310(7) 0.6910(4) 0.0493(18) Uani 1 1 d . . . . .
H18 H 0.7161 0.3699 0.6707 0.059 Uiso 1 1 calc R . . . .
C42 C 0.3570(2) 0.3386(6) 0.6524(4) 0.0337(13) Uani 1 1 d . . . . .
C34 C 0.3793(2) 0.3912(5) 0.5255(3) 0.0310(12) Uani 1 1 d . . . . .
C49 C 0.3403(3) 0.1771(6) 0.7213(5) 0.0486(18) Uani 1 1 d . . . . .
H49A H 0.3096 0.1541 0.6826 0.058 Uiso 1 1 calc R . . . .
H49B H 0.3427 0.1635 0.7781 0.058 Uiso 1 1 calc R . . . .
F3 F 0.8256(2) 0.5958(7) 1.0140(5) 0.113(3) Uani 1 1 d . . . . .
C29 C 0.3032(3) 0.0710(6) 0.3613(4) 0.0455(16) Uani 1 1 d . . . . .
H29 H 0.2794 0.0202 0.3476 0.055 Uiso 1 1 calc R . . . .
C5 C 0.6158(2) 0.7464(5) 1.0763(4) 0.0350(13) Uani 1 1 d . . . . .
C46 C 0.2975(3) 0.4536(8) 0.8395(4) 0.053(2) Uani 1 1 d . . . . .
H46 H 0.2851 0.4514 0.8804 0.063 Uiso 1 1 calc R . . . .
C43 C 0.3331(2) 0.4666(6) 0.7190(4) 0.0331(13) Uani 1 1 d . . . . .
C26 C 0.5613(3) 0.9875(7) 0.8195(5) 0.0491(18) Uani 1 1 d . . . . .
H26 H 0.5408 1.0310 0.8326 0.059 Uiso 1 1 calc R . . . .
C24 C 0.6003(3) 0.9419(6) 0.7328(4) 0.0458(17) Uani 1 1 d . . . . .
H24 H 0.6054 0.9522 0.6838 0.055 Uiso 1 1 calc R . . . .
C8 C 0.5863(2) 0.4623(5) 1.0208(4) 0.0355(13) Uani 1 1 d . . . . .
F14 F 0.1792(3) 0.3645(9) 0.5043(6) 0.136(3) Uani 1 1 d . . . . .
C3 C 0.6640(3) 0.8616(7) 1.1859(4) 0.052(2) Uani 1 1 d . . . . .
H3 H 0.6733 0.8888 1.2403 0.063 Uiso 1 1 calc R . . . .
C35 C 0.4121(2) 0.4994(5) 0.4595(4) 0.0347(13) Uani 1 1 d . . . . .
F6 F 0.8123(4) 0.6935(8) 1.1096(5) 0.142(3) Uani 1 1 d . . . . .
C50 C 0.3765(2) 0.1119(6) 0.7058(4) 0.0354(14) Uani 1 1 d . . . . .
C9 C 0.5628(3) 0.4119(6) 1.0646(5) 0.0461(17) Uani 1 1 d . . . . .
H9 H 0.5487 0.4513 1.0939 0.055 Uiso 1 1 calc R . . . .
C21 C 0.6774(2) 0.6121(6) 0.7451(4) 0.0357(13) Uani 1 1 d . . . . .
C31 C 0.3569(3) 0.1739(6) 0.3269(4) 0.0443(17) Uani 1 1 d . . . . .
H31 H 0.3702 0.1929 0.2891 0.053 Uiso 1 1 calc R . . . .
C4 C 0.6286(3) 0.7886(6) 1.1563(4) 0.0457(17) Uani 1 1 d . . . . .
H4 H 0.6131 0.7672 1.1899 0.055 Uiso 1 1 calc R . . . .
C10 C 0.5614(3) 0.3029(7) 1.0627(6) 0.060(2) Uani 1 1 d . . . . .
H10 H 0.5465 0.2671 1.0923 0.072 Uiso 1 1 calc R . . . .
C14 C 0.6533(3) 0.4456(6) 0.8924(4) 0.0392(15) Uani 1 1 d . . . . .
H14A H 0.6850 0.4290 0.9306 0.047 Uiso 1 1 calc R . . . .
H14B H 0.6399 0.3811 0.8602 0.047 Uiso 1 1 calc R . . . .
C41 C 0.3541(2) 0.5297(6) 0.6022(4) 0.0368(14) Uani 1 1 d . . . . .
H41A H 0.3229 0.5544 0.5678 0.044 Uiso 1 1 calc R . . . .
H41B H 0.3715 0.5903 0.6353 0.044 Uiso 1 1 calc R . . . .
C16 C 0.6737(2) 0.5120(6) 0.7774(4) 0.0351(14) Uani 1 1 d . . . . .
C1 C 0.6714(3) 0.8501(6) 1.0550(4) 0.0426(16) Uani 1 1 d . . . . .
H1 H 0.6860 0.8722 1.0199 0.051 Uiso 1 1 calc R . . . .
C36 C 0.4343(3) 0.5409(6) 0.4097(4) 0.0445(16) Uani 1 1 d . . . . .
H36 H 0.4447 0.4976 0.3767 0.053 Uiso 1 1 calc R . . . .
C27 C 0.5844(2) 0.9032(6) 0.8724(4) 0.0392(15) Uani 1 1 d . . . . .
H27 H 0.5776 0.8885 0.9191 0.047 Uiso 1 1 calc R . . . .
C30 C 0.3207(3) 0.0999(7) 0.3037(4) 0.0493(18) Uani 1 1 d . . . . .
H30 H 0.3086 0.0707 0.2498 0.059 Uiso 1 1 calc R . . . .
C51 C 0.4007(3) 0.0320(7) 0.7622(4) 0.0469(17) Uani 1 1 d . . . . .
H51 H 0.3977 0.0255 0.8134 0.056 Uiso 1 1 calc R . . . .
F4 F 0.7901(3) 0.5220(6) 1.0886(5) 0.114(3) Uani 1 1 d . . . . .
C25 C 0.5688(3) 1.0057(7) 0.7485(5) 0.053(2) Uani 1 1 d . . . . .
H25 H 0.5529 1.0602 0.7113 0.064 Uiso 1 1 calc R . . . .
F18 F 0.2571(4) 0.3139(9) 0.4426(8) 0.184(6) Uani 1 1 d . . . . .
C47 C 0.3103(2) 0.3597(7) 0.8140(4) 0.0453(17) Uani 1 1 d . . . . .
H47 H 0.3069 0.2934 0.8361 0.054 Uiso 1 1 calc R . . . .
C20 C 0.6963(3) 0.6254(7) 0.6847(4) 0.0448(16) Uani 1 1 d . . . . .
H20 H 0.6988 0.6925 0.6629 0.054 Uiso 1 1 calc R . . . .
C2 C 0.6859(3) 0.8948(7) 1.1342(5) 0.0538(19) Uani 1 1 d . . . . .
H2 H 0.7097 0.9457 1.1524 0.065 Uiso 1 1 calc R . . . .
C53 C 0.4338(3) -0.0245(7) 0.6672(5) 0.0476(17) Uani 1 1 d . . . . .
H53 H 0.4526 -0.0707 0.6519 0.057 Uiso 1 1 calc R . . . .
F5 F 0.7363(3) 0.6479(8) 1.0463(8) 0.150(4) Uani 1 1 d . . . . .
C11 C 0.5816(3) 0.2426(7) 1.0181(5) 0.056(2) Uani 1 1 d . . . . .
H11 H 0.5792 0.1679 1.0178 0.068 Uiso 1 1 calc R . . . .
C38 C 0.4237(3) 0.7158(7) 0.4620(5) 0.056(2) Uani 1 1 d . . . . .
H38 H 0.4282 0.7899 0.4619 0.068 Uiso 1 1 calc R . . . .
C19 C 0.7113(3) 0.5295(8) 0.6592(4) 0.0497(18) Uani 1 1 d . . . . .
H19 H 0.7246 0.5333 0.6197 0.060 Uiso 1 1 calc R . . . .
F17 F 0.2292(5) 0.2293(8) 0.5232(7) 0.172(5) Uani 1 1 d . . . . .
C45 C 0.3024(3) 0.5538(7) 0.8063(4) 0.0511(18) Uani 1 1 d . . . . .
H45 H 0.2935 0.6159 0.8262 0.061 Uiso 1 1 calc R . . . .
C40 C 0.3964(2) 0.5628(5) 0.5076(4) 0.0349(13) Uani 1 1 d . . . . .
C52 C 0.4291(3) -0.0376(6) 0.7424(5) 0.0496(18) Uani 1 1 d . . . . .
H52 H 0.4448 -0.0925 0.7793 0.060 Uiso 1 1 calc R . . . .
C48 C 0.3289(2) 0.3688(7) 0.7523(4) 0.0397(15) Uani 1 1 d . . . . .
F12 F 0.4729(3) 0.5425(9) 0.6931(5) 0.177(5) Uani 1 1 d . . . . .
C22 C 0.6625(3) 0.8025(6) 0.7767(5) 0.0481(18) Uani 1 1 d . . . . .
H22A H 0.6617 0.8184 0.7212 0.058 Uiso 1 1 calc R . . . .
H22B H 0.6922 0.8273 0.8179 0.058 Uiso 1 1 calc R . . . .
F2 F 0.7750(5) 0.7299(8) 0.9787(7) 0.175(5) Uani 1 1 d . . . . .
C39 C 0.4014(3) 0.6744(6) 0.5106(5) 0.0461(17) Uani 1 1 d . . . . .
H39 H 0.3906 0.7180 0.5428 0.055 Uiso 1 1 calc R . . . .
C33 C 0.4129(3) 0.2970(6) 0.4353(4) 0.0424(16) Uani 1 1 d . . . . .
H33A H 0.4402 0.2631 0.4774 0.051 Uiso 1 1 calc R . . . .
H33B H 0.4205 0.3175 0.3880 0.051 Uiso 1 1 calc R . . . .
F15 F 0.1842(4) 0.2697(9) 0.3991(6) 0.162(4) Uani 1 1 d . . . . .
C37 C 0.4397(3) 0.6524(7) 0.4137(5) 0.055(2) Uani 1 1 d . . . . .
H37 H 0.4545 0.6851 0.3827 0.066 Uiso 1 1 calc R . . . .
C17 C 0.6887(2) 0.4183(6) 0.7524(4) 0.0421(15) Uani 1 1 d . . . . .
H17 H 0.6868 0.3514 0.7750 0.050 Uiso 1 1 calc R . . . .
F7 F 0.4604(6) 0.6995(8) 0.7101(8) 0.268(10) Uani 1 1 d . . . . .
F11 F 0.5127(4) 0.5286(8) 0.8354(7) 0.218(7) Uani 1 1 d . . . . .
F9 F 0.4440(3) 0.584(2) 0.7754(7) 0.321(13) Uani 1 1 d . . . . .
F8 F 0.5029(5) 0.6890(11) 0.8446(6) 0.255(8) Uani 1 1 d . . . . .
F16 F 0.2514(3) 0.4048(11) 0.5471(7) 0.180(5) Uani 1 1 d . . . . .
F10 F 0.5324(3) 0.626(2) 0.7665(7) 0.331(14) Uani 1 1 d . . . . .
N13 N 0.4352(4) 0.3094(8) 0.2582(6) 0.088(3) Uani 1 1 d . . . . .
C55 C 0.4671(5) 0.2961(9) 0.2480(7) 0.082(3) Uani 1 1 d . . . . .
C56 C 0.5078(4) 0.2771(11) 0.2317(11) 0.120(5) Uani 1 1 d . . . . .
H56A H 0.5025 0.2172 0.1939 0.181 Uiso 1 1 calc GR . . . .
H56B H 0.5336 0.2611 0.2837 0.181 Uiso 1 1 calc GR . . . .
H56C H 0.5148 0.3401 0.2067 0.181 Uiso 1 1 calc GR . . . .
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'
F F 0.0171 0.0103 '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'
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
N1 Ni1 N6 93.8(2) . . ?
C7 Ni1 N6 157.6(2) . . ?
C7 Ni1 N1 90.2(2) . . ?
C7 Ni1 C15 89.3(3) . . ?
C15 Ni1 N6 93.9(2) . . ?
C15 Ni1 N1 160.8(2) . . ?
N7 Ni2 N12 93.1(2) . . ?
C42 Ni2 N7 159.9(3) . . ?
C42 Ni2 N12 94.1(3) . . ?
C42 Ni2 C34 89.7(3) . . ?
C34 Ni2 N7 90.8(2) . . ?
C34 Ni2 N12 157.4(3) . . ?
F20 P4 F20 178.5(4) 2_657 . ?
F20 P4 F19 89.5(3) 2_657 . ?
F20 P4 F19 89.4(3) . 2_657 ?
F20 P4 F19 89.5(3) 2_657 2_657 ?
F20 P4 F19 89.5(3) . . ?
F21 P4 F20 90.6(3) 2_657 2_657 ?
F21 P4 F20 90.6(3) . . ?
F21 P4 F20 90.4(3) . 2_657 ?
F21 P4 F20 90.4(3) 2_657 . ?
F21 P4 F21 90.7(4) 2_657 . ?
F21 P4 F19 89.8(2) 2_657 . ?
F21 P4 F19 179.4(3) 2_657 2_657 ?
F21 P4 F19 179.4(3) . . ?
F21 P4 F19 89.8(2) . 2_657 ?
F19 P4 F19 89.6(4) 2_657 . ?
F24 P5 F24 90.6(4) . 2_656 ?
F24 P5 F23 90.1(3) . . ?
F24 P5 F23 90.1(3) 2_656 2_656 ?
F24 P5 F23 90.9(3) 2_656 . ?
F24 P5 F23 90.9(3) . 2_656 ?
F24 P5 F22 179.2(3) . . ?
F24 P5 F22 179.2(3) 2_656 2_656 ?
F24 P5 F22 90.1(3) . 2_656 ?
F24 P5 F22 90.1(3) 2_656 . ?
F23 P5 F23 178.6(5) 2_656 . ?
F23 P5 F22 89.6(3) 2_656 . ?
F23 P5 F22 89.4(3) 2_656 2_656 ?
F23 P5 F22 89.4(3) . . ?
F23 P5 F22 89.6(3) . 2_656 ?
F22 P5 F22 89.3(4) . 2_656 ?
F1 P1 F4 87.8(6) . . ?
F3 P1 F1 86.2(5) . . ?
F3 P1 F4 88.4(5) . . ?
F6 P1 F1 175.8(6) . . ?
F6 P1 F3 90.2(5) . . ?
F6 P1 F4 89.9(5) . . ?
F5 P1 F1 90.4(6) . . ?
F5 P1 F3 175.6(6) . . ?
F5 P1 F6 93.1(6) . . ?
F5 P1 F4 88.7(5) . . ?
F2 P1 F1 94.6(6) . . ?
F2 P1 F3 90.6(6) . . ?
F2 P1 F6 87.7(6) . . ?
F2 P1 F4 177.3(6) . . ?
F2 P1 F5 92.5(6) . . ?
F12 P2 F11 96.6(6) . . ?
F7 P2 F12 85.2(6) . . ?
F7 P2 F11 174.3(11) . . ?
F7 P2 F8 94.2(7) . . ?
F9 P2 F12 85.4(9) . . ?
F9 P2 F7 86.3(11) . . ?
F9 P2 F11 88.4(11) . . ?
F9 P2 F8 95.3(11) . . ?
F8 P2 F12 179.0(10) . . ?
F8 P2 F11 84.2(6) . . ?
F10 P2 F12 89.4(9) . . ?
F10 P2 F7 102.3(13) . . ?
F10 P2 F11 83.1(10) . . ?
F10 P2 F9 169.5(16) . . ?
F10 P2 F8 90.0(9) . . ?
F14 P3 F13 87.4(5) . . ?
F18 P3 F13 89.5(5) . . ?
F18 P3 F14 176.9(6) . . ?
F18 P3 F17 91.2(6) . . ?
F18 P3 F15 89.4(8) . . ?
F18 P3 F16 92.4(7) . . ?
F17 P3 F13 173.2(7) . . ?
F17 P3 F14 91.8(6) . . ?
F17 P3 F15 85.8(7) . . ?
F15 P3 F13 87.4(5) . . ?
F15 P3 F14 90.8(6) . . ?
F16 P3 F13 90.8(7) . . ?
F16 P3 F14 87.4(5) . . ?
F16 P3 F17 96.0(8) . . ?
F16 P3 F15 177.5(7) . . ?
C32 N7 Ni2 125.1(5) . . ?
C28 N7 Ni2 114.9(4) . . ?
C28 N7 C32 119.2(5) . . ?
C7 N3 C13 110.7(5) . . ?
C7 N3 C14 125.4(5) . . ?
C13 N3 C14 123.7(6) . . ?
C23 N6 Ni1 125.9(5) . . ?
C27 N6 Ni1 114.1(4) . . ?
C27 N6 C23 117.3(6) . . ?
C34 N8 C35 109.9(5) . . ?
C34 N8 C33 124.6(5) . . ?
C35 N8 C33 125.3(5) . . ?
C15 N4 C14 126.7(5) . . ?
C15 N4 C16 111.0(5) . . ?
C16 N4 C14 121.1(6) . . ?
C15 N5 C21 112.0(5) . . ?
C15 N5 C22 124.4(5) . . ?
C21 N5 C22 123.0(5) . . ?
C5 N1 Ni1 126.1(5) . . ?
C1 N1 Ni1 115.1(4) . . ?
C1 N1 C5 118.2(5) . . ?
C54 N12 Ni2 116.0(4) . . ?
C54 N12 C50 117.8(6) . . ?
C50 N12 Ni2 123.7(5) . . ?
C42 N10 C43 110.0(5) . . ?
C42 N10 C41 128.2(5) . . ?
C43 N10 C41 120.7(5) . . ?
C7 N2 C6 123.6(5) . . ?
C7 N2 C8 110.6(5) . . ?
C8 N2 C6 125.7(5) . . ?
N7 C32 C31 120.7(6) . . ?
N7 C32 C33 117.4(5) . . ?
C31 C32 C33 121.8(6) . . ?
N6 C23 C24 121.7(7) . . ?
N6 C23 C22 117.4(6) . . ?
C24 C23 C22 120.8(6) . . ?
N3 C7 Ni1 130.9(4) . . ?
N2 C7 Ni1 122.0(5) . . ?
N2 C7 N3 106.3(5) . . ?
N7 C28 H28 118.9 . . ?
N7 C28 C29 122.2(6) . . ?
C29 C28 H28 118.9 . . ?
C43 C44 H44 122.3 . . ?
C43 C44 C45 115.3(8) . . ?
C45 C44 H44 122.3 . . ?
N4 C15 Ni1 129.8(4) . . ?
N5 C15 Ni1 124.2(5) . . ?
N5 C15 N4 104.8(5) . . ?
C42 N11 C49 126.4(6) . . ?
C42 N11 C48 110.5(6) . . ?
C48 N11 C49 122.2(6) . . ?
N2 C6 H6A 109.4 . . ?
N2 C6 H6B 109.4 . . ?
N2 C6 C5 111.3(5) . . ?
H6A C6 H6B 108.0 . . ?
C5 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
N12 C54 H54 118.2 . . ?
N12 C54 C53 123.5(6) . . ?
C53 C54 H54 118.2 . . ?
C34 N9 C41 126.4(5) . . ?
C34 N9 C40 110.2(5) . . ?
C40 N9 C41 123.3(6) . . ?
C12 C13 N3 131.8(6) . . ?
C12 C13 C8 122.0(6) . . ?
C8 C13 N3 106.2(6) . . ?
C13 C12 H12 121.7 . . ?
C11 C12 C13 116.6(7) . . ?
C11 C12 H12 121.7 . . ?
C19 C18 H18 118.5 . . ?
C19 C18 C17 122.9(7) . . ?
C17 C18 H18 118.5 . . ?
N10 C42 Ni2 128.9(5) . . ?
N11 C42 Ni2 123.3(5) . . ?
N11 C42 N10 106.9(5) . . ?
N8 C34 Ni2 121.4(5) . . ?
N9 C34 Ni2 130.6(4) . . ?
N9 C34 N8 107.2(5) . . ?
N11 C49 H49A 109.0 . . ?
N11 C49 H49B 109.0 . . ?
N11 C49 C50 112.8(6) . . ?
H49A C49 H49B 107.8 . . ?
C50 C49 H49A 109.0 . . ?
C50 C49 H49B 109.0 . . ?
C28 C29 H29 120.3 . . ?
C30 C29 C28 119.4(7) . . ?
C30 C29 H29 120.3 . . ?
N1 C5 C6 116.1(5) . . ?
N1 C5 C4 121.4(7) . . ?
C4 C5 C6 122.5(6) . . ?
C47 C46 H46 118.9 . . ?
C47 C46 C45 122.3(6) . . ?
C45 C46 H46 118.9 . . ?
C44 C43 N10 130.7(7) . . ?
C48 C43 N10 106.4(6) . . ?
C48 C43 C44 122.9(6) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C25 C26 C27 119.3(7) . . ?
C23 C24 H24 119.7 . . ?
C23 C24 C25 120.6(6) . . ?
C25 C24 H24 119.7 . . ?
C13 C8 N2 106.2(5) . . ?
C13 C8 C9 120.6(6) . . ?
C9 C8 N2 133.2(6) . . ?
C4 C3 H3 120.4 . . ?
C4 C3 C2 119.2(6) . . ?
C2 C3 H3 120.4 . . ?
C36 C35 N8 130.7(6) . . ?
C40 C35 N8 106.3(5) . . ?
C40 C35 C36 123.0(6) . . ?
N12 C50 C49 118.6(6) . . ?
N12 C50 C51 121.1(6) . . ?
C51 C50 C49 120.1(6) . . ?
C8 C9 H9 121.5 . . ?
C10 C9 C8 117.0(7) . . ?
C10 C9 H9 121.5 . . ?
N5 C21 C16 105.7(5) . . ?
N5 C21 C20 132.1(7) . . ?
C16 C21 C20 122.3(7) . . ?
C32 C31 H31 120.2 . . ?
C32 C31 C30 119.7(6) . . ?
C30 C31 H31 120.2 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 C5 120.0(7) . . ?
C3 C4 H4 120.0 . . ?
C9 C10 H10 118.8 . . ?
C9 C10 C11 122.4(7) . . ?
C11 C10 H10 118.8 . . ?
N3 C14 H14A 109.2 . . ?
N3 C14 H14B 109.2 . . ?
N4 C14 N3 112.1(6) . . ?
N4 C14 H14A 109.2 . . ?
N4 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
N10 C41 H41A 109.2 . . ?
N10 C41 H41B 109.2 . . ?
N9 C41 N10 111.9(5) . . ?
N9 C41 H41A 109.2 . . ?
N9 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
C21 C16 N4 106.5(6) . . ?
C17 C16 N4 131.1(7) . . ?
C17 C16 C21 122.4(6) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.1(7) . . ?
C2 C1 H1 118.4 . . ?
C35 C36 H36 122.8 . . ?
C37 C36 C35 114.5(7) . . ?
C37 C36 H36 122.8 . . ?
N6 C27 C26 122.4(6) . . ?
N6 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
C29 C30 C31 118.7(6) . . ?
C29 C30 H30 120.6 . . ?
C31 C30 H30 120.6 . . ?
C50 C51 H51 120.0 . . ?
C52 C51 C50 120.1(6) . . ?
C52 C51 H51 120.0 . . ?
C26 C25 C24 118.6(7) . . ?
C26 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C46 C47 H47 122.0 . . ?
C46 C47 C48 116.0(8) . . ?
C48 C47 H47 122.0 . . ?
C21 C20 H20 122.5 . . ?
C21 C20 C19 115.0(7) . . ?
C19 C20 H20 122.5 . . ?
C3 C2 H2 121.0 . . ?
C1 C2 C3 118.0(8) . . ?
C1 C2 H2 121.0 . . ?
C54 C53 H53 120.7 . . ?
C52 C53 C54 118.6(7) . . ?
C52 C53 H53 120.7 . . ?
C12 C11 C10 121.4(7) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C39 C38 H38 118.5 . . ?
C37 C38 H38 118.5 . . ?
C37 C38 C39 123.0(8) . . ?
C18 C19 C20 121.8(6) . . ?
C18 C19 H19 119.1 . . ?
C20 C19 H19 119.1 . . ?
C44 C45 C46 121.8(7) . . ?
C44 C45 H45 119.1 . . ?
C46 C45 H45 119.1 . . ?
C35 C40 N9 106.4(6) . . ?
C35 C40 C39 122.1(6) . . ?
C39 C40 N9 131.5(7) . . ?
C51 C52 H52 120.6 . . ?
C53 C52 C51 118.8(7) . . ?
C53 C52 H52 120.6 . . ?
N11 C48 C47 132.1(7) . . ?
C43 C48 N11 106.2(5) . . ?
C43 C48 C47 121.7(7) . . ?
N5 C22 C23 113.9(6) . . ?
N5 C22 H22A 108.8 . . ?
N5 C22 H22B 108.8 . . ?
C23 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C38 C39 C40 115.0(7) . . ?
C38 C39 H39 122.5 . . ?
C40 C39 H39 122.5 . . ?
N8 C33 C32 110.2(5) . . ?
N8 C33 H33A 109.6 . . ?
N8 C33 H33B 109.6 . . ?
C32 C33 H33A 109.6 . . ?
C32 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
C36 C37 H37 118.9 . . ?
C38 C37 C36 122.3(7) . . ?
C38 C37 H37 118.9 . . ?
C18 C17 H17 122.2 . . ?
C16 C17 C18 115.5(7) . . ?
C16 C17 H17 122.2 . . ?
N13 C55 C56 178.0(15) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 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 N6 1.938(5) . ?
Ni1 N1 1.929(5) . ?
Ni1 C7 1.842(6) . ?
Ni1 C15 1.852(6) . ?
Ni2 N7 1.935(5) . ?
Ni2 N12 1.963(6) . ?
Ni2 C42 1.863(6) . ?
Ni2 C34 1.864(6) . ?
P4 F20 1.596(5) . ?
P4 F20 1.596(5) 2_657 ?
P4 F21 1.590(5) 2_657 ?
P4 F21 1.590(5) . ?
P4 F19 1.597(5) . ?
P4 F19 1.597(5) 2_657 ?
P5 F24 1.587(5) 2_656 ?
P5 F24 1.587(5) . ?
P5 F23 1.600(4) 2_656 ?
P5 F23 1.600(4) . ?
P5 F22 1.601(5) . ?
P5 F22 1.601(5) 2_656 ?
P1 F1 1.581(7) . ?
P1 F3 1.570(6) . ?
P1 F6 1.558(8) . ?
P1 F4 1.591(7) . ?
P1 F5 1.551(7) . ?
P1 F2 1.537(8) . ?
P2 F12 1.522(7) . ?
P2 F7 1.480(9) . ?
P2 F11 1.534(9) . ?
P2 F9 1.466(11) . ?
P2 F8 1.494(8) . ?
P2 F10 1.417(9) . ?
P3 F13 1.576(8) . ?
P3 F14 1.562(7) . ?
P3 F18 1.519(7) . ?
P3 F17 1.535(8) . ?
P3 F15 1.559(8) . ?
P3 F16 1.525(9) . ?
N7 C32 1.348(7) . ?
N7 C28 1.334(9) . ?
N3 C7 1.353(8) . ?
N3 C13 1.389(8) . ?
N3 C14 1.439(7) . ?
N6 C23 1.354(7) . ?
N6 C27 1.348(8) . ?
N8 C34 1.346(7) . ?
N8 C35 1.405(8) . ?
N8 C33 1.464(8) . ?
N4 C15 1.360(8) . ?
N4 C14 1.433(8) . ?
N4 C16 1.386(7) . ?
N5 C15 1.356(8) . ?
N5 C21 1.381(8) . ?
N5 C22 1.474(9) . ?
N1 C5 1.345(7) . ?
N1 C1 1.340(9) . ?
N12 C54 1.337(9) . ?
N12 C50 1.353(7) . ?
N10 C42 1.346(9) . ?
N10 C43 1.408(7) . ?
N10 C41 1.449(8) . ?
N2 C7 1.347(7) . ?
N2 C6 1.460(8) . ?
N2 C8 1.394(9) . ?
C32 C31 1.386(9) . ?
C32 C33 1.489(10) . ?
C23 C24 1.367(10) . ?
C23 C22 1.490(10) . ?
C28 H28 0.9300 . ?
C28 C29 1.383(9) . ?
C44 H44 0.9300 . ?
C44 C43 1.384(10) . ?
C44 C45 1.391(10) . ?
N11 C42 1.342(8) . ?
N11 C49 1.447(10) . ?
N11 C48 1.403(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.492(10) . ?
C54 H54 0.9300 . ?
C54 C53 1.377(10) . ?
N9 C34 1.335(8) . ?
N9 C41 1.441(8) . ?
N9 C40 1.405(8) . ?
C13 C12 1.384(10) . ?
C13 C8 1.385(9) . ?
C12 H12 0.9300 . ?
C12 C11 1.368(10) . ?
C18 H18 0.9300 . ?
C18 C19 1.371(12) . ?
C18 C17 1.390(9) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 C50 1.496(10) . ?
C29 H29 0.9300 . ?
C29 C30 1.360(10) . ?
C5 C4 1.381(9) . ?
C46 H46 0.9300 . ?
C46 C47 1.361(12) . ?
C46 C45 1.402(13) . ?
C43 C48 1.370(10) . ?
C26 H26 0.9300 . ?
C26 C27 1.389(10) . ?
C26 C25 1.355(11) . ?
C24 H24 0.9300 . ?
C24 C25 1.370(11) . ?
C8 C9 1.393(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.362(12) . ?
C3 C2 1.386(11) . ?
C35 C36 1.400(9) . ?
C35 C40 1.368(9) . ?
C50 C51 1.386(10) . ?
C9 H9 0.9300 . ?
C9 C10 1.353(12) . ?
C21 C16 1.385(10) . ?
C21 C20 1.397(9) . ?
C31 H31 0.9300 . ?
C31 C30 1.387(11) . ?
C4 H4 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.389(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C16 C17 1.385(10) . ?
C1 H1 0.9300 . ?
C1 C2 1.377(10) . ?
C36 H36 0.9300 . ?
C36 C37 1.392(11) . ?
C27 H27 0.9300 . ?
C30 H30 0.9300 . ?
C51 H51 0.9300 . ?
C51 C52 1.374(11) . ?
C25 H25 0.9300 . ?
C47 H47 0.9300 . ?
C47 C48 1.407(9) . ?
C20 H20 0.9300 . ?
C20 C19 1.412(11) . ?
C2 H2 0.9300 . ?
C53 H53 0.9300 . ?
C53 C52 1.374(10) . ?
C11 H11 0.9300 . ?
C38 H38 0.9300 . ?
C38 C39 1.384(10) . ?
C38 C37 1.373(12) . ?
C19 H19 0.9300 . ?
C45 H45 0.9300 . ?
C40 C39 1.393(10) . ?
C52 H52 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C39 H39 0.9300 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C37 H37 0.9300 . ?
C17 H17 0.9300 . ?
N13 C55 1.091(14) . ?
C55 C56 1.425(16) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.586(18)
2 0.414(18)
