#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/28/4302893.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_4302893
loop_
_publ_author_name
'T. V. Brinzari'
'C. Tian'
'G. J. Halder'
'J. L. Musfeldt'
'M.-H. Whangbo'
'J. A. Schlueter'
_publ_contact_author_address
;
Materials Science Division
Argonne National Laboratory
Argonne, IL 60439-4831, USA
;
_publ_contact_author_email       JASchlueter@anl.gov
_publ_contact_author_fax         '(630) 252-9151'
_publ_contact_author_name        'Dr. John Schlueter'
_publ_contact_author_phone       '(630) 252-3588'
_publ_section_title
;
Color Properties and Structural Phase Transition in Penta- And
Hexacoordinate Isothiocyanato Ni(II) Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7650
_journal_page_last               7658
_journal_paper_doi               10.1021/ic802120n
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '4(C8 H20 N 1+), C6 N6 Ni S6 4-'
_chemical_formula_sum            'C38 H80 N10 Ni S6'
_chemical_formula_weight         928.19
_chemical_melting_point          449
_chemical_name_common
; 
Tetrabutylammonium hexathiocyanato nickalate(II) 
;
_chemical_name_systematic
; 
Tetraethylammonium hexathiocyanato nickalate(II) 
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      64
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   18.7942(12)
_cell_length_b                   20.8981(15)
_cell_length_c                   38.107(3)
_cell_measurement_reflns_used    1946
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.186
_cell_measurement_theta_min      3.106
_cell_volume                     14967.0(19)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Siemens, 1997-1998)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2001), PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'area detector ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            62709
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.07
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(Sheldrick, 2001)
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6024
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.972
_refine_diff_density_min         -1.550
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.422
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         9461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.422
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0380P)²+10.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                7708
_reflns_number_total             9461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802120n_si_002_4.cif
_cod_data_source_block           TEANiNCS_150K
_cod_original_cell_volume        14966.9(18)
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               4302893
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.483160(16) 0.163629(9) 0.02435(9) Uani 1 2 d S . .
S1 S 0.0000 0.36942(5) 0.27556(2) 0.0434(2) Uani 1 2 d S . .
S2 S 0.18970(3) 0.63345(3) 0.189541(17) 0.04812(18) Uani 1 1 d . . .
S3 S 0.16804(3) 0.31288(3) 0.140775(19) 0.04832(17) Uani 1 1 d . . .
S4 S 0.0000 0.59710(4) 0.05179(2) 0.03283(17) Uani 1 2 d S . .
N1 N 0.0000 0.43659(11) 0.21203(6) 0.0279(5) Uani 1 2 d S . .
N2 N 0.07974(9) 0.54498(8) 0.18089(5) 0.0329(4) Uani 1 1 d . . .
N3 N 0.07873(9) 0.41959(8) 0.14621(5) 0.0310(4) Uani 1 1 d . . .
N4 N 0.0000 0.53116(12) 0.11561(7) 0.0348(6) Uani 1 2 d S . .
C1 C 0.0000 0.40889(13) 0.23808(7) 0.0252(5) Uani 1 2 d S . .
C2 C 0.12523(10) 0.58116(10) 0.18448(5) 0.0263(4) Uani 1 1 d . . .
C3 C 0.11588(10) 0.37587(10) 0.14380(5) 0.0271(4) Uani 1 1 d . . .
C4 C 0.0000 0.55873(13) 0.08937(7) 0.0254(5) Uani 1 2 d S . .
Ni2 Ni 0.0000 0.0000 0.0000 0.03261(14) Uani 1 4 d S . .
S5 S 0.18903(3) 0.15197(3) -0.022315(16) 0.03900(14) Uani 1 1 d . . .
S6 S 0.0000 -0.00356(4) 0.12793(2) 0.04080(19) Uani 1 2 d S . .
N5 N 0.07967(9) 0.06899(10) -0.00236(5) 0.0385(4) Uani 1 1 d . . .
N6 N 0.0000 0.00418(13) 0.05454(7) 0.0367(6) Uani 1 2 d S . .
C5 C 0.12507(10) 0.10305(10) -0.01052(5) 0.0268(4) Uani 1 1 d . . .
C6 C 0.0000 0.00105(13) 0.08491(8) 0.0272(6) Uani 1 2 d S . .
N10 N 0.0000 0.28323(10) 0.04784(6) 0.0225(4) Uani 1 2 d S . .
C11 C 0.06464(10) 0.27585(10) 0.02424(5) 0.0303(4) Uani 1 1 d . . .
H11A H 0.0623 0.2333 0.0128 0.036 Uiso 1 1 calc R . .
H11B H 0.0619 0.3085 0.0055 0.036 Uiso 1 1 calc R . .
C12 C 0.13596(11) 0.28204(12) 0.04220(6) 0.0405(5) Uani 1 1 d . . .
H12A H 0.1740 0.2768 0.0249 0.061 Uiso 1 1 calc R . .
H12B H 0.1404 0.2489 0.0603 0.061 Uiso 1 1 calc R . .
H12C H 0.1397 0.3244 0.0531 0.061 Uiso 1 1 calc R . .
C13 C 0.0000 0.23314(14) 0.07657(8) 0.0290(6) Uani 1 2 d S . .
H13A H 0.0425 0.2401 0.0915 0.035 Uiso 0.50 1 calc PR . .
H13B H -0.0425 0.2401 0.0915 0.035 Uiso 0.50 1 calc PR . .
C14 C 0.0000 0.16458(16) 0.06455(10) 0.0447(8) Uani 1 2 d S . .
H14A H 0.0000 0.1362 0.0850 0.067 Uiso 1 2 calc SR . .
H14B H 0.0426 0.1564 0.0504 0.067 Uiso 0.50 1 calc PR . .
H14C H -0.0426 0.1564 0.0504 0.067 Uiso 0.50 1 calc PR . .
C15 C 0.0000 0.34742(14) 0.06636(7) 0.0288(6) Uani 1 2 d S . .
H15A H -0.0425 0.3498 0.0817 0.035 Uiso 0.50 1 calc PR . .
H15B H 0.0425 0.3498 0.0817 0.035 Uiso 0.50 1 calc PR . .
C16 C 0.0000 0.40487(15) 0.04229(10) 0.0409(8) Uani 1 2 d S . .
H16A H 0.0000 0.4441 0.0563 0.061 Uiso 1 2 calc SR . .
H16B H -0.0426 0.4039 0.0274 0.061 Uiso 0.50 1 calc PR . .
H16C H 0.0426 0.4039 0.0274 0.061 Uiso 0.50 1 calc PR . .
N20 N 0.0000 0.67109(11) 0.28825(5) 0.0217(4) Uani 1 2 d S . .
C25 C 0.0000 0.71336(13) 0.32048(7) 0.0252(5) Uani 1 2 d S . .
H25A H -0.0425 0.7030 0.3347 0.030 Uiso 0.50 1 calc PR . .
H25B H 0.0425 0.7030 0.3347 0.030 Uiso 0.50 1 calc PR . .
C26 C 0.0000 0.78421(14) 0.31313(9) 0.0354(7) Uani 1 2 d S . .
H26A H 0.0000 0.8078 0.3354 0.053 Uiso 1 2 calc SR . .
H26B H -0.0426 0.7955 0.2996 0.053 Uiso 0.50 1 calc PR . .
H26C H 0.0426 0.7955 0.2996 0.053 Uiso 0.50 1 calc PR . .
C21 C 0.06473(10) 0.68427(10) 0.26541(5) 0.0284(4) Uani 1 1 d . . .
H21A H 0.0639 0.6544 0.2452 0.034 Uiso 1 1 calc R . .
H21B H 0.0608 0.7282 0.2559 0.034 Uiso 1 1 calc R . .
C22 C 0.13577(11) 0.67777(12) 0.28383(6) 0.0366(5) Uani 1 1 d . . .
H22A H 0.1742 0.6869 0.2672 0.055 Uiso 1 1 calc R . .
H22B H 0.1410 0.6341 0.2928 0.055 Uiso 1 1 calc R . .
H22C H 0.1381 0.7081 0.3034 0.055 Uiso 1 1 calc R . .
C23 C 0.0000 0.60276(13) 0.30125(7) 0.0311(6) Uani 1 2 d S . .
H23A H 0.0425 0.5964 0.3162 0.037 Uiso 0.50 1 calc PR . .
H23B H -0.0425 0.5964 0.3162 0.037 Uiso 0.50 1 calc PR . .
C24 C 0.0000 0.55187(17) 0.27311(10) 0.0526(10) Uani 1 2 d S . .
H24A H 0.0000 0.5095 0.2841 0.079 Uiso 1 2 calc SR . .
H24B H 0.0426 0.5566 0.2585 0.079 Uiso 0.50 1 calc PR . .
H24C H -0.0426 0.5566 0.2585 0.079 Uiso 0.50 1 calc PR . .
N30 N 0.25147(8) 0.05173(8) 0.08428(4) 0.0240(3) Uani 1 1 d . . .
C31 C 0.17882(10) 0.08310(10) 0.08438(5) 0.0286(4) Uani 1 1 d . . .
H31A H 0.1748 0.1107 0.0633 0.034 Uiso 1 1 calc R . .
H31B H 0.1421 0.0493 0.0824 0.034 Uiso 1 1 calc R . .
C32 C 0.16292(12) 0.12313(12) 0.11648(6) 0.0408(5) Uani 1 1 d . . .
H32A H 0.1153 0.1419 0.1143 0.061 Uiso 1 1 calc R . .
H32B H 0.1983 0.1574 0.1185 0.061 Uiso 1 1 calc R . .
H32C H 0.1648 0.0961 0.1375 0.061 Uiso 1 1 calc R . .
C33 C 0.25702(11) 0.01493(10) 0.05000(5) 0.0292(4) Uani 1 1 d . . .
H33A H 0.2169 -0.0156 0.0486 0.035 Uiso 1 1 calc R . .
H33B H 0.2521 0.0454 0.0303 0.035 Uiso 1 1 calc R . .
C34 C 0.32611(12) -0.02165(12) 0.04564(6) 0.0388(5) Uani 1 1 d . . .
H34A H 0.3260 -0.0438 0.0230 0.058 Uiso 1 1 calc R . .
H34B H 0.3307 -0.0531 0.0646 0.058 Uiso 1 1 calc R . .
H34C H 0.3662 0.0083 0.0466 0.058 Uiso 1 1 calc R . .
C35 C 0.26045(12) 0.00729(10) 0.11557(5) 0.0328(5) Uani 1 1 d . . .
H35A H 0.3092 -0.0107 0.1151 0.039 Uiso 1 1 calc R . .
H35B H 0.2557 0.0327 0.1374 0.039 Uiso 1 1 calc R . .
C36 C 0.20737(15) -0.04745(11) 0.11667(6) 0.0455(6) Uani 1 1 d . . .
H36A H 0.2162 -0.0737 0.1375 0.068 Uiso 1 1 calc R . .
H36B H 0.2127 -0.0738 0.0956 0.068 Uiso 1 1 calc R . .
H36C H 0.1589 -0.0302 0.1176 0.068 Uiso 1 1 calc R . .
C37 C 0.31034(10) 0.10137(10) 0.08728(5) 0.0310(4) Uani 1 1 d . . .
H37A H 0.3070 0.1219 0.1106 0.037 Uiso 1 1 calc R . .
H37B H 0.3568 0.0791 0.0861 0.037 Uiso 1 1 calc R . .
C38 C 0.30895(13) 0.15304(12) 0.05951(7) 0.0441(6) Uani 1 1 d . . .
H38A H 0.3486 0.1827 0.0634 0.066 Uiso 1 1 calc R . .
H38B H 0.2639 0.1765 0.0609 0.066 Uiso 1 1 calc R . .
H38C H 0.3135 0.1335 0.0363 0.066 Uiso 1 1 calc R . .
N40 N 0.0000 0.27686(10) 0.37862(5) 0.0179(4) Uani 1 2 d S . .
C41 C 0.06481(10) 0.31309(9) 0.36533(5) 0.0236(4) Uani 1 1 d . . .
H41A H 0.0636 0.3135 0.3394 0.028 Uiso 1 1 calc R . .
H41B H 0.0615 0.3580 0.3734 0.028 Uiso 1 1 calc R . .
C42 C 0.13554(11) 0.28603(11) 0.37702(6) 0.0333(5) Uani 1 1 d . . .
H42A H 0.1742 0.3122 0.3674 0.050 Uiso 1 1 calc R . .
H42B H 0.1402 0.2420 0.3685 0.050 Uiso 1 1 calc R . .
H42C H 0.1380 0.2864 0.4027 0.050 Uiso 1 1 calc R . .
C43 C 0.0000 0.20808(12) 0.36533(7) 0.0232(5) Uani 1 2 d S . .
H43A H 0.0425 0.1861 0.3748 0.028 Uiso 0.50 1 calc PR . .
H43B H -0.0425 0.1861 0.3748 0.028 Uiso 0.50 1 calc PR . .
C44 C 0.0000 0.20094(15) 0.32604(8) 0.0344(7) Uani 1 2 d S . .
H44A H 0.0000 0.1554 0.3199 0.052 Uiso 1 2 calc SR . .
H44B H 0.0426 0.2214 0.3163 0.052 Uiso 0.50 1 calc PR . .
H44C H -0.0426 0.2214 0.3163 0.052 Uiso 0.50 1 calc PR . .
C45 C 0.0000 0.27385(13) 0.41832(6) 0.0235(5) Uani 1 2 d S . .
H45A H -0.0425 0.2497 0.4261 0.028 Uiso 0.50 1 calc PR . .
H45B H 0.0425 0.2497 0.4261 0.028 Uiso 0.50 1 calc PR . .
C46 C 0.0000 0.33799(15) 0.43624(7) 0.0316(6) Uani 1 2 d S . .
H46A H 0.0000 0.3318 0.4617 0.047 Uiso 1 2 calc SR . .
H46B H -0.0426 0.3619 0.4293 0.047 Uiso 0.50 1 calc PR . .
H46C H 0.0426 0.3619 0.4293 0.047 Uiso 0.50 1 calc PR . .
N50 N 0.2500 0.40364(11) 0.2500 0.0265(5) Uani 1 2 d S . .
C51A C 0.25410(17) 0.44325(16) 0.28276(8) 0.0446(3) Uiso 0.803(3) 1 d P A 1
H51A H 0.2980 0.4694 0.2820 0.054 Uiso 0.803(3) 1 calc PR A 1
H51B H 0.2576 0.4143 0.3033 0.054 Uiso 0.803(3) 1 calc PR A 1
C52A C 0.18949(13) 0.48815(13) 0.28782(7) 0.0446(3) Uiso 0.803(3) 1 d P A 1
H52A H 0.1953 0.5125 0.3096 0.067 Uiso 0.803(3) 1 calc PR A 1
H52B H 0.1458 0.4626 0.2891 0.067 Uiso 0.803(3) 1 calc PR A 1
H52C H 0.1864 0.5178 0.2679 0.067 Uiso 0.803(3) 1 calc PR A 1
C53A C 0.31623(16) 0.36088(15) 0.24974(9) 0.0446(3) Uiso 0.803(3) 1 d P A 1
H53A H 0.3590 0.3885 0.2485 0.054 Uiso 0.803(3) 1 calc PR A 1
H53B H 0.3183 0.3371 0.2722 0.054 Uiso 0.803(3) 1 calc PR A 1
C54A C 0.31884(18) 0.31326(16) 0.21978(9) 0.0446(3) Uiso 0.803(3) 1 d P A 1
H54A H 0.3628 0.2882 0.2213 0.067 Uiso 0.803(3) 1 calc PR A 1
H54B H 0.3176 0.3363 0.1974 0.067 Uiso 0.803(3) 1 calc PR A 1
H54C H 0.2778 0.2845 0.2213 0.067 Uiso 0.803(3) 1 calc PR A 1
C51B C 0.1839(7) 0.4492(6) 0.2536(3) 0.0446(3) Uiso 0.197(3) 1 d P A 2
H51C H 0.1820 0.4786 0.2333 0.054 Uiso 0.197(3) 1 calc PR A 2
H51D H 0.1396 0.4235 0.2538 0.054 Uiso 0.197(3) 1 calc PR A 2
C52B C 0.18949(13) 0.48815(13) 0.28782(7) 0.0446(3) Uiso 0.197(3) 1 d P A 2
H52D H 0.1462 0.5138 0.2909 0.067 Uiso 0.197(3) 1 calc PR A 2
H52E H 0.2309 0.5166 0.2866 0.067 Uiso 0.197(3) 1 calc PR A 2
H52F H 0.1949 0.4589 0.3077 0.067 Uiso 0.197(3) 1 calc PR A 2
C53B C 0.2357(7) 0.3674(6) 0.2176(3) 0.0446(3) Uiso 0.197(3) 1 d P A 2
H53C H 0.2312 0.3979 0.1979 0.054 Uiso 0.197(3) 1 calc PR A 2
H53D H 0.1895 0.3451 0.2202 0.054 Uiso 0.197(3) 1 calc PR A 2
C54B C 0.2921(7) 0.3186(7) 0.2085(4) 0.0446(3) Uiso 0.197(3) 1 d P A 2
H54D H 0.2788 0.2964 0.1868 0.067 Uiso 0.197(3) 1 calc PR A 2
H54E H 0.2963 0.2874 0.2276 0.067 Uiso 0.197(3) 1 calc PR A 2
H54F H 0.3379 0.3402 0.2051 0.067 Uiso 0.197(3) 1 calc PR A 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'
S S 0.1246 0.1234 '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'
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
N2 Ni1 N2 91.91(10) . 12 ?
N2 Ni1 N1 90.58(7) . . ?
N2 Ni1 N1 90.58(7) 12 . ?
N2 Ni1 N4 88.78(7) . . ?
N2 Ni1 N4 88.78(7) 12 . ?
N1 Ni1 N4 179.09(10) . . ?
N2 Ni1 N3 89.15(7) . . ?
N2 Ni1 N3 178.90(7) 12 . ?
N1 Ni1 N3 89.10(7) . . ?
N4 Ni1 N3 91.54(7) . . ?
N2 Ni1 N3 178.90(7) . 12 ?
N2 Ni1 N3 89.15(7) 12 12 ?
N1 Ni1 N3 89.10(7) . 12 ?
N4 Ni1 N3 91.55(7) . 12 ?
N3 Ni1 N3 89.79(10) . 12 ?
C1 N1 Ni1 177.6(2) . . ?
C2 N2 Ni1 168.43(17) . . ?
C3 N3 Ni1 162.61(16) . . ?
C4 N4 Ni1 178.8(3) . . ?
N1 C1 S1 179.8(3) . . ?
N2 C2 S2 179.4(2) . . ?
N3 C3 S3 179.1(2) . . ?
N4 C4 S4 179.3(3) . . ?
N6 Ni2 N6 180.0 9 . ?
N6 Ni2 N5 89.19(7) 9 12 ?
N6 Ni2 N5 90.81(7) . 12 ?
N6 Ni2 N5 89.19(7) 9 . ?
N6 Ni2 N5 90.81(7) . . ?
N5 Ni2 N5 92.06(10) 12 . ?
N6 Ni2 N5 90.81(7) 9 9 ?
N6 Ni2 N5 89.19(7) . 9 ?
N5 Ni2 N5 87.94(10) 12 9 ?
N5 Ni2 N5 180.0 . 9 ?
N6 Ni2 N5 90.81(7) 9 4 ?
N6 Ni2 N5 89.19(7) . 4 ?
N5 Ni2 N5 180.0 12 4 ?
N5 Ni2 N5 87.94(10) . 4 ?
N5 Ni2 N5 92.06(10) 9 4 ?
C5 N5 Ni2 166.26(19) . . ?
C6 N6 Ni2 174.4(3) . . ?
N5 C5 S5 179.4(2) . . ?
N6 C6 S6 179.9(3) . . ?
C13 N10 C15 106.0(2) . . ?
C13 N10 C11 110.95(14) . 12 ?
C15 N10 C11 111.44(14) . 12 ?
C13 N10 C11 110.95(14) . . ?
C15 N10 C11 111.44(14) . . ?
C11 N10 C11 106.2(2) 12 . ?
C12 C11 N10 115.64(17) . . ?
C12 C11 H11A 108.4 . . ?
N10 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
N10 C11 H11B 108.4 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N10 116.0(3) . . ?
C14 C13 H13A 108.3 . . ?
N10 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
N10 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N10 114.9(2) . . ?
C16 C15 H15A 108.5 . . ?
N10 C15 H15A 108.5 . . ?
C16 C15 H15B 108.5 . . ?
N10 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C23 N20 C25 106.6(2) . . ?
C23 N20 C21 111.01(14) . 12 ?
C25 N20 C21 111.03(14) . 12 ?
C23 N20 C21 111.01(14) . . ?
C25 N20 C21 111.03(14) . . ?
C21 N20 C21 106.23(19) 12 . ?
C26 C25 N20 115.0(2) . . ?
C26 C25 H25A 108.5 . . ?
N20 C25 H25A 108.5 . . ?
C26 C25 H25B 108.5 . . ?
N20 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C21 N20 115.07(16) . . ?
C22 C21 H21A 108.5 . . ?
N20 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
N20 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N20 115.6(2) . . ?
C24 C23 H23A 108.4 . . ?
N20 C23 H23A 108.4 . . ?
C24 C23 H23B 108.4 . . ?
N20 C23 H23B 108.4 . . ?
H23A C23 H23B 107.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C31 N30 C33 106.43(14) . . ?
C31 N30 C35 111.25(15) . . ?
C33 N30 C35 110.95(15) . . ?
C31 N30 C37 111.12(15) . . ?
C33 N30 C37 111.10(15) . . ?
C35 N30 C37 106.07(15) . . ?
C32 C31 N30 114.81(16) . . ?
C32 C31 H31A 108.6 . . ?
N30 C31 H31A 108.6 . . ?
C32 C31 H31B 108.6 . . ?
N30 C31 H31B 108.6 . . ?
H31A C31 H31B 107.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N30 114.09(16) . . ?
C34 C33 H33A 108.7 . . ?
N30 C33 H33A 108.7 . . ?
C34 C33 H33B 108.7 . . ?
N30 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N30 114.13(17) . . ?
C36 C35 H35A 108.7 . . ?
N30 C35 H35A 108.7 . . ?
C36 C35 H35B 108.7 . . ?
N30 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N30 114.95(16) . . ?
C38 C37 H37A 108.5 . . ?
N30 C37 H37A 108.5 . . ?
C38 C37 H37B 108.5 . . ?
N30 C37 H37B 108.5 . . ?
H37A C37 H37B 107.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C45 N40 C41 110.69(13) . 12 ?
C45 N40 C41 110.69(13) . . ?
C41 N40 C41 106.43(19) 12 . ?
C45 N40 C43 107.04(19) . . ?
C41 N40 C43 111.02(13) 12 . ?
C41 N40 C43 111.02(13) . . ?
C42 C41 N40 114.83(16) . . ?
C42 C41 H41A 108.6 . . ?
N40 C41 H41A 108.6 . . ?
C42 C41 H41B 108.6 . . ?
N40 C41 H41B 108.6 . . ?
H41A C41 H41B 107.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 N40 115.1(2) . . ?
C44 C43 H43A 108.5 . . ?
N40 C43 H43A 108.5 . . ?
C44 C43 H43B 108.5 . . ?
N40 C43 H43B 108.5 . . ?
H43A C43 H43B 107.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N40 114.6(2) . . ?
C46 C45 H45A 108.6 . . ?
N40 C45 H45A 108.6 . . ?
C46 C45 H45B 108.6 . . ?
N40 C45 H45B 108.6 . . ?
H45A C45 H45B 107.6 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C53B N50 C53B 118.1(10) 7_545 . ?
C53B N50 C51A 172.2(5) 7_545 7_545 ?
C53B N50 C51A 65.0(5) . 7_545 ?
C53B N50 C51A 65.0(5) 7_545 . ?
C53B N50 C51A 172.2(5) . . ?
C51A N50 C51A 113.0(3) 7_545 . ?
C53B N50 C53A 80.9(5) 7_545 7_545 ?
C53B N50 C53A 63.7(5) . 7_545 ?
C51A N50 C53A 106.60(17) 7_545 7_545 ?
C51A N50 C53A 110.99(17) . 7_545 ?
C53B N50 C53A 63.7(5) 7_545 . ?
C53B N50 C53A 80.9(5) . . ?
C51A N50 C53A 110.99(17) 7_545 . ?
C51A N50 C53A 106.59(17) . . ?
C53A N50 C53A 108.6(3) 7_545 . ?
C53B N50 C51B 112.5(7) 7_545 . ?
C53B N50 C51B 103.9(7) . . ?
C51A N50 C51B 72.4(5) 7_545 . ?
C51A N50 C51B 68.5(5) . . ?
C53A N50 C51B 73.2(5) 7_545 . ?
C53A N50 C51B 175.0(5) . . ?
C53B N50 C51B 103.9(7) 7_545 7_545 ?
C53B N50 C51B 112.5(7) . 7_545 ?
C51A N50 C51B 68.5(5) 7_545 7_545 ?
C51A N50 C51B 72.4(5) . 7_545 ?
C53A N50 C51B 175.0(5) 7_545 7_545 ?
C53A N50 C51B 73.2(5) . 7_545 ?
C51B N50 C51B 105.4(10) . 7_545 ?
N50 C51A C52A 113.5(2) . . ?
N50 C51A H51A 108.9 . . ?
C52A C51A H51A 108.9 . . ?
N50 C51A H51B 108.9 . . ?
C52A C51A H51B 108.9 . . ?
H51A C51A H51B 107.7 . . ?
C51A C52A H52A 109.5 . . ?
C51A C52A H52B 109.5 . . ?
H52A C52A H52B 109.5 . . ?
C51A C52A H52C 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C54A C53A N50 114.5(2) . . ?
C54A C53A H53A 108.6 . . ?
N50 C53A H53A 108.6 . . ?
C54A C53A H53B 108.6 . . ?
N50 C53A H53B 108.6 . . ?
H53A C53A H53B 107.6 . . ?
C53A C54A H54A 109.5 . . ?
C53A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C53A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
N50 C51B H51C 109.7 . . ?
N50 C51B H51D 109.7 . . ?
H51C C51B H51D 108.2 . . ?
N50 C53B C54B 114.4(10) . . ?
N50 C53B H53C 108.7 . . ?
C54B C53B H53C 108.7 . . ?
N50 C53B H53D 108.7 . . ?
C54B C53B H53D 108.7 . . ?
H53C C53B H53D 107.6 . . ?
C53B C54B H54D 109.5 . . ?
C53B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C53B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 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 N2 2.0850(18) . ?
Ni1 N2 2.0850(18) 12 ?
Ni1 N1 2.085(2) . ?
Ni1 N4 2.087(3) . ?
Ni1 N3 2.0964(18) . ?
Ni1 N3 2.0964(18) 12 ?
S1 C1 1.649(3) . ?
S2 C2 1.643(2) . ?
S3 C3 1.645(2) . ?
S4 C4 1.641(3) . ?
N1 C1 1.149(4) . ?
N2 C2 1.149(3) . ?
N3 C3 1.154(3) . ?
N4 C4 1.154(4) . ?
Ni2 N6 2.080(3) 9 ?
Ni2 N6 2.080(3) . ?
Ni2 N5 2.0806(19) 12 ?
Ni2 N5 2.0806(19) . ?
Ni2 N5 2.0806(19) 9 ?
Ni2 N5 2.0806(19) 4 ?
S5 C5 1.641(2) . ?
S6 C6 1.642(3) . ?
N5 C5 1.154(3) . ?
N6 C6 1.159(4) . ?
N10 C13 1.515(3) . ?
N10 C15 1.516(3) . ?
N10 C11 1.519(2) 12 ?
N10 C11 1.519(2) . ?
C11 C12 1.511(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.504(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.511(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N20 C23 1.511(3) . ?
N20 C25 1.513(3) . ?
N20 C21 1.521(2) 12 ?
N20 C21 1.521(2) . ?
C25 C26 1.507(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C21 C22 1.515(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.510(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N30 C31 1.515(2) . ?
N30 C33 1.519(2) . ?
N30 C35 1.521(2) . ?
N30 C37 1.521(2) . ?
C31 C32 1.512(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.516(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.519(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.512(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N40 C45 1.514(3) . ?
N40 C41 1.521(2) 12 ?
N40 C41 1.521(2) . ?
N40 C43 1.524(3) . ?
C41 C42 1.512(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.505(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.504(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
N50 C53B 1.472(12) 7_545 ?
N50 C53B 1.472(12) . ?
N50 C51A 1.500(3) 7_545 ?
N50 C51A 1.500(3) . ?
N50 C53A 1.532(3) 7_545 ?
N50 C53A 1.532(3) . ?
N50 C51B 1.571(13) . ?
N50 C51B 1.571(13) 7_545 ?
C51A C52A 1.547(4) . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C53A C54A 1.515(4) . ?
C53A H53A 0.9900 . ?
C53A H53B 0.9900 . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C51B H51C 0.9900 . ?
C51B H51D 0.9900 . ?
C53B C54B 1.513(18) . ?
C53B H53C 0.9900 . ?
C53B H53D 0.9900 . ?
C54B H54D 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54F 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
C13 N10 C11 C12 -59.8(2) . . . . ?
C15 N10 C11 C12 58.0(3) . . . . ?
C11 N10 C11 C12 179.51(13) 12 . . . ?
C15 N10 C13 C14 180.0 . . . . ?
C11 N10 C13 C14 58.90(14) 12 . . . ?
C11 N10 C13 C14 -58.90(14) . . . . ?
C13 N10 C15 C16 180.0 . . . . ?
C11 N10 C15 C16 -59.22(14) 12 . . . ?
C11 N10 C15 C16 59.21(14) . . . . ?
C23 N20 C25 C26 180.0 . . . . ?
C21 N20 C25 C26 -58.97(13) 12 . . . ?
C21 N20 C25 C26 58.97(13) . . . . ?
C23 N20 C21 C22 -62.7(2) . . . . ?
C25 N20 C21 C22 55.7(2) . . . . ?
C21 N20 C21 C22 176.57(13) 12 . . . ?
C25 N20 C23 C24 180.0 . . . . ?
C21 N20 C23 C24 58.96(13) 12 . . . ?
C21 N20 C23 C24 -58.96(13) . . . . ?
C33 N30 C31 C32 -179.32(18) . . . . ?
C35 N30 C31 C32 59.7(2) . . . . ?
C37 N30 C31 C32 -58.2(2) . . . . ?
C31 N30 C33 C34 -178.28(18) . . . . ?
C35 N30 C33 C34 -57.1(2) . . . . ?
C37 N30 C33 C34 60.6(2) . . . . ?
C31 N30 C35 C36 60.8(2) . . . . ?
C33 N30 C35 C36 -57.4(2) . . . . ?
C37 N30 C35 C36 -178.20(18) . . . . ?
C31 N30 C37 C38 -55.8(2) . . . . ?
C33 N30 C37 C38 62.5(2) . . . . ?
C35 N30 C37 C38 -176.88(18) . . . . ?
C45 N40 C41 C42 57.3(2) . . . . ?
C41 N40 C41 C42 177.68(12) 12 . . . ?
C43 N40 C41 C42 -61.4(2) . . . . ?
C45 N40 C43 C44 180.0 . . . . ?
C41 N40 C43 C44 59.09(13) 12 . . . ?
C41 N40 C43 C44 -59.09(13) . . . . ?
C41 N40 C45 C46 -58.88(13) 12 . . . ?
C41 N40 C45 C46 58.88(13) . . . . ?
C43 N40 C45 C46 180.0 . . . . ?
C51A N50 C51A C52A 59.6(2) 7_545 . . . ?
C53A N50 C51A C52A -60.1(3) 7_545 . . . ?
C53A N50 C51A C52A -178.2(2) . . . . ?
C51A N50 C53A C54A -61.1(3) 7_545 . . . ?
C51A N50 C53A C54A 175.5(3) . . . . ?
C53A N50 C53A C54A 55.8(2) 7_545 . . . ?
C53B N50 C53B C54B -53.7(9) 7_545 . . . ?
C51B N50 C53B C54B -179.1(10) . . . . ?
C51B N50 C53B C54B 67.4(12) 7_545 . . . ?
