#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:23:40 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228841 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/99/1549959.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_1549959
loop_
_publ_author_name
'Truong, Phan T.'
'Broering, Ellen P.'
'Dzul, Stephen P.'
'Chakraborty, Indranil'
'Stemmler, Timothy L.'
'Harrop, Todd C.'
_publ_section_title
;
 Simultaneous nitrosylation and N-nitrosation of a Ni-thiolate model
 complex of Ni-containing SOD.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              8567
_journal_page_last               8574
_journal_paper_doi               10.1039/c8sc03321h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety
'2(C14 H6 F6 N4 Ni O2 S2), 3(C8 H20 N), C3 H6 N0.5, C4 N0.5, C4 H10 O'
_chemical_formula_sum            'C63 H88 F12 N12 Ni2 O5 S4'
_chemical_formula_weight         1567.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-09
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-07-12 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                112.8160(10)
_cell_angle_beta                 92.7190(10)
_cell_angle_gamma                91.167(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3985(6)
_cell_length_b                   16.8518(9)
_cell_length_c                   18.0347(9)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.43
_cell_volume                     3745.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest PHOTON 100 CMOS'
_diffrn_measurement_method       'PhiΩ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15409
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.458
_diffrn_reflns_theta_min         1.968
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.745373
_exptl_absorpt_correction_T_min  0.579933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER TWINABS'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       plate
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.254
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         15409
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      4.031
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0896P)²+11.0518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.2002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11647
_reflns_number_total             15409
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc03321h2.cif
_cod_data_source_block           twin5
_cod_depositor_comments
'Adding full bibliography for 1549958--1549959.cif.'
_cod_database_code               1549959
_shelx_shelxl_version_number     2018/3
_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   0.966
_shelx_estimated_absorpt_t_min   0.862
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5089(14)
 0.4911(14)
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. Restrained distances
 C55-C56
 1.5 with sigma of 0.02
 N12-C54
 1.45 with sigma of 0.02
 C59-C61
 1.45 with sigma of 0.02
 C62-C63
 1.45 with sigma of 0.02
 C62-C64
 1.54 with sigma of 0.02
 O5-C67
 1.46 with sigma of 0.02
 O5-C66
 1.53 with sigma of 0.02
 C65-C66
 1.78 with sigma of 0.02
 C67-C68
 1.65 with sigma of 0.02
 N12-C54 \\sim N12-C56 \\sim N12-C48
 with sigma of 0.02
 N13-C60 \\sim N13-C61 \\sim N13-C63 \\sim N13-C64
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(F3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C55) = Uanis(C56)
Uanis(C53) = Uanis(C54)
Uanis(C68) = Uanis(C67)
Uanis(F7') = Uanis(F7)
Uanis(F11) = Uanis(F12')
Uanis(F1) = Uanis(F1')
Uanis(F3) = Uanis(F3')
Uanis(F2) = Uanis(F2')
Uanis(F8') = Uanis(F8)
Uanis(F9) = Uanis(F9')
Uanis(F9') = Uanis(F8)
Uanis(F7) = Uanis(F8')
Uanis(F12) = Uanis(F10')
Uanis(C64) = Uanis(C62)
Uanis(C60) = Uanis(C63)
5. Same fragment restrains
{F1', F2', F3'} sigma for 1-2: 0.02, 1-3: 0.04
as
{F1, F2, F3}
{F7', F8', F9'} sigma for 1-2: 0.02, 1-3: 0.04
as
{F7, F8, F9}
{F10', F11', F12'} sigma for 1-2: 0.02, 1-3: 0.04
as
{F10, F11, F12}
6. Others
 Sof(F1')=Sof(F2')=Sof(F3')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F7')=Sof(F8')=Sof(F9')=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(F10')=Sof(F11')=Sof(F12')=1-FVAR(3)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(3)
 Fixed Sof: C54(0.5) C56(0.5) C60(0.5) C61(0.5) C63(0.5) C64(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B), C22(H22A,H22B), C24(H24A,
 H24B), C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C46(H46A,H46B),
 C48(H48A,H48B), C50(H50A,H50B), C52(H52A,H52B), C66(H66A,H66B), C67(H67A,H67B)
7.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C65(H65A,H65B,
 H65C), C68(H68A,H68B,H68C)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C33(H33), C35(H35),
 C36(H36), C40(H40), C42(H42), C43(H43)
;
_olex2_submission_special_instructions 'No special instructions were received'
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 0.49662(5) 0.31138(5) 0.15161(4) 0.02193(18) Uani 1 1 d . . . . .
S1 S 0.36561(11) 0.28817(10) 0.06456(9) 0.0260(3) Uani 1 1 d . . . . .
S2 S 0.61862(11) 0.29681(11) 0.23075(9) 0.0296(3) Uani 1 1 d . . . . .
N1 N 0.4008(4) 0.3288(3) 0.2291(3) 0.0242(10) Uani 1 1 d . . . . .
N2 N 0.3990(3) 0.3820(3) 0.3045(3) 0.0248(10) Uani 1 1 d . . . . .
N3 N 0.5931(3) 0.2906(3) 0.0731(3) 0.0230(10) Uani 1 1 d . . . . .
N4 N 0.5946(4) 0.3143(3) 0.0116(3) 0.0277(11) Uani 1 1 d . . . . .
O1 O 0.4767(3) 0.4323(3) 0.3315(2) 0.0276(9) Uani 1 1 d . . . . .
O2 O 0.5246(3) 0.3599(3) 0.0058(3) 0.0301(9) Uani 1 1 d . . . . .
C1 C 0.2875(4) 0.2483(3) 0.1187(4) 0.0249(12) Uani 1 1 d . . . . .
C2 C 0.3127(4) 0.2742(3) 0.2018(3) 0.0231(12) Uani 1 1 d . . . . .
C3 C 0.2553(4) 0.2468(4) 0.2503(4) 0.0291(13) Uani 1 1 d . . . . .
H3 H 0.272671 0.265690 0.306315 0.035 Uiso 1 1 calc R . . . .
C4 C 0.1722(5) 0.1914(4) 0.2160(4) 0.0321(14) Uani 1 1 d . . . . .
C5 C 0.1478(4) 0.1643(4) 0.1342(4) 0.0321(14) Uani 1 1 d . . . . .
H5 H 0.091617 0.125834 0.110826 0.039 Uiso 1 1 calc R . . . .
C6 C 0.2049(5) 0.1929(4) 0.0851(4) 0.0333(15) Uani 1 1 d . . . . .
H6 H 0.186830 0.174348 0.029165 0.040 Uiso 1 1 calc R . . . .
C7 C 0.1121(5) 0.1592(5) 0.2657(5) 0.0409(17) Uani 1 1 d . . . . .
F1 F 0.1392(5) 0.0854(3) 0.2659(4) 0.075(2) Uani 0.835(6) 1 d D . . A 1
F2 F 0.1225(5) 0.2099(4) 0.3454(3) 0.074(2) Uani 0.835(6) 1 d D . . A 1
F3 F 0.0144(4) 0.1558(6) 0.2493(5) 0.086(2) Uani 0.835(6) 1 d D U . A 1
F1' F 0.054(3) 0.0907(16) 0.2159(17) 0.075(2) Uani 0.165(6) 1 d D . . A 2
F2' F 0.155(2) 0.153(2) 0.3190(18) 0.074(2) Uani 0.165(6) 1 d D . . A 2
F3' F 0.040(2) 0.218(2) 0.297(2) 0.086(2) Uani 0.165(6) 1 d D . . A 2
C8 C 0.6967(4) 0.2402(4) 0.1541(4) 0.0277(13) Uani 1 1 d . . . . .
C9 C 0.6771(4) 0.2423(3) 0.0791(4) 0.0243(12) Uani 1 1 d . . . . .
C10 C 0.7374(4) 0.2003(4) 0.0157(4) 0.0271(13) Uani 1 1 d . . . . .
H10 H 0.723939 0.202673 -0.035618 0.032 Uiso 1 1 calc R . . . .
C11 C 0.8173(4) 0.1551(4) 0.0284(4) 0.0298(13) Uani 1 1 d . . . . .
C12 C 0.8368(4) 0.1510(4) 0.1033(4) 0.0353(16) Uani 1 1 d . . . . .
H12 H 0.891440 0.119702 0.111577 0.042 Uiso 1 1 calc R . . . .
C13 C 0.7761(5) 0.1928(4) 0.1658(4) 0.0330(14) Uani 1 1 d . . . . .
H13 H 0.788422 0.189221 0.216686 0.040 Uiso 1 1 calc R . . . .
C14 C 0.8837(5) 0.1137(4) -0.0378(5) 0.0408(17) Uani 1 1 d . . . . .
F4 F 0.9378(4) 0.0526(3) -0.0301(3) 0.0671(13) Uani 1 1 d . . . . .
F5 F 0.8406(4) 0.0831(5) -0.1089(3) 0.100(2) Uani 1 1 d . . . . .
F6 F 0.9551(5) 0.1706(3) -0.0397(4) 0.102(2) Uani 1 1 d . . . . .
N5 N -0.5434(3) 0.4144(3) 0.8004(3) 0.0201(10) Uani 1 1 d . . . . .
C15 C -0.6356(4) 0.4312(4) 0.9267(4) 0.0317(14) Uani 1 1 d . . . . .
H15A H -0.668653 0.397385 0.952736 0.048 Uiso 1 1 calc R . . . .
H15B H -0.579583 0.465959 0.962136 0.048 Uiso 1 1 calc R . . . .
H15C H -0.683544 0.469287 0.916142 0.048 Uiso 1 1 calc R . . . .
C16 C -0.5967(4) 0.3710(4) 0.8478(3) 0.0252(12) Uani 1 1 d . . . . .
H16A H -0.550117 0.331818 0.859308 0.030 Uiso 1 1 calc R . . . .
H16B H -0.653817 0.335138 0.813429 0.030 Uiso 1 1 calc R . . . .
C17 C -0.7048(4) 0.4589(4) 0.7488(4) 0.0301(13) Uani 1 1 d . . . . .
H17A H -0.738197 0.509083 0.746222 0.045 Uiso 1 1 calc R . . . .
H17B H -0.696946 0.416741 0.694057 0.045 Uiso 1 1 calc R . . . .
H17C H -0.745200 0.432731 0.777903 0.045 Uiso 1 1 calc R . . . .
C18 C -0.6042(4) 0.4868(4) 0.7919(4) 0.0248(12) Uani 1 1 d . . . . .
H18A H -0.613175 0.530733 0.846494 0.030 Uiso 1 1 calc R . . . .
H18B H -0.565022 0.514777 0.762824 0.030 Uiso 1 1 calc R . . . .
C19 C -0.4652(5) 0.3727(4) 0.6646(4) 0.0349(15) Uani 1 1 d . . . . .
H19A H -0.459463 0.323655 0.613384 0.052 Uiso 1 1 calc R . . . .
H19B H -0.497044 0.419696 0.654582 0.052 Uiso 1 1 calc R . . . .
H19C H -0.398383 0.392439 0.690818 0.052 Uiso 1 1 calc R . . . .
C20 C -0.5277(4) 0.3455(4) 0.7187(3) 0.0260(12) Uani 1 1 d . . . . .
H20A H -0.495585 0.296777 0.726694 0.031 Uiso 1 1 calc R . . . .
H20B H -0.593976 0.323959 0.690557 0.031 Uiso 1 1 calc R . . . .
C21 C -0.3697(5) 0.3958(4) 0.8542(4) 0.0349(15) Uani 1 1 d . . . . .
H21A H -0.308251 0.428004 0.882600 0.052 Uiso 1 1 calc R . . . .
H21B H -0.398249 0.365534 0.885450 0.052 Uiso 1 1 calc R . . . .
H21C H -0.354229 0.353863 0.801052 0.052 Uiso 1 1 calc R . . . .
C22 C -0.4448(4) 0.4581(4) 0.8440(4) 0.0286(13) Uani 1 1 d . . . . .
H22A H -0.458593 0.501109 0.897937 0.034 Uiso 1 1 calc R . . . .
H22B H -0.414617 0.489450 0.813626 0.034 Uiso 1 1 calc R . . . .
N6 N 0.2515(4) 0.5475(3) 0.5169(3) 0.0241(8) Uani 1 1 d . . . . .
C23 C 0.1182(4) 0.4271(4) 0.4467(4) 0.0317(14) Uani 1 1 d . . . . .
H23A H 0.082901 0.394795 0.394367 0.048 Uiso 1 1 calc R . . . .
H23B H 0.154700 0.387168 0.464579 0.048 Uiso 1 1 calc R . . . .
H23C H 0.069819 0.456718 0.486284 0.048 Uiso 1 1 calc R . . . .
C24 C 0.1911(4) 0.4925(4) 0.4389(3) 0.0247(12) Uani 1 1 d . . . . .
H24A H 0.153523 0.531199 0.419322 0.030 Uiso 1 1 calc R . . . .
H24B H 0.238242 0.461781 0.397659 0.030 Uiso 1 1 calc R . . . .
C25 C 0.1293(4) 0.6704(4) 0.5617(4) 0.0306(14) Uani 1 1 d . . . . .
H25A H 0.088281 0.702622 0.606378 0.046 Uiso 1 1 calc R . . . .
H25B H 0.177875 0.710138 0.553540 0.046 Uiso 1 1 calc R . . . .
H25C H 0.086239 0.642364 0.512466 0.046 Uiso 1 1 calc R . . . .
C26 C 0.1841(4) 0.6030(4) 0.5814(4) 0.0277(13) Uani 1 1 d . . . . .
H26A H 0.134151 0.564569 0.591219 0.033 Uiso 1 1 calc R . . . .
H26B H 0.225569 0.632182 0.632194 0.033 Uiso 1 1 calc R . . . .
C27 C 0.3879(4) 0.6668(4) 0.5612(4) 0.0338(15) Uani 1 1 d . . . . .
H27A H 0.433235 0.697822 0.539710 0.051 Uiso 1 1 calc R . . . .
H27B H 0.344172 0.707621 0.598326 0.051 Uiso 1 1 calc R . . . .
H27C H 0.426980 0.638056 0.590103 0.051 Uiso 1 1 calc R . . . .
C28 C 0.3249(4) 0.6002(4) 0.4926(4) 0.0274(13) Uani 1 1 d . . . . .
H28A H 0.287554 0.630036 0.463022 0.033 Uiso 1 1 calc R . . . .
H28B H 0.370168 0.560633 0.454819 0.033 Uiso 1 1 calc R . . . .
C29 C 0.3704(5) 0.4243(4) 0.4990(4) 0.0324(14) Uani 1 1 d . . . . .
H29A H 0.400800 0.392162 0.528727 0.049 Uiso 1 1 calc R . . . .
H29B H 0.329864 0.384595 0.452145 0.049 Uiso 1 1 calc R . . . .
H29C H 0.423053 0.452614 0.480969 0.049 Uiso 1 1 calc R . . . .
C30 C 0.3044(4) 0.4918(4) 0.5535(4) 0.0292(13) Uani 1 1 d . . . . .
H30A H 0.346178 0.529924 0.601394 0.035 Uiso 1 1 calc R . . . .
H30B H 0.253284 0.462120 0.572662 0.035 Uiso 1 1 calc R . . . .
Ni2 Ni -0.00891(5) 0.30588(5) 0.70852(4) 0.02200(18) Uani 1 1 d . . . . .
S3 S -0.13720(10) 0.30349(10) 0.62638(9) 0.0258(3) Uani 1 1 d . . . . .
S4 S 0.11830(12) 0.27370(10) 0.77232(9) 0.0307(3) Uani 1 1 d . . . . .
N7 N -0.1051(4) 0.2857(3) 0.7739(3) 0.0264(11) Uani 1 1 d . . . . .
N8 N -0.1033(4) 0.3090(3) 0.8524(3) 0.0296(11) Uani 1 1 d . . . . .
N9 N 0.0873(3) 0.3209(3) 0.6402(3) 0.0245(10) Uani 1 1 d . . . . .
N10 N 0.0931(4) 0.3757(3) 0.6060(3) 0.0267(11) Uani 1 1 d . . . . .
O3 O -0.0256(3) 0.3523(3) 0.8899(2) 0.0336(10) Uani 1 1 d . . . . .
O4 O 0.0229(3) 0.4273(3) 0.6177(2) 0.0281(9) Uani 1 1 d . . . . .
C31 C -0.2201(4) 0.2445(4) 0.6603(3) 0.0238(12) Uani 1 1 d . . . . .
C32 C -0.1957(4) 0.2408(4) 0.7353(4) 0.0246(12) Uani 1 1 d . . . . .
C33 C -0.2579(5) 0.1962(4) 0.7662(4) 0.0298(13) Uani 1 1 d . . . . .
H33 H -0.241082 0.194042 0.817143 0.036 Uiso 1 1 calc R . . . .
C34 C -0.3450(5) 0.1545(4) 0.7223(4) 0.0317(14) Uani 1 1 d . . . . .
C35 C -0.3696(4) 0.1570(4) 0.6475(4) 0.0347(16) Uani 1 1 d . . . . .
H35 H -0.428647 0.127635 0.617183 0.042 Uiso 1 1 calc R . . . .
C36 C -0.3077(4) 0.2022(4) 0.6178(4) 0.0316(14) Uani 1 1 d . . . . .
H36 H -0.325198 0.204626 0.567061 0.038 Uiso 1 1 calc R . . . .
C37 C -0.4123(5) 0.1082(5) 0.7550(5) 0.0472(19) Uani 1 1 d . . . . .
F7 F -0.4076(8) 0.1384(7) 0.8362(6) 0.0699(13) Uani 0.528(6) 1 d D . . B 1
F8 F -0.5054(7) 0.1047(7) 0.7322(7) 0.0699(13) Uani 0.528(6) 1 d D . . B 1
F9 F -0.3868(7) 0.0246(6) 0.7337(6) 0.0699(13) Uani 0.528(6) 1 d D . . B 1
F7' F -0.3798(9) 0.1003(8) 0.8217(8) 0.0699(13) Uani 0.472(6) 1 d D . . B 2
F8' F -0.5027(8) 0.1548(8) 0.7802(7) 0.0699(13) Uani 0.472(6) 1 d D . . B 2
F9' F -0.4604(9) 0.0393(7) 0.7022(7) 0.0699(13) Uani 0.472(6) 1 d D . . B 2
C38 C 0.1905(4) 0.2361(4) 0.6880(4) 0.0274(13) Uani 1 1 d . . . . .
C39 C 0.1703(4) 0.2664(4) 0.6265(4) 0.0258(12) Uani 1 1 d . . . . .
C40 C 0.2248(4) 0.2415(4) 0.5589(4) 0.0281(13) Uani 1 1 d . . . . .
H40 H 0.210428 0.263114 0.518268 0.034 Uiso 1 1 calc R . . . .
C41 C 0.3015(5) 0.1841(4) 0.5505(4) 0.0344(15) Uani 1 1 d . . . . .
C42 C 0.3227(5) 0.1523(4) 0.6098(4) 0.0380(16) Uani 1 1 d . . . . .
H42 H 0.374481 0.113003 0.603834 0.046 Uiso 1 1 calc R . . . .
C43 C 0.2668(5) 0.1788(4) 0.6785(4) 0.0342(15) Uani 1 1 d . . . . .
H43 H 0.281198 0.157273 0.719156 0.041 Uiso 1 1 calc R . . . .
C44 C 0.3594(5) 0.1566(5) 0.4780(5) 0.0434(17) Uani 1 1 d . . . . .
F10 F 0.3235(7) 0.1702(10) 0.4170(5) 0.113(6) Uani 0.693(8) 1 d D . . C 1
F11 F 0.3931(9) 0.0760(5) 0.4571(6) 0.098(4) Uani 0.693(8) 1 d D . . C 1
F12 F 0.4511(5) 0.1968(6) 0.4931(5) 0.082(3) Uani 0.693(8) 1 d D . . C 1
F10' F 0.3703(15) 0.2122(12) 0.4466(14) 0.082(3) Uani 0.307(8) 1 d D . . C 2
F11' F 0.3182(13) 0.0830(11) 0.4197(9) 0.061(5) Uani 0.307(8) 1 d D . . C 2
F12' F 0.4447(18) 0.1313(14) 0.4882(12) 0.098(4) Uani 0.307(8) 1 d D . . C 2
N11 N 0.0331(3) 0.4209(3) 1.1399(3) 0.0204(10) Uani 1 1 d . . . . .
C45 C -0.1412(4) 0.4034(4) 1.0698(4) 0.0278(13) Uani 1 1 d . . . . .
H45A H -0.199050 0.436194 1.065082 0.042 Uiso 1 1 calc R . . . .
H45B H -0.114464 0.374663 1.016695 0.042 Uiso 1 1 calc R . . . .
H45C H -0.161901 0.360102 1.090461 0.042 Uiso 1 1 calc R . . . .
C46 C -0.0621(4) 0.4634(4) 1.1266(4) 0.0251(12) Uani 1 1 d . . . . .
H46A H -0.090991 0.493258 1.179415 0.030 Uiso 1 1 calc R . . . .
H46B H -0.043664 0.507785 1.105819 0.030 Uiso 1 1 calc R . . . .
C47 C -0.0525(5) 0.3743(4) 1.2410(4) 0.0325(14) Uani 1 1 d . . . . .
H47A H -0.067976 0.324486 1.254289 0.049 Uiso 1 1 calc R . . . .
H47B H -0.012023 0.417458 1.285727 0.049 Uiso 1 1 calc R . . . .
H47C H -0.114807 0.399494 1.231820 0.049 Uiso 1 1 calc R . . . .
C48 C 0.0048(5) 0.3462(4) 1.1662(4) 0.0307(14) Uani 1 1 d D . . . .
H48A H -0.035978 0.301573 1.121760 0.037 Uiso 1 1 calc R . . . .
H48B H 0.066715 0.319520 1.175618 0.037 Uiso 1 1 calc R . . . .
C49 C 0.1984(4) 0.4638(4) 1.2245(4) 0.0310(14) Uani 1 1 d . . . . .
H49A H 0.235494 0.514069 1.264542 0.047 Uiso 1 1 calc R . . . .
H49B H 0.187025 0.420568 1.247362 0.047 Uiso 1 1 calc R . . . .
H49C H 0.237074 0.439192 1.176579 0.047 Uiso 1 1 calc R . . . .
C50 C 0.0991(4) 0.4911(4) 1.2012(3) 0.0245(12) Uani 1 1 d . . . . .
H50A H 0.062048 0.517615 1.250592 0.029 Uiso 1 1 calc R . . . .
H50B H 0.111957 0.536187 1.180007 0.029 Uiso 1 1 calc R . . . .
C51 C 0.1280(4) 0.4405(4) 1.0283(4) 0.0283(13) Uani 1 1 d . . . . .
H51A H 0.159517 0.408334 0.977989 0.042 Uiso 1 1 calc R . . . .
H51B H 0.074608 0.474409 1.017995 0.042 Uiso 1 1 calc R . . . .
H51C H 0.178221 0.479202 1.067786 0.042 Uiso 1 1 calc R . . . .
C52 C 0.0850(4) 0.3789(4) 1.0607(3) 0.0240(12) Uani 1 1 d . . . . .
H52A H 0.139436 0.343950 1.069290 0.029 Uiso 1 1 calc R . . . .
H52B H 0.036040 0.339168 1.019602 0.029 Uiso 1 1 calc R . . . .
N12 N -0.500000 0.000000 1.000000 0.0342(17) Uani 1 2 d DS T P . .
C53 C -0.6188(6) 0.0575(6) 0.9194(5) 0.065(2) Uani 1 1 d . . . . .
H53A H -0.637688 0.101823 0.899484 0.097 Uiso 1 1 calc R . . . .
H53B H -0.610366 0.003057 0.873685 0.097 Uiso 1 1 calc R . . . .
H53C H -0.671311 0.049468 0.952218 0.097 Uiso 1 1 calc R . . . .
C54 C -0.5176(13) 0.0864(9) 0.9723(10) 0.065(2) Uani 0.5 1 d D . . . .
C55 C -0.4093(11) -0.0611(7) 0.8735(8) 0.120(5) Uani 1 1 d D . . . .
H55A H -0.358794 -0.065903 0.834624 0.180 Uiso 1 1 calc R . . . .
H55B H -0.407138 -0.110907 0.888736 0.180 Uiso 1 1 calc R . . . .
H55C H -0.475765 -0.059323 0.849188 0.180 Uiso 1 1 calc R . . . .
C56 C -0.3879(16) 0.0213(12) 0.9483(12) 0.120(5) Uani 0.5 1 d D . . . .
N13 N 0.000000 0.000000 0.500000 0.0361(17) Uani 1 2 d DS T P . .
C59 C -0.0361(10) 0.1221(6) 0.4529(7) 0.097(4) Uani 1 1 d D . . . .
C60 C 0.0253(15) 0.0962(9) 0.5165(16) 0.090(5) Uani 0.5 1 d D . . . .
C61 C -0.0631(19) 0.0285(13) 0.4413(16) 0.122(11) Uani 0.5 1 d D . . . .
C62 C 0.1310(12) -0.0340(8) 0.3960(9) 0.150(7) Uani 1 1 d D . . . .
C63 C 0.1125(11) 0.0110(10) 0.4872(11) 0.090(5) Uani 0.5 1 d D . . . .
C64 C 0.0227(17) -0.0581(13) 0.4102(12) 0.150(7) Uani 0.5 1 d D . . . .
O5 O 1.2183(10) -0.0220(7) -0.2886(9) 0.184(6) Uani 1 1 d D . . . .
C65 C 1.0787(13) 0.0711(10) -0.1888(14) 0.192(10) Uani 1 1 d D . . . .
H65A H 1.071680 0.074591 -0.133808 0.288 Uiso 1 1 calc R . . . .
H65B H 1.092824 0.128928 -0.187533 0.288 Uiso 1 1 calc R . . . .
H65C H 1.016374 0.046902 -0.221310 0.288 Uiso 1 1 calc R . . . .
C66 C 1.1664(11) 0.0120(12) -0.2267(7) 0.137(6) Uani 1 1 d D . . . .
H66A H 1.220589 0.039933 -0.184744 0.165 Uiso 1 1 calc R . . . .
H66B H 1.145954 -0.040144 -0.217720 0.165 Uiso 1 1 calc R . . . .
C67 C 1.3089(12) -0.0714(11) -0.3074(11) 0.223(9) Uani 1 1 d D . . . .
H67A H 1.296538 -0.128007 -0.303980 0.268 Uiso 1 1 calc R . . . .
H67B H 1.363760 -0.040241 -0.267225 0.268 Uiso 1 1 calc R . . . .
C68 C 1.3416(14) -0.0859(12) -0.3958(11) 0.223(9) Uani 1 1 d D . . . .
H68A H 1.402317 -0.119099 -0.406871 0.335 Uiso 1 1 calc R . . . .
H68B H 1.287774 -0.117622 -0.435635 0.335 Uiso 1 1 calc R . . . .
H68C H 1.354920 -0.029954 -0.398922 0.335 Uiso 1 1 calc R . . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
S2 Ni1 S1 164.30(7) . .
N1 Ni1 S1 85.10(15) . .
N1 Ni1 S2 93.39(15) . .
N1 Ni1 N3 178.5(2) . .
N3 Ni1 S1 94.89(14) . .
N3 Ni1 S2 86.20(14) . .
C1 S1 Ni1 94.1(2) . .
C8 S2 Ni1 96.6(2) . .
N2 N1 Ni1 132.4(4) . .
N2 N1 C2 112.5(5) . .
C2 N1 Ni1 115.2(4) . .
O1 N2 N1 114.6(4) . .
N4 N3 Ni1 129.3(4) . .
N4 N3 C9 113.2(5) . .
C9 N3 Ni1 117.5(4) . .
O2 N4 N3 115.5(5) . .
C2 C1 S1 116.8(4) . .
C6 C1 S1 124.4(5) . .
C6 C1 C2 118.8(6) . .
C1 C2 N1 113.8(5) . .
C3 C2 N1 124.8(5) . .
C3 C2 C1 121.4(5) . .
C2 C3 C4 119.4(6) . .
C3 C4 C7 120.4(6) . .
C5 C4 C3 119.7(6) . .
C5 C4 C7 119.9(6) . .
C4 C5 C6 121.1(6) . .
C1 C6 C5 119.7(6) . .
F1 C7 C4 114.1(6) . .
F1 C7 F2 101.2(7) . .
F1 C7 F3 109.5(7) . .
F2 C7 C4 113.1(6) . .
F3 C7 C4 114.4(6) . .
F3 C7 F2 103.3(7) . .
F1' C7 C4 108.4(13) . .
F1' C7 F3' 100.4(18) . .
F2' C7 C4 115.0(15) . .
F2' C7 F1' 118.1(19) . .
F2' C7 F3' 106(2) . .
F3' C7 C4 107.1(14) . .
C9 C8 S2 117.6(5) . .
C9 C8 C13 119.5(6) . .
C13 C8 S2 122.9(5) . .
C8 C9 N3 115.0(5) . .
C8 C9 C10 120.8(6) . .
C10 C9 N3 124.1(5) . .
C11 C10 C9 119.2(6) . .
C10 C11 C12 120.6(6) . .
C10 C11 C14 119.1(6) . .
C12 C11 C14 120.3(6) . .
C13 C12 C11 119.7(6) . .
C12 C13 C8 120.2(6) . .
F4 C14 C11 115.0(6) . .
F4 C14 F6 101.8(6) . .
F5 C14 C11 115.4(6) . .
F5 C14 F4 107.4(6) . .
F5 C14 F6 105.1(7) . .
F6 C14 C11 110.8(6) . .
C16 N5 C18 111.6(4) . .
C16 N5 C22 111.0(4) . .
C20 N5 C16 106.9(4) . .
C20 N5 C18 110.7(4) . .
C20 N5 C22 111.7(4) . .
C22 N5 C18 105.0(4) . .
N5 C16 C15 115.5(5) . .
C17 C18 N5 115.0(5) . .
C19 C20 N5 115.8(5) . .
N5 C22 C21 113.7(5) . .
C26 N6 C24 111.7(5) . .
C28 N6 C24 105.0(4) . .
C28 N6 C26 112.7(4) . .
C28 N6 C30 111.2(5) . .
C30 N6 C24 111.2(4) . .
C30 N6 C26 105.2(4) . .
C23 C24 N6 114.8(5) . .
C25 C26 N6 115.3(5) . .
N6 C28 C27 115.3(5) . .
C29 C30 N6 116.3(5) . .
S4 Ni2 S3 165.76(7) . .
N7 Ni2 S3 85.93(15) . .
N7 Ni2 S4 93.88(16) . .
N7 Ni2 N9 177.5(2) . .
N9 Ni2 S3 93.73(15) . .
N9 Ni2 S4 85.85(15) . .
C31 S3 Ni2 96.2(2) . .
C38 S4 Ni2 94.6(2) . .
N8 N7 Ni2 130.2(4) . .
N8 N7 C32 112.0(5) . .
C32 N7 Ni2 117.7(4) . .
O3 N8 N7 114.5(5) . .
N10 N9 Ni2 130.8(4) . .
N10 N9 C39 113.1(5) . .
C39 N9 Ni2 116.0(4) . .
O4 N10 N9 116.0(5) . .
C32 C31 S3 117.3(4) . .
C36 C31 S3 124.1(5) . .
C36 C31 C32 118.6(5) . .
C31 C32 N7 114.4(5) . .
C33 C32 N7 125.1(5) . .
C33 C32 C31 120.5(5) . .
C32 C33 C34 119.7(6) . .
C33 C34 C35 120.4(6) . .
C33 C34 C37 120.1(6) . .
C35 C34 C37 119.5(6) . .
C36 C35 C34 119.4(6) . .
C35 C36 C31 121.4(6) . .
F7 C37 C34 114.2(7) . .
F7 C37 F9 102.8(8) . .
F8 C37 C34 115.5(7) . .
F8 C37 F7 106.6(9) . .
F8 C37 F9 105.5(8) . .
F9 C37 C34 111.2(7) . .
F7' C37 C34 116.5(7) . .
F7' C37 F8' 101.4(9) . .
F7' C37 F9' 114.5(9) . .
F8' C37 C34 110.8(7) . .
F9' C37 C34 116.1(7) . .
F9' C37 F8' 93.9(8) . .
C39 C38 S4 117.7(5) . .
C43 C38 S4 124.0(5) . .
C43 C38 C39 118.3(6) . .
C38 C39 N9 113.6(5) . .
C40 C39 N9 124.8(5) . .
C40 C39 C38 121.5(6) . .
C39 C40 C41 119.4(6) . .
C40 C41 C44 119.6(6) . .
C42 C41 C40 120.4(6) . .
C42 C41 C44 120.0(6) . .
C41 C42 C43 119.4(6) . .
C38 C43 C42 121.0(6) . .
F10 C44 C41 117.9(6) . .
F10 C44 F11 112.4(9) . .
F10 C44 F12 103.4(9) . .
F11 C44 C41 113.0(7) . .
F12 C44 C41 111.8(6) . .
F12 C44 F11 95.6(8) . .
F10' C44 C41 115.6(10) . .
F10' C44 F11' 107.9(13) . .
F11' C44 C41 111.1(9) . .
F12' C44 C41 113.6(11) . .
F12' C44 F10' 107.6(14) . .
F12' C44 F11' 99.9(13) . .
C46 N11 C48 109.2(4) . .
C46 N11 C52 110.6(4) . .
C50 N11 C46 106.4(4) . .
C50 N11 C48 113.9(4) . .
C50 N11 C52 111.0(4) . .
C52 N11 C48 105.8(4) . .
C45 C46 N11 115.3(5) . .
C47 C48 N11 113.5(5) . .
N11 C50 C49 115.9(5) . .
C51 C52 N11 115.0(5) . .
C54 N12 C54 180.0(3) 2_457 .
C54 N12 C56 68.4(8) . .
C54 N12 C56 111.6(8) . 2_457
C54 N12 C56 68.4(8) 2_457 2_457
C54 N12 C56 111.6(8) 2_457 .
C56 N12 C56 180.0(11) . 2_457
C53 C54 N12 101.1(9) . .
C55 C56 N12 92.8(12) . .
C60 N13 C60 180(2) 2_556 .
C60 N13 C63 109.2(10) 2_556 .
C60 N13 C63 109.2(10) . 2_556
C60 N13 C63 70.8(10) . .
C60 N13 C63 70.8(10) 2_556 2_556
C60 N13 C64 70.6(12) 2_556 .
C60 N13 C64 109.4(12) . .
C60 N13 C64 109.4(12) 2_556 2_556
C60 N13 C64 70.6(12) . 2_556
C61 N13 C60 110.4(11) . 2_556
C61 N13 C60 69.6(11) 2_556 2_556
C61 N13 C60 110.4(11) 2_556 .
C61 N13 C60 69.6(11) . .
C61 N13 C61 180.0(14) 2_556 .
C61 N13 C63 71.3(13) . 2_556
C61 N13 C63 71.3(13) 2_556 .
C61 N13 C63 108.7(13) 2_556 2_556
C61 N13 C63 108.7(13) . .
C61 N13 C64 70.5(15) 2_556 2_556
C61 N13 C64 70.5(15) . .
C61 N13 C64 109.5(15) . 2_556
C61 N13 C64 109.5(15) 2_556 .
C63 N13 C63 180.0 . 2_556
C64 N13 C63 109.6(10) . 2_556
C64 N13 C63 70.4(10) . .
C64 N13 C63 109.6(10) 2_556 .
C64 N13 C63 70.4(10) 2_556 2_556
C64 N13 C64 180.0(9) . 2_556
N13 C60 C59 109.3(13) . .
N13 C61 C64 55.7(9) . .
N13 C63 C64 55.6(6) . .
C62 C63 N13 109.5(11) . .
C62 C63 C64 54.6(8) . .
N13 C64 C61 53.9(8) . .
N13 C64 C63 54.1(7) . .
C63 C64 C61 88.4(10) . .
C66 O5 C67 136.6(17) . .
O5 C66 C65 147.0(16) . .
O5 C67 C68 111.1(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S1 2.2211(16) .
Ni1 S2 2.1991(16) .
Ni1 N1 1.885(5) .
Ni1 N3 1.899(5) .
S1 C1 1.754(6) .
S2 C8 1.753(6) .
N1 N2 1.309(7) .
N1 C2 1.426(7) .
N2 O1 1.279(6) .
N3 N4 1.317(7) .
N3 C9 1.426(7) .
N4 O2 1.251(6) .
C1 C2 1.409(8) .
C1 C6 1.386(8) .
C2 C3 1.390(8) .
C3 C4 1.393(9) .
C4 C5 1.384(9) .
C4 C7 1.474(9) .
C5 C6 1.408(9) .
C7 F1 1.305(8) .
C7 F2 1.355(10) .
C7 F3 1.324(8) .
C7 F1' 1.35(3) .
C7 F2' 1.14(3) .
C7 F3' 1.38(3) .
C8 C9 1.380(9) .
C8 C13 1.399(9) .
C9 C10 1.395(8) .
C10 C11 1.388(8) .
C11 C12 1.391(9) .
C11 C14 1.478(9) .
C12 C13 1.386(9) .
C14 F4 1.317(8) .
C14 F5 1.284(8) .
C14 F6 1.353(8) .
N5 C16 1.516(7) .
N5 C18 1.533(7) .
N5 C20 1.508(7) .
N5 C22 1.522(7) .
C15 C16 1.516(8) .
C17 C18 1.495(8) .
C19 C20 1.506(8) .
C21 C22 1.525(9) .
N6 C24 1.530(7) .
N6 C26 1.528(7) .
N6 C28 1.502(7) .
N6 C30 1.512(7) .
C23 C24 1.509(8) .
C25 C26 1.511(8) .
C27 C28 1.513(8) .
C29 C30 1.515(9) .
Ni2 S3 2.2044(16) .
Ni2 S4 2.2042(17) .
Ni2 N7 1.898(5) .
Ni2 N9 1.903(5) .
S3 C31 1.757(6) .
S4 C38 1.752(6) .
N7 N8 1.312(7) .
N7 C32 1.416(7) .
N8 O3 1.262(6) .
N9 N10 1.297(7) .
N9 C39 1.426(7) .
N10 O4 1.263(6) .
C31 C32 1.401(8) .
C31 C36 1.389(8) .
C32 C33 1.384(8) .
C33 C34 1.389(9) .
C34 C35 1.390(9) .
C34 C37 1.465(9) .
C35 C36 1.375(9) .
C37 F7 1.348(13) .
C37 F8 1.288(12) .
C37 F9 1.364(12) .
C37 F7' 1.314(14) .
C37 F8' 1.451(14) .
C37 F9' 1.314(12) .
C38 C39 1.407(8) .
C38 C43 1.390(9) .
C39 C40 1.377(8) .
C40 C41 1.400(9) .
C41 C42 1.389(10) .
C41 C44 1.472(10) .
C42 C43 1.403(10) .
C44 F10 1.281(11) .
C44 F11 1.356(10) .
C44 F12 1.354(10) .
C44 F10' 1.28(2) .
C44 F11' 1.362(14) .
C44 F12' 1.26(2) .
N11 C46 1.530(7) .
N11 C48 1.554(7) .
N11 C50 1.501(7) .
N11 C52 1.534(7) .
C45 C46 1.498(8) .
C47 C48 1.499(9) .
C49 C50 1.509(8) .
C51 C52 1.493(8) .
N12 C54 1.730(12) 2_457
N12 C54 1.730(12) .
N12 C56 1.90(2) 2_457
N12 C56 1.90(2) .
C53 C54 1.573(18) .
C55 C56 1.523(17) .
N13 C60 1.557(12) .
N13 C60 1.557(12) 2_556
N13 C61 1.547(14) 2_556
N13 C61 1.547(14) .
N13 C63 1.553(13) .
N13 C63 1.553(13) 2_556
N13 C64 1.582(15) .
N13 C64 1.582(15) 2_556
C59 C60 1.58(3) .
C61 C64 1.80(3) .
C62 C63 1.557(16) .
C63 C64 1.81(3) .
O5 C66 1.285(13) .
O5 C67 1.464(15) .
C65 C66 1.561(15) .
C67 C68 1.601(16) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
Ni1 S1 C1 C2 23.7(4) .
Ni1 S1 C1 C6 -155.4(5) .
Ni1 S2 C8 C9 16.6(5) .
Ni1 S2 C8 C13 -162.6(5) .
Ni1 N1 N2 O1 0.4(7) .
Ni1 N1 C2 C1 -29.5(6) .
Ni1 N1 C2 C3 149.9(5) .
Ni1 N3 N4 O2 3.1(7) .
Ni1 N3 C9 C8 -20.4(6) .
Ni1 N3 C9 C10 160.3(4) .
S1 Ni1 N1 N2 -143.4(5) .
S1 Ni1 N1 C2 36.9(4) .
S1 Ni1 N3 N4 40.9(5) .
S1 Ni1 N3 C9 -138.9(4) .
S1 C1 C2 N1 -1.1(6) .
S1 C1 C2 C3 179.5(4) .
S1 C1 C6 C5 179.5(5) .
S2 Ni1 N1 N2 52.3(5) .
S2 Ni1 N1 C2 -127.4(4) .
S2 Ni1 N3 N4 -154.8(5) .
S2 Ni1 N3 C9 25.4(4) .
S2 C8 C9 N3 -0.7(7) .
S2 C8 C9 C10 178.6(4) .
S2 C8 C13 C12 -178.4(5) .
N1 C2 C3 C4 -178.2(5) .
N2 N1 C2 C1 150.7(5) .
N2 N1 C2 C3 -29.9(7) .
N3 C9 C10 C11 -179.9(5) .
N4 N3 C9 C8 159.8(5) .
N4 N3 C9 C10 -19.5(7) .
C1 C2 C3 C4 1.1(8) .
C2 N1 N2 O1 -179.9(4) .
C2 C1 C6 C5 0.4(8) .
C2 C3 C4 C5 0.1(9) .
C2 C3 C4 C7 178.0(5) .
C3 C4 C5 C6 -1.0(9) .
C3 C4 C7 F1 -92.9(8) .
C3 C4 C7 F2 22.1(9) .
C3 C4 C7 F3 140.0(8) .
C3 C4 C7 F1' -163.8(16) .
C3 C4 C7 F2' -29(2) .
C3 C4 C7 F3' 88.6(17) .
C4 C5 C6 C1 0.7(9) .
C5 C4 C7 F1 85.1(8) .
C5 C4 C7 F2 -160.0(6) .
C5 C4 C7 F3 -42.1(10) .
C5 C4 C7 F1' 14.1(17) .
C5 C4 C7 F2' 149(2) .
C5 C4 C7 F3' -93.4(17) .
C6 C1 C2 N1 178.1(5) .
C6 C1 C2 C3 -1.4(8) .
C7 C4 C5 C6 -178.9(6) .
C8 C9 C10 C11 0.8(8) .
C9 N3 N4 O2 -177.1(5) .
C9 C8 C13 C12 2.4(9) .
C9 C10 C11 C12 0.5(9) .
C9 C10 C11 C14 -177.5(5) .
C10 C11 C12 C13 -0.3(9) .
C10 C11 C14 F4 -160.9(6) .
C10 C11 C14 F5 -35.0(9) .
C10 C11 C14 F6 84.4(8) .
C11 C12 C13 C8 -1.2(9) .
C12 C11 C14 F4 21.1(9) .
C12 C11 C14 F5 147.1(7) .
C12 C11 C14 F6 -93.6(8) .
C13 C8 C9 N3 178.4(5) .
C13 C8 C9 C10 -2.2(8) .
C14 C11 C12 C13 177.6(6) .
C16 N5 C18 C17 -60.8(6) .
C16 N5 C20 C19 -173.3(5) .
C16 N5 C22 C21 62.8(6) .
C18 N5 C16 C15 -48.9(6) .
C18 N5 C20 C19 64.9(6) .
C18 N5 C22 C21 -176.4(5) .
C20 N5 C16 C15 -170.0(5) .
C20 N5 C18 C17 58.1(6) .
C20 N5 C22 C21 -56.4(6) .
C22 N5 C16 C15 67.9(6) .
C22 N5 C18 C17 178.9(5) .
C22 N5 C20 C19 -51.7(7) .
C24 N6 C26 C25 -64.4(6) .
C24 N6 C28 C27 174.5(5) .
C24 N6 C30 C29 54.0(7) .
C26 N6 C24 C23 -63.3(6) .
C26 N6 C28 C27 52.8(7) .
C26 N6 C30 C29 175.0(5) .
C28 N6 C24 C23 174.3(5) .
C28 N6 C26 C25 53.5(7) .
C28 N6 C30 C29 -62.7(7) .
C30 N6 C24 C23 53.9(7) .
C30 N6 C26 C25 174.9(5) .
C30 N6 C28 C27 -65.0(6) .
Ni2 S3 C31 C32 17.8(4) .
Ni2 S3 C31 C36 -162.6(5) .
Ni2 S4 C38 C39 23.6(4) .
Ni2 S4 C38 C43 -156.8(5) .
Ni2 N7 N8 O3 0.7(8) .
Ni2 N7 C32 C31 -22.7(6) .
Ni2 N7 C32 C33 157.4(5) .
Ni2 N9 N10 O4 -1.8(7) .
Ni2 N9 C39 C38 -24.4(6) .
Ni2 N9 C39 C40 153.2(5) .
S3 Ni2 N7 N8 -149.9(5) .
S3 Ni2 N7 C32 28.1(4) .
S3 C31 C32 N7 -0.4(7) .
S3 C31 C32 C33 179.5(4) .
S3 C31 C36 C35 179.9(5) .
S4 Ni2 N7 N8 44.4(5) .
S4 Ni2 N7 C32 -137.6(4) .
S4 C38 C39 N9 -3.7(7) .
S4 C38 C39 C40 178.7(4) .
S4 C38 C43 C42 -179.1(5) .
N7 C32 C33 C34 -179.9(6) .
N8 N7 C32 C31 155.6(5) .
N8 N7 C32 C33 -24.3(8) .
N9 C39 C40 C41 -176.7(5) .
N10 N9 C39 C38 152.7(5) .
N10 N9 C39 C40 -29.8(8) .
C31 C32 C33 C34 0.2(9) .
C32 N7 N8 O3 -177.3(5) .
C32 C31 C36 C35 -0.4(9) .
C32 C33 C34 C35 0.4(9) .
C32 C33 C34 C37 -179.0(6) .
C33 C34 C35 C36 -1.0(10) .
C33 C34 C37 F7 26.6(11) .
C33 C34 C37 F8 150.7(8) .
C33 C34 C37 F9 -89.2(9) .
C33 C34 C37 F7' -7.7(12) .
C33 C34 C37 F8' 107.5(8) .
C33 C34 C37 F9' -147.1(9) .
C34 C35 C36 C31 1.0(10) .
C35 C34 C37 F7 -152.8(8) .
C35 C34 C37 F8 -28.7(11) .
C35 C34 C37 F9 91.5(9) .
C35 C34 C37 F7' 172.9(9) .
C35 C34 C37 F8' -71.9(9) .
C35 C34 C37 F9' 33.6(12) .
C36 C31 C32 N7 179.9(5) .
C36 C31 C32 C33 -0.2(8) .
C37 C34 C35 C36 178.4(7) .
C38 C39 C40 C41 0.7(8) .
C39 N9 N10 O4 -178.3(5) .
C39 C38 C43 C42 0.5(9) .
C39 C40 C41 C42 0.0(9) .
C39 C40 C41 C44 179.4(6) .
C40 C41 C42 C43 -0.4(9) .
C40 C41 C44 F10 -15.7(13) .
C40 C41 C44 F11 -149.5(9) .
C40 C41 C44 F12 103.9(8) .
C40 C41 C44 F10' 31.5(14) .
C40 C41 C44 F11' -91.8(12) .
C40 C41 C44 F12' 156.5(13) .
C41 C42 C43 C38 0.2(9) .
C42 C41 C44 F10 163.7(11) .
C42 C41 C44 F11 29.8(11) .
C42 C41 C44 F12 -76.7(9) .
C42 C41 C44 F10' -149.2(13) .
C42 C41 C44 F11' 87.5(13) .
C42 C41 C44 F12' -24.1(15) .
C43 C38 C39 N9 176.7(5) .
C43 C38 C39 C40 -0.9(8) .
C44 C41 C42 C43 -179.8(6) .
C46 N11 C48 C47 -57.7(6) .
C46 N11 C50 C49 179.7(5) .
C46 N11 C52 C51 67.6(6) .
C48 N11 C46 C45 -53.8(6) .
C48 N11 C50 C49 59.3(6) .
C48 N11 C52 C51 -174.2(5) .
C50 N11 C46 C45 -177.2(5) .
C50 N11 C48 C47 61.1(6) .
C50 N11 C52 C51 -50.2(6) .
C52 N11 C46 C45 62.2(6) .
C52 N11 C48 C47 -176.8(5) .
C52 N11 C50 C49 -59.9(6) .
C56 N12 C54 C53 -55.6(12) 2_457
C56 N12 C54 C53 124.4(12) .
N13 C61 C64 C63 -45.0(9) .
N13 C63 C64 C61 44.9(10) .
C60 N13 C61 C64 120.5(14) .
C60 N13 C61 C64 -59.5(14) 2_556
C60 N13 C63 C62 -110.6(16) .
C60 N13 C63 C62 69.4(16) 2_556
C60 N13 C63 C64 60.2(15) 2_556
C60 N13 C63 C64 -119.8(15) .
C60 N13 C64 C61 -58.9(13) .
C60 N13 C64 C61 121.1(13) 2_556
C60 N13 C64 C63 -119.7(13) 2_556
C60 N13 C64 C63 60.3(13) .
C61 N13 C60 C59 177.1(17) 2_556
C61 N13 C60 C59 -2.9(17) .
C61 N13 C63 C62 128.9(15) 2_556
C61 N13 C63 C62 -51.1(15) .
C61 N13 C63 C64 -60.3(14) .
C61 N13 C63 C64 119.7(14) 2_556
C61 N13 C64 C61 180.000(8) 2_556
C61 N13 C64 C63 -60.8(12) 2_556
C61 N13 C64 C63 119.2(12) .
C62 C63 C64 N13 -169.3(15) .
C62 C63 C64 C61 -124.4(16) .
C63 N13 C60 C59 116.5(17) .
C63 N13 C60 C59 -63.5(17) 2_556
C63 N13 C61 C64 -119.8(11) 2_556
C63 N13 C61 C64 60.2(11) .
C63 N13 C64 C61 60.8(12) 2_556
C63 N13 C64 C61 -119.2(12) .
C63 N13 C64 C63 180.000(3) 2_556
C64 N13 C60 C59 -123.5(17) 2_556
C64 N13 C60 C59 56.5(17) .
C64 N13 C61 C64 180.000(4) 2_556
C64 N13 C63 C62 -170.8(13) 2_556
C64 N13 C63 C62 9.2(13) .
C64 N13 C63 C64 180.000(2) 2_556
C66 O5 C67 C68 -173.6(18) .
C67 O5 C66 C65 172(2) .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5089(14)
2 0.4911(14)
