#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:37:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179193 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/34/4313444.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_4313444
loop_
_publ_author_name
'John F. Berry'
'F. Albert Cotton'
'Lee M. Daniels'
'Carlos A. Murillo'
'Xiaoping Wang'
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, PO Box  30012
   College Station, TX 77842-3012, USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(979) 845 9351'
_publ_contact_author_name        'F. A. Cotton'
_publ_contact_author_phone       '(979) 845 4432'
_publ_section_title
;
 Oxidation of Ni3(dpa)4Cl2 and Cu3(dpa)4Cl2: Nickel-Nickel Bonding
 Interaction, but No Copper-Copper Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2418
_journal_page_last               2427
_journal_paper_doi               10.1021/ic0262740
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C45 H42 Cl10 F18 N12 Ni3 P3'
_chemical_formula_weight         1716.45
_chemical_name_common            'Ni3(C10H8N3)4(PF6)3 (CH2Cl2)5'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.509(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.072(2)
_cell_length_b                   11.8337(11)
_cell_length_c                   25.771(2)
_cell_measurement_reflns_used    7073
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.7
_cell_measurement_theta_min      4.9
_cell_volume                     6546.2(10)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32830
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.431
_exptl_absorpt_correction_T_max  0.526
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'navy blue'
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3428
_exptl_crystal_size_max          0.658
_exptl_crystal_size_mid          0.568
_exptl_crystal_size_min          0.449
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         11466
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.060P)²+28.0P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                9582
_reflns_number_total             11466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0262740si20030129_021710_4.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6546.2(11)
_cod_database_code               4313444
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.14884(3) 0.03813(5) 0.24440(2) 0.02679(15) Uani 1 1 d . . .
Ni2 Ni 0.2500 0.03703(7) 0.2500 0.02464(19) Uani 1 2 d S . .
N1 N 0.16265(19) -0.1136(3) 0.27405(17) 0.0323(9) Uani 1 1 d . . .
N2 N 0.26824(19) -0.0754(3) 0.30510(17) 0.0325(9) Uani 1 1 d . . .
N3 N 0.37145(19) -0.0238(3) 0.32927(16) 0.0308(9) Uani 1 1 d . . .
N4 N 0.17878(18) 0.1002(3) 0.31861(17) 0.0309(9) Uani 1 1 d . . .
N5 N 0.27041(18) 0.1498(3) 0.30594(16) 0.0272(8) Uani 1 1 d . . .
N6 N 0.35594(17) 0.1909(3) 0.28314(16) 0.0282(8) Uani 1 1 d . . .
C1 C 0.1135(3) -0.1849(5) 0.2637(2) 0.0427(13) Uani 1 1 d . . .
H1 H 0.0735 -0.1588 0.2434 0.051 Uiso 1 1 calc R . .
C2 C 0.1214(3) -0.2940(5) 0.2822(3) 0.0521(15) Uani 1 1 d . . .
H2 H 0.0871 -0.3413 0.2753 0.063 Uiso 1 1 calc R . .
C3 C 0.1813(3) -0.3335(5) 0.3117(3) 0.0528(15) Uani 1 1 d . . .
H3 H 0.1874 -0.4069 0.3255 0.063 Uiso 1 1 calc R . .
C4 C 0.2310(3) -0.2637(4) 0.3201(2) 0.0425(13) Uani 1 1 d . . .
H4 H 0.2713 -0.2908 0.3382 0.051 Uiso 1 1 calc R . .
C5 C 0.2216(2) -0.1509(4) 0.3017(2) 0.0329(11) Uani 1 1 d . . .
C6 C 0.3278(2) -0.0774(4) 0.3443(2) 0.0323(11) Uani 1 1 d . . .
C7 C 0.3449(3) -0.1252(5) 0.3973(2) 0.0409(12) Uani 1 1 d . . .
H7 H 0.3152 -0.1617 0.4077 0.049 Uiso 1 1 calc R . .
C8 C 0.4053(3) -0.1186(5) 0.4340(2) 0.0518(15) Uani 1 1 d . . .
H8 H 0.4169 -0.1518 0.4691 0.062 Uiso 1 1 calc R . .
C9 C 0.4493(3) -0.0617(5) 0.4184(2) 0.0474(14) Uani 1 1 d . . .
H9 H 0.4904 -0.0558 0.4430 0.057 Uiso 1 1 calc R . .
C10 C 0.4313(2) -0.0150(5) 0.3668(2) 0.0397(12) Uani 1 1 d . . .
H10 H 0.4604 0.0242 0.3567 0.048 Uiso 1 1 calc R . .
C11 C 0.1431(3) 0.0948(5) 0.3504(2) 0.0391(12) Uani 1 1 d . . .
H11 H 0.1057 0.0554 0.3370 0.047 Uiso 1 1 calc R . .
C12 C 0.1608(3) 0.1460(6) 0.4016(3) 0.0525(15) Uani 1 1 d . . .
H12 H 0.1354 0.1422 0.4224 0.063 Uiso 1 1 calc R . .
C13 C 0.2169(3) 0.2032(6) 0.4219(2) 0.0507(15) Uani 1 1 d . . .
H13 H 0.2291 0.2398 0.4561 0.061 Uiso 1 1 calc R . .
C14 C 0.2541(3) 0.2057(5) 0.3912(2) 0.0402(12) Uani 1 1 d . . .
H14 H 0.2926 0.2415 0.4053 0.048 Uiso 1 1 calc R . .
C15 C 0.2349(2) 0.1551(4) 0.33895(19) 0.0282(10) Uani 1 1 d . . .
C16 C 0.3137(2) 0.2272(4) 0.30516(19) 0.0275(10) Uani 1 1 d . . .
C17 C 0.3136(2) 0.3423(4) 0.3200(2) 0.0371(11) Uani 1 1 d . . .
H17 H 0.2854 0.3680 0.3355 0.045 Uiso 1 1 calc R . .
C18 C 0.3550(3) 0.4155(4) 0.3115(2) 0.0422(13) Uani 1 1 d . . .
H18 H 0.3552 0.4911 0.3214 0.051 Uiso 1 1 calc R . .
C19 C 0.3969(3) 0.3774(4) 0.2879(2) 0.0411(12) Uani 1 1 d . . .
H19 H 0.4251 0.4269 0.2819 0.049 Uiso 1 1 calc R . .
C20 C 0.3957(2) 0.2657(4) 0.2738(2) 0.0344(11) Uani 1 1 d . . .
H20 H 0.4230 0.2402 0.2573 0.041 Uiso 1 1 calc R . .
Ni3 Ni 0.64395(3) 0.42202(5) 0.20607(3) 0.03032(16) Uani 1 1 d . . .
Ni4 Ni 0.7500 0.42026(7) 0.2500 0.0280(2) Uani 1 2 d S . .
N7 N 0.6564(2) 0.4822(4) 0.14117(17) 0.0348(9) Uani 1 1 d . . .
N8 N 0.7558(2) 0.5325(3) 0.20033(17) 0.0331(9) Uani 1 1 d . . .
N9 N 0.8534(2) 0.5733(3) 0.26555(17) 0.0341(9) Uani 1 1 d . . .
N10 N 0.65145(19) 0.2714(4) 0.18055(17) 0.0335(9) Uani 1 1 d . . .
N11 N 0.75619(19) 0.3083(4) 0.20101(17) 0.0332(9) Uani 1 1 d . . .
N12 N 0.85899(19) 0.3643(3) 0.22500(17) 0.0315(9) Uani 1 1 d . . .
C21 C 0.6119(3) 0.4711(5) 0.0899(2) 0.0457(13) Uani 1 1 d . . .
H21 H 0.5744 0.4369 0.0865 0.055 Uiso 1 1 calc R . .
C22 C 0.6201(3) 0.5087(6) 0.0425(3) 0.0595(17) Uani 1 1 d . . .
H22 H 0.5883 0.5022 0.0077 0.071 Uiso 1 1 calc R . .
C23 C 0.6773(4) 0.5568(6) 0.0481(3) 0.0624(18) Uani 1 1 d . . .
H23 H 0.6845 0.5808 0.0167 0.075 Uiso 1 1 calc R . .
C24 C 0.7230(3) 0.5690(5) 0.1000(2) 0.0513(15) Uani 1 1 d . . .
H24 H 0.7609 0.6017 0.1037 0.062 Uiso 1 1 calc R . .
C25 C 0.7121(3) 0.5316(4) 0.1475(2) 0.0357(11) Uani 1 1 d . . .
C26 C 0.8030(2) 0.6085(4) 0.2211(2) 0.0354(11) Uani 1 1 d . . .
C27 C 0.7993(3) 0.7217(5) 0.2033(3) 0.0496(14) Uani 1 1 d . . .
H27 H 0.7647 0.7466 0.1735 0.060 Uiso 1 1 calc R . .
C28 C 0.8471(3) 0.7953(5) 0.2300(3) 0.0588(17) Uani 1 1 d . . .
H28 H 0.8451 0.8698 0.2179 0.071 Uiso 1 1 calc R . .
C29 C 0.8984(3) 0.7585(5) 0.2753(3) 0.0585(17) Uani 1 1 d . . .
H29 H 0.9311 0.8073 0.2936 0.070 Uiso 1 1 calc R . .
C30 C 0.8993(3) 0.6472(5) 0.2922(3) 0.0459(13) Uani 1 1 d . . .
H30 H 0.9328 0.6225 0.3231 0.055 Uiso 1 1 calc R . .
C31 C 0.6025(3) 0.1996(5) 0.1643(2) 0.0385(12) Uani 1 1 d . . .
H31 H 0.5652 0.2236 0.1668 0.046 Uiso 1 1 calc R . .
C32 C 0.6051(3) 0.0945(5) 0.1447(3) 0.0526(15) Uani 1 1 d . . .
H32 H 0.5698 0.0489 0.1325 0.063 Uiso 1 1 calc R . .
C33 C 0.6608(3) 0.0560(5) 0.1432(3) 0.0554(16) Uani 1 1 d . . .
H33 H 0.6635 -0.0162 0.1300 0.066 Uiso 1 1 calc R . .
C34 C 0.7125(3) 0.1251(4) 0.1612(2) 0.0427(13) Uani 1 1 d . . .
H34 H 0.7506 0.0991 0.1613 0.051 Uiso 1 1 calc R . .
C35 C 0.7072(2) 0.2345(4) 0.1795(2) 0.0338(11) Uani 1 1 d . . .
C36 C 0.8079(2) 0.3144(4) 0.1867(2) 0.0329(11) Uani 1 1 d . . .
C37 C 0.8088(3) 0.2818(5) 0.1346(2) 0.0401(12) Uani 1 1 d . . .
H37 H 0.7742 0.2469 0.1086 0.048 Uiso 1 1 calc R . .
C38 C 0.8615(3) 0.3019(5) 0.1220(2) 0.0427(13) Uani 1 1 d . . .
H38 H 0.8624 0.2809 0.0876 0.051 Uiso 1 1 calc R . .
C39 C 0.9125(3) 0.3536(5) 0.1614(2) 0.0439(13) Uani 1 1 d . . .
H39 H 0.9483 0.3670 0.1538 0.053 Uiso 1 1 calc R . .
C40 C 0.9101(3) 0.3851(5) 0.2121(2) 0.0371(12) Uani 1 1 d . . .
H40 H 0.9442 0.4214 0.2380 0.045 Uiso 1 1 calc R . .
P1 P -0.03279(7) 0.04586(12) 0.22944(6) 0.0401(3) Uani 1 1 d . . .
F1 F 0.04147(14) 0.0385(3) 0.23825(14) 0.0450(7) Uani 1 1 d . . .
F2 F -0.02053(16) 0.1681(3) 0.25693(16) 0.0553(9) Uani 1 1 d . . .
F3 F -0.04556(16) 0.1000(3) 0.16972(15) 0.0552(9) Uani 1 1 d . . .
F4 F -0.04199(16) -0.0768(3) 0.20245(17) 0.0594(9) Uani 1 1 d . . .
F5 F -0.01686(17) -0.0092(3) 0.28958(16) 0.0613(10) Uani 1 1 d . . .
F6 F -0.10470(15) 0.0535(3) 0.22076(18) 0.0623(10) Uani 1 1 d . . .
P2 P 0.45479(7) 0.43793(14) 0.13100(7) 0.0474(4) Uani 1 1 d . . .
F7 F 0.53118(15) 0.4241(3) 0.16139(13) 0.0499(8) Uani 1 1 d . . .
F8 F 0.4561(3) 0.3595(5) 0.0827(2) 0.117(2) Uani 1 1 d . . .
F9 F 0.4672(2) 0.5433(4) 0.0995(2) 0.1083(19) Uani 1 1 d . . .
F10 F 0.4573(3) 0.5165(6) 0.1807(2) 0.119(2) Uani 1 1 d . . .
F11 F 0.4459(2) 0.3355(5) 0.1648(2) 0.120(2) Uani 1 1 d . . .
F12 F 0.3825(2) 0.4529(5) 0.1000(2) 0.1037(18) Uani 1 1 d . . .
P3 P 0.32262(8) 0.54422(14) 0.46633(7) 0.0526(4) Uani 1 1 d . . .
F13 F 0.3910(3) 0.5594(8) 0.5016(3) 0.168(3) Uani 1 1 d . . .
F14 F 0.3116(5) 0.6725(5) 0.4703(3) 0.180(4) Uani 1 1 d . . .
F15 F 0.3097(4) 0.5211(6) 0.5196(3) 0.143(3) Uani 1 1 d . . .
F16 F 0.3356(4) 0.4177(5) 0.4611(3) 0.161(3) Uani 1 1 d . . .
F17 F 0.3351(4) 0.5751(6) 0.4110(2) 0.138(3) Uani 1 1 d . . .
F18 F 0.2542(3) 0.5299(9) 0.4290(4) 0.209(5) Uani 1 1 d . . .
C101 C 0.0321(4) 0.3086(7) 0.0419(3) 0.071(2) Uani 1 1 d . . .
Cl1 Cl 0.07722(8) 0.20611(17) 0.02371(8) 0.0680(5) Uani 1 1 d . . .
Cl2 Cl -0.00539(9) 0.24622(18) 0.08280(7) 0.0715(5) Uani 1 1 d . . .
C102 C -0.0561(6) -0.3772(12) 0.1008(4) 0.129(5) Uani 1 1 d . . .
Cl3 Cl 0.02454(14) -0.3889(3) 0.10768(12) 0.1230(10) Uani 1 1 d . . .
Cl4 Cl -0.0599(3) -0.3414(3) 0.16452(18) 0.183(2) Uani 1 1 d . . .
C103 C 0.5367(8) -0.1908(12) 0.0127(6) 0.083(5) Uiso 0.644(18) 1 d PD A 1
Cl5A Cl 0.5692(3) -0.0694(5) -0.0056(3) 0.093(2) Uani 0.644(18) 1 d PD A 1
Cl6A Cl 0.5710(6) -0.2134(4) 0.0835(3) 0.127(4) Uani 0.644(18) 1 d PD A 1
C203 C 0.5163(12) -0.175(2) 0.0017(7) 0.083(9) Uiso 0.356(18) 1 d PD A 2
Cl5B Cl 0.5805(13) -0.093(3) 0.0025(11) 0.280(17) Uani 0.356(18) 1 d PD A 2
Cl6B Cl 0.5270(12) -0.2167(18) 0.0686(7) 0.234(11) Uani 0.356(18) 1 d PD A 2
C104 C -0.1665(5) -0.0483(13) 0.0835(5) 0.132(5) Uani 1 1 d . . .
Cl7 Cl -0.24110(13) -0.0985(3) 0.07465(11) 0.1088(9) Uani 1 1 d . B .
Cl81 Cl -0.1511(6) -0.0137(19) 0.0308(7) 0.148(6) Uani 0.51(4) 1 d P B 1
Cl82 Cl -0.1713(17) 0.029(2) 0.0256(7) 0.195(9) Uani 0.49(4) 1 d P B 2
C105 C 0.6512(5) 0.2571(8) -0.0468(5) 0.105(3) Uani 1 1 d . . .
Cl9 Cl 0.64859(13) 0.2160(3) 0.01879(11) 0.1074(8) Uani 1 1 d . C .
Cl92 Cl 0.6642(5) 0.1423(5) -0.0773(3) 0.169(5) Uani 0.613(9) 1 d P C 1
Cl91 Cl 0.5855(5) 0.1674(6) -0.1037(3) 0.107(3) Uani 0.387(9) 1 d P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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
N4 Ni1 N3 173.51(17) . 2 ?
N4 Ni1 N6 87.65(17) . 2 ?
N3 Ni1 N6 91.91(16) 2 2 ?
N4 Ni1 N1 90.84(17) . . ?
N3 Ni1 N1 88.96(17) 2 . ?
N6 Ni1 N1 174.19(17) 2 . ?
N4 Ni1 Ni2 87.32(12) . . ?
N3 Ni1 Ni2 86.19(12) 2 . ?
N6 Ni1 Ni2 87.01(12) 2 . ?
N1 Ni1 Ni2 87.32(12) . . ?
N2 Ni2 N2 89.8(3) . 2 ?
N2 Ni2 N5 89.98(17) . . ?
N2 Ni2 N5 178.65(17) 2 . ?
N2 Ni2 N5 178.65(17) . 2 ?
N2 Ni2 N5 89.97(17) 2 2 ?
N5 Ni2 N5 90.3(2) . 2 ?
N2 Ni2 Ni1 90.90(12) . 2 ?
N2 Ni2 Ni1 89.56(12) 2 2 ?
N5 Ni2 Ni1 89.13(12) . 2 ?
N5 Ni2 Ni1 90.41(12) 2 2 ?
N2 Ni2 Ni1 89.56(12) . . ?
N2 Ni2 Ni1 90.90(12) 2 . ?
N5 Ni2 Ni1 90.41(12) . . ?
N5 Ni2 Ni1 89.13(12) 2 . ?
Ni1 Ni2 Ni1 179.35(5) 2 . ?
C5 N1 C1 120.3(4) . . ?
C5 N1 Ni1 119.9(3) . . ?
C1 N1 Ni1 119.6(4) . . ?
C5 N2 C6 125.7(4) . . ?
C5 N2 Ni2 117.2(3) . . ?
C6 N2 Ni2 117.0(3) . . ?
C6 N3 C10 119.6(4) . . ?
C6 N3 Ni1 121.3(3) . 2 ?
C10 N3 Ni1 119.1(3) . 2 ?
C11 N4 C15 119.2(4) . . ?
C11 N4 Ni1 120.3(4) . . ?
C15 N4 Ni1 120.4(3) . . ?
C16 N5 C15 125.7(4) . . ?
C16 N5 Ni2 116.2(3) . . ?
C15 N5 Ni2 117.5(3) . . ?
C20 N6 C16 120.1(4) . . ?
C20 N6 Ni1 119.7(3) . 2 ?
C16 N6 Ni1 119.6(3) . 2 ?
N1 C1 C2 121.6(5) . . ?
C1 C2 C3 119.1(6) . . ?
C4 C3 C2 119.5(5) . . ?
C3 C4 C5 120.2(5) . . ?
N1 C5 N2 115.6(4) . . ?
N1 C5 C4 119.1(5) . . ?
N2 C5 C4 125.0(5) . . ?
N3 C6 N2 115.3(4) . . ?
N3 C6 C7 119.6(5) . . ?
N2 C6 C7 125.1(5) . . ?
C8 C7 C6 120.3(5) . . ?
C7 C8 C9 119.4(5) . . ?
C10 C9 C8 119.1(5) . . ?
C9 C10 N3 122.0(5) . . ?
N4 C11 C12 121.8(5) . . ?
C11 C12 C13 119.2(5) . . ?
C14 C13 C12 119.5(5) . . ?
C13 C14 C15 120.5(5) . . ?
N4 C15 N5 115.7(4) . . ?
N4 C15 C14 119.7(4) . . ?
N5 C15 C14 124.4(4) . . ?
N5 C16 N6 115.8(4) . . ?
N5 C16 C17 124.6(4) . . ?
N6 C16 C17 119.2(4) . . ?
C18 C17 C16 119.7(5) . . ?
C17 C18 C19 120.2(5) . . ?
C20 C19 C18 118.8(5) . . ?
N6 C20 C19 122.0(5) . . ?
N9 Ni3 N12 89.22(17) 2_655 2_655 ?
N9 Ni3 N10 173.52(18) 2_655 . ?
N12 Ni3 N10 91.40(17) 2_655 . ?
N9 Ni3 N7 89.54(18) 2_655 . ?
N12 Ni3 N7 173.86(18) 2_655 . ?
N10 Ni3 N7 89.16(17) . . ?
N9 Ni3 Ni4 86.64(13) 2_655 . ?
N12 Ni3 Ni4 86.18(13) 2_655 . ?
N10 Ni3 Ni4 86.97(13) . . ?
N7 Ni3 Ni4 87.74(13) . . ?
N11 Ni4 N11 89.9(3) 2_655 . ?
N11 Ni4 N8 89.92(17) 2_655 2_655 ?
N11 Ni4 N8 179.6(2) . 2_655 ?
N11 Ni4 N8 179.6(2) 2_655 . ?
N11 Ni4 N8 89.91(17) . . ?
N8 Ni4 N8 90.3(3) 2_655 . ?
N11 Ni4 Ni3 90.46(13) 2_655 . ?
N11 Ni4 Ni3 90.28(13) . . ?
N8 Ni4 Ni3 90.00(13) 2_655 . ?
N8 Ni4 Ni3 89.26(13) . . ?
N11 Ni4 Ni3 90.28(13) 2_655 2_655 ?
N11 Ni4 Ni3 90.46(13) . 2_655 ?
N8 Ni4 Ni3 89.27(13) 2_655 2_655 ?
N8 Ni4 Ni3 90.00(13) . 2_655 ?
Ni3 Ni4 Ni3 178.96(5) . 2_655 ?
C21 N7 C25 120.2(4) . . ?
C21 N7 Ni3 120.7(4) . . ?
C25 N7 Ni3 119.0(3) . . ?
C26 N8 C25 126.1(4) . . ?
C26 N8 Ni4 116.4(3) . . ?
C25 N8 Ni4 117.5(3) . . ?
C30 N9 C26 119.8(5) . . ?
C30 N9 Ni3 119.9(4) . 2_655 ?
C26 N9 Ni3 120.1(3) . 2_655 ?
C31 N10 C35 118.6(4) . . ?
C31 N10 Ni3 121.1(3) . . ?
C35 N10 Ni3 120.3(3) . . ?
C35 N11 C36 126.3(4) . . ?
C35 N11 Ni4 117.8(3) . . ?
C36 N11 Ni4 115.7(3) . . ?
C40 N12 C36 119.8(4) . . ?
C40 N12 Ni3 119.2(4) . 2_655 ?
C36 N12 Ni3 120.5(3) . 2_655 ?
N7 C21 C22 122.4(6) . . ?
C21 C22 C23 118.1(6) . . ?
C24 C23 C22 120.2(6) . . ?
C23 C24 C25 119.7(6) . . ?
N7 C25 N8 116.3(4) . . ?
N7 C25 C24 119.3(5) . . ?
N8 C25 C24 124.2(5) . . ?
N8 C26 N9 116.2(4) . . ?
N8 C26 C27 123.8(5) . . ?
N9 C26 C27 119.7(5) . . ?
C28 C27 C26 119.8(6) . . ?
C27 C28 C29 120.0(6) . . ?
C30 C29 C28 118.1(6) . . ?
N9 C30 C29 122.5(6) . . ?
N10 C31 C32 123.2(5) . . ?
C31 C32 C33 119.0(6) . . ?
C32 C33 C34 119.7(5) . . ?
C33 C34 C35 119.3(5) . . ?
N10 C35 N11 115.5(4) . . ?
N10 C35 C34 120.1(5) . . ?
N11 C35 C34 124.2(5) . . ?
N12 C36 N11 115.6(4) . . ?
N12 C36 C37 120.0(5) . . ?
N11 C36 C37 124.2(5) . . ?
C38 C37 C36 119.8(5) . . ?
C39 C38 C37 119.1(5) . . ?
C40 C39 C38 119.7(5) . . ?
N12 C40 C39 121.5(5) . . ?
F4 P1 F3 89.8(2) . . ?
F4 P1 F2 177.6(2) . . ?
F3 P1 F2 90.2(2) . . ?
F4 P1 F6 91.5(2) . . ?
F3 P1 F6 91.6(2) . . ?
F2 P1 F6 91.0(2) . . ?
F4 P1 F5 89.9(2) . . ?
F3 P1 F5 177.5(2) . . ?
F2 P1 F5 89.9(2) . . ?
F6 P1 F5 91.0(2) . . ?
F4 P1 F1 88.68(18) . . ?
F3 P1 F1 88.23(18) . . ?
F2 P1 F1 88.90(18) . . ?
F6 P1 F1 179.8(2) . . ?
F5 P1 F1 89.25(19) . . ?
F11 P2 F8 91.6(4) . . ?
F11 P2 F10 88.7(4) . . ?
F8 P2 F10 177.0(3) . . ?
F11 P2 F9 176.8(3) . . ?
F8 P2 F9 90.0(4) . . ?
F10 P2 F9 89.6(4) . . ?
F11 P2 F12 92.2(3) . . ?
F8 P2 F12 89.4(3) . . ?
F10 P2 F12 93.6(3) . . ?
F9 P2 F12 90.5(3) . . ?
F11 P2 F7 89.6(2) . . ?
F8 P2 F7 89.4(2) . . ?
F10 P2 F7 87.6(2) . . ?
F9 P2 F7 87.6(2) . . ?
F12 P2 F7 177.8(3) . . ?
F13 P3 F18 178.1(5) . . ?
F13 P3 F15 89.2(5) . . ?
F18 P3 F15 92.7(5) . . ?
F13 P3 F16 88.6(5) . . ?
F18 P3 F16 91.5(5) . . ?
F15 P3 F16 90.8(4) . . ?
F13 P3 F14 90.2(5) . . ?
F18 P3 F14 89.6(6) . . ?
F15 P3 F14 91.5(4) . . ?
F16 P3 F14 177.5(5) . . ?
F13 P3 F17 91.1(4) . . ?
F18 P3 F17 86.9(5) . . ?
F15 P3 F17 177.0(4) . . ?
F16 P3 F17 92.2(4) . . ?
F14 P3 F17 85.5(4) . . ?
Cl2 C101 Cl1 109.8(4) . . ?
Cl4 C102 Cl3 109.5(7) . . ?
Cl6A C103 Cl5A 109.5(8) . . ?
Cl6B C203 Cl5B 109.4(8) . . ?
Cl81 C104 Cl82 22.8(12) . . ?
Cl81 C104 Cl7 119.7(9) . . ?
Cl82 C104 Cl7 108.6(13) . . ?
Cl92 C105 Cl9 107.6(6) . . ?
Cl92 C105 Cl91 55.4(5) . . ?
Cl9 C105 Cl91 105.8(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 N4 1.925(4) . y
Ni1 N3 1.926(4) 2 y
Ni1 N6 1.931(4) 2 y
Ni1 N1 1.931(4) . y
Ni1 Ni2 2.2851(6) . y
Ni2 N2 1.878(4) . y
Ni2 N2 1.878(4) 2 y
Ni2 N5 1.893(4) . y
Ni2 N5 1.893(4) 2 y
Ni2 Ni1 2.2850(6) . y
N1 C5 1.357(6) . ?
N1 C1 1.360(7) . ?
N2 C5 1.376(6) . ?
N2 C6 1.375(6) . ?
N3 C6 1.362(6) . ?
N3 C10 1.368(7) . ?
N3 Ni1 1.926(4) 2 ?
N4 C11 1.358(6) . ?
N4 C15 1.369(6) . ?
N5 C16 1.361(6) . ?
N5 C15 1.382(6) . ?
N6 C20 1.359(6) . ?
N6 C16 1.364(6) . ?
N6 Ni1 1.931(4) 2 ?
C1 C2 1.366(8) . ?
C2 C3 1.391(9) . ?
C3 C4 1.365(8) . ?
C4 C5 1.407(7) . ?
C6 C7 1.394(7) . ?
C7 C8 1.370(8) . ?
C8 C9 1.395(9) . ?
C9 C10 1.356(8) . ?
C11 C12 1.371(8) . ?
C12 C13 1.382(9) . ?
C13 C14 1.364(8) . ?
C14 C15 1.389(7) . ?
C16 C17 1.415(7) . ?
C17 C18 1.366(7) . ?
C18 C19 1.391(8) . ?
C19 C20 1.369(7) . ?
Ni3 N9 1.927(4) 2_655 y
Ni3 N12 1.928(4) 2_655 y
Ni3 N10 1.930(4) . y
Ni3 N7 1.934(4) . y
Ni3 Ni4 2.2885(7) . y
Ni4 N11 1.871(4) 2_655 y
Ni4 N11 1.871(4) . y
Ni4 N8 1.883(4) 2_655 y
Ni4 N8 1.883(4) . y
Ni4 Ni3 2.2886(7) 2_655 y
N7 C21 1.349(7) . ?
N7 C25 1.366(7) . ?
N8 C26 1.361(7) . ?
N8 C25 1.364(7) . ?
N9 C30 1.351(7) . ?
N9 C26 1.364(7) . ?
N9 Ni3 1.927(4) 2_655 ?
N10 C31 1.351(7) . ?
N10 C35 1.367(6) . ?
N11 C35 1.375(6) . ?
N11 C36 1.374(6) . ?
N12 C40 1.361(6) . ?
N12 C36 1.364(7) . ?
N12 Ni3 1.927(4) 2_655 ?
C21 C22 1.376(8) . ?
C22 C23 1.396(10) . ?
C23 C24 1.372(9) . ?
C24 C25 1.410(7) . ?
C26 C27 1.408(7) . ?
C27 C28 1.376(9) . ?
C28 C29 1.392(10) . ?
C29 C30 1.385(8) . ?
C31 C32 1.352(8) . ?
C32 C33 1.378(9) . ?
C33 C34 1.380(8) . ?
C34 C35 1.399(7) . ?
C36 C37 1.402(7) . ?
C37 C38 1.388(8) . ?
C38 C39 1.384(8) . ?
C39 C40 1.377(7) . ?
P1 F4 1.589(4) . y
P1 F3 1.592(4) . y
P1 F2 1.590(4) . y
P1 F6 1.593(3) . y
P1 F5 1.595(4) . y
P1 F1 1.646(3) . y
P2 F11 1.550(5) . y
P2 F8 1.561(5) . y
P2 F10 1.567(5) . y
P2 F9 1.571(5) . y
P2 F12 1.573(4) . y
P2 F7 1.654(4) . y
P3 F13 1.515(6) . y
P3 F18 1.527(7) . y
P3 F15 1.534(5) . y
P3 F16 1.542(5) . y
P3 F14 1.548(5) . y
P3 F17 1.597(6) . y
C101 Cl2 1.753(7) . ?
C101 Cl1 1.769(8) . ?
C102 Cl4 1.729(11) . ?
C102 Cl3 1.808(12) . ?
C103 Cl6A 1.722(13) . ?
C103 Cl5A 1.763(11) . ?
C203 Cl6B 1.722(13) . ?
C203 Cl5B 1.763(11) . ?
C104 Cl81 1.579(18) . ?
C104 Cl82 1.717(19) . ?
C104 Cl7 1.755(11) . ?
C105 Cl92 1.651(11) . ?
C105 Cl9 1.782(10) . ?
C105 Cl91 1.986(14) . ?
