#------------------------------------------------------------------------------
#$Date: 2022-11-08 21:23:43 +0200 (Tue, 08 Nov 2022) $
#$Revision: 279108 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/42/2244209.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2244209
loop_
_publ_author_name
'Krebs, Christoph'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Syntheses and crystal structures of the ethanol, acetonitrile and diethyl
 ether Werner clathrates
 bis(isothiocyanato-κN)tetrakis(3-methylpyridine-κN)nickel(II)
;
_journal_coeditor_code           HB8036
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              993
_journal_page_last               998
_journal_paper_doi               10.1107/S2056989022008891
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Ni (N C S )2 (C6 H7 N )4], C4 H10 O'
_chemical_formula_moiety         'C26 H28 N6 Ni S2, C4 H10 O'
_chemical_formula_sum            'C30 H38 N6 Ni O S2'
_chemical_formula_weight         621.49
_chemical_name_systematic
;
Bis(isothiocyanato-κN)tetrakis(3-methylpyridine-κN)\
nickel(II) diethyl ether monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2275(10)
_cell_length_b                   25.04680(10)
_cell_length_c                   12.71800(10)
_cell_measurement_reflns_used    43692
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      78.9940
_cell_measurement_theta_min      3.4710
_cell_volume                     3247.4(3)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      99.97(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0079
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            56224
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.642
_diffrn_reflns_theta_min         3.529
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.317
_refine_ls_extinction_coef       0.00020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2016/6 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0356P)²+1.9652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                6907
_reflns_number_total             6974
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb8036sup1.cif
_cod_data_source_block           3
_cod_database_code               2244209
_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_min   0.655
_shelx_estimated_absorpt_t_max   0.723
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.24076(2) 0.61197(2) 0.27926(2) 0.01630(7) Uani d 1 . .
N N1 0.24400(11) 0.60562(4) 0.44028(9) 0.0217(2) Uani d 1 . .
C C1 0.24082(12) 0.62304(5) 0.52491(10) 0.0188(2) Uani d 1 . .
S S1 0.23850(4) 0.64887(2) 0.64199(3) 0.03244(9) Uani d 1 . .
N N2 0.23270(11) 0.61727(4) 0.11760(9) 0.0209(2) Uani d 1 . .
C C2 0.26680(12) 0.62259(5) 0.03386(10) 0.0195(2) Uani d 1 . .
S S2 0.31719(4) 0.63063(2) -0.08404(3) 0.02805(9) Uani d 1 . .
N N11 0.11637(10) 0.54346(4) 0.26359(8) 0.0182(2) Uani d 1 . .
C C11 0.12071(12) 0.51046(5) 0.18089(10) 0.0195(2) Uani d 1 . .
H H11 0.180894 0.518406 0.129934 0.023 Uiso calc 1 . .
C C12 0.04240(12) 0.46529(5) 0.16522(10) 0.0212(2) Uani d 1 . .
C C13 -0.04471(13) 0.45407(5) 0.24070(11) 0.0252(3) Uani d 1 . .
H H13 -0.100594 0.423786 0.233060 0.030 Uiso calc 1 . .
C C14 -0.04931(13) 0.48748(6) 0.32726(11) 0.0259(3) Uani d 1 . .
H H14 -0.107695 0.480129 0.379882 0.031 Uiso calc 1 . .
C C15 0.03222(12) 0.53170(5) 0.33612(10) 0.0218(2) Uani d 1 . .
H H15 0.028503 0.554484 0.395516 0.026 Uiso calc 1 . .
C C16 0.05390(14) 0.42992(6) 0.07075(11) 0.0286(3) Uani d 1 . .
H H16A 0.090667 0.450425 0.014493 0.043 Uiso calc 1 . .
H H16B -0.033150 0.416564 0.045699 0.043 Uiso calc 1 . .
H H16C 0.111655 0.399722 0.090543 0.043 Uiso calc 1 . .
N N21 0.40489(10) 0.55986(4) 0.27878(8) 0.0181(2) Uani d 1 . .
C C21 0.48770(12) 0.56126(5) 0.20234(10) 0.0209(2) Uani d 1 . .
H H21 0.479956 0.589974 0.153433 0.025 Uiso calc 1 . .
C C22 0.58430(13) 0.52316(5) 0.19038(11) 0.0249(3) Uani d 1 . .
C C23 0.59499(13) 0.48144(5) 0.26294(11) 0.0251(3) Uani d 1 . .
H H23 0.658347 0.454105 0.256871 0.030 Uiso calc 1 . .
C C24 0.51244(13) 0.48016(5) 0.34399(11) 0.0240(3) Uani d 1 . .
H H24 0.519758 0.452469 0.395165 0.029 Uiso calc 1 . .
C C25 0.41891(12) 0.51993(5) 0.34931(10) 0.0208(2) Uani d 1 . .
H H25 0.362470 0.518900 0.405078 0.025 Uiso calc 1 . .
C C26 0.67263(16) 0.52747(7) 0.10169(14) 0.0393(4) Uani d 1 . .
H H26A 0.632509 0.551229 0.046997 0.059 Uiso calc 1 . .
H H26B 0.685163 0.492004 0.071558 0.059 Uiso calc 1 . .
H H26C 0.757741 0.541995 0.128735 0.059 Uiso calc 1 . .
N N31 0.36520(10) 0.68134(4) 0.29236(8) 0.0190(2) Uani d 1 . .
C C31 0.44241(12) 0.69197(5) 0.38051(10) 0.0206(2) Uani d 1 . .
H H31 0.445853 0.666502 0.436028 0.025 Uiso calc 1 . .
C C32 0.51760(12) 0.73812(5) 0.39515(10) 0.0220(3) Uani d 1 . .
C C33 0.51474(13) 0.77437(5) 0.31195(11) 0.0240(3) Uani d 1 . .
H H33 0.565253 0.806207 0.318239 0.029 Uiso calc 1 . .
C C34 0.43767(14) 0.76355(5) 0.22017(11) 0.0262(3) Uani d 1 . .
H H34 0.435711 0.787548 0.162214 0.031 Uiso calc 1 . .
C C35 0.36329(13) 0.71725(5) 0.21377(11) 0.0238(3) Uani d 1 . .
H H35 0.308631 0.710622 0.151170 0.029 Uiso calc 1 . .
C C36 0.59863(15) 0.74773(6) 0.49744(12) 0.0310(3) Uani d 1 . .
H H36A 0.567883 0.780167 0.530802 0.046 Uiso calc 1 . .
H H36B 0.690902 0.752064 0.483540 0.046 Uiso calc 1 . .
H H36C 0.589876 0.717217 0.544596 0.046 Uiso calc 1 . .
N N41 0.07440(10) 0.66297(4) 0.28090(9) 0.0202(2) Uani d 1 . .
C C41 -0.02476(13) 0.65985(5) 0.20552(11) 0.0228(3) Uani d 1 . .
H H41 -0.020280 0.633303 0.152574 0.027 Uiso calc 1 . .
C C42 -0.13370(13) 0.69318(6) 0.20032(12) 0.0277(3) Uani d 1 . .
C C43 -0.13848(14) 0.73168(5) 0.27870(12) 0.0291(3) Uani d 1 . .
H H43 -0.211005 0.755405 0.278184 0.035 Uiso calc 1 . .
C C44 -0.03766(15) 0.73536(5) 0.35720(12) 0.0291(3) Uani d 1 . .
H H44 -0.040057 0.761438 0.411257 0.035 Uiso calc 1 . .
C C45 0.06728(14) 0.70034(5) 0.35589(11) 0.0252(3) Uani d 1 . .
H H45 0.136618 0.702897 0.410014 0.030 Uiso calc 1 . .
C C46 -0.24086(16) 0.68799(8) 0.11234(16) 0.0458(4) Uani d 1 . .
H H46A -0.215254 0.661426 0.061268 0.069 Uiso calc 1 . .
H H46B -0.254755 0.722555 0.077099 0.069 Uiso calc 1 . .
H H46C -0.322232 0.676613 0.141465 0.069 Uiso calc 1 . .
O O1 0.69662(10) 0.62578(4) 0.59182(9) 0.0317(2) Uani d 1 . .
C C51 0.73601(16) 0.60727(7) 0.41488(14) 0.0366(3) Uani d 1 . .
H H51A 0.795731 0.589524 0.369494 0.055 Uiso calc 1 . .
H H51B 0.732205 0.645494 0.398425 0.055 Uiso calc 1 . .
H H51C 0.648145 0.591754 0.402625 0.055 Uiso calc 1 . .
C C52 0.78480(15) 0.59971(6) 0.52804(14) 0.0347(3) Uani d 1 . .
H H52A 0.789405 0.561178 0.545302 0.042 Uiso calc 1 . .
H H52B 0.873782 0.615096 0.541081 0.042 Uiso calc 1 . .
C C53 0.72920(16) 0.61857(6) 0.70157(13) 0.0343(3) Uani d 1 . .
H H53A 0.820988 0.629759 0.720164 0.041 Uiso calc 1 . .
H H53B 0.720701 0.580448 0.720396 0.041 Uiso calc 1 . .
C C54 0.63737(18) 0.65180(8) 0.76094(14) 0.0444(4) Uani d 1 . .
H H54A 0.546535 0.642006 0.738825 0.067 Uiso calc 1 . .
H H54B 0.651052 0.689678 0.745921 0.067 Uiso calc 1 . .
H H54C 0.654630 0.645388 0.836800 0.067 Uiso calc 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 N2 . . 178.45(4) ?
N1 Ni1 N11 . . 89.58(4) ?
N1 Ni1 N21 . . 90.33(4) ?
N1 Ni1 N31 . . 91.33(4) ?
N1 Ni1 N41 . . 89.18(4) ?
N2 Ni1 N11 . . 89.02(4) ?
N2 Ni1 N21 . . 90.29(4) ?
N2 Ni1 N31 . . 90.07(4) ?
N2 Ni1 N41 . . 90.18(4) ?
N11 Ni1 N31 . . 179.05(4) ?
N21 Ni1 N11 . . 88.35(4) ?
N21 Ni1 N31 . . 91.93(4) ?
N21 Ni1 N41 . . 178.94(4) ?
N41 Ni1 N11 . . 90.72(4) ?
N41 Ni1 N31 . . 89.02(4) ?
C1 N1 Ni1 . . 153.43(10) ?
N1 C1 S1 . . 178.36(12) ?
C2 N2 Ni1 . . 159.93(10) ?
N2 C2 S2 . . 179.10(13) ?
C11 N11 Ni1 . . 120.75(8) ?
C11 N11 C15 . . 117.80(11) ?
C15 N11 Ni1 . . 121.44(8) ?
N11 C11 H11 . . 118.0 ?
N11 C11 C12 . . 123.96(12) ?
C12 C11 H11 . . 118.0 ?
C11 C12 C16 . . 120.81(12) ?
C13 C12 C11 . . 117.33(12) ?
C13 C12 C16 . . 121.86(12) ?
C12 C13 H13 . . 120.3 ?
C14 C13 C12 . . 119.39(12) ?
C14 C13 H13 . . 120.3 ?
C13 C14 H14 . . 120.4 ?
C15 C14 C13 . . 119.24(12) ?
C15 C14 H14 . . 120.4 ?
N11 C15 C14 . . 122.27(12) ?
N11 C15 H15 . . 118.9 ?
C14 C15 H15 . . 118.9 ?
C12 C16 H16A . . 109.5 ?
C12 C16 H16B . . 109.5 ?
C12 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C21 N21 Ni1 . . 122.07(8) ?
C21 N21 C25 . . 117.64(11) ?
C25 N21 Ni1 . . 119.80(8) ?
N21 C21 H21 . . 118.1 ?
N21 C21 C22 . . 123.87(12) ?
C22 C21 H21 . . 118.1 ?
C21 C22 C23 . . 117.46(12) ?
C21 C22 C26 . . 120.49(13) ?
C23 C22 C26 . . 122.06(12) ?
C22 C23 H23 . . 120.3 ?
C24 C23 C22 . . 119.38(12) ?
C24 C23 H23 . . 120.3 ?
C23 C24 H24 . . 120.5 ?
C23 C24 C25 . . 118.96(12) ?
C25 C24 H24 . . 120.5 ?
N21 C25 C24 . . 122.64(12) ?
N21 C25 H25 . . 118.7 ?
C24 C25 H25 . . 118.7 ?
C22 C26 H26A . . 109.5 ?
C22 C26 H26B . . 109.5 ?
C22 C26 H26C . . 109.5 ?
H26A C26 H26B . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
C31 N31 Ni1 . . 121.89(8) ?
C35 N31 Ni1 . . 120.64(9) ?
C35 N31 C31 . . 117.39(11) ?
N31 C31 H31 . . 118.1 ?
N31 C31 C32 . . 123.82(12) ?
C32 C31 H31 . . 118.1 ?
C31 C32 C33 . . 117.51(12) ?
C31 C32 C36 . . 120.55(12) ?
C33 C32 C36 . . 121.94(12) ?
C32 C33 H33 . . 120.3 ?
C34 C33 C32 . . 119.32(12) ?
C34 C33 H33 . . 120.3 ?
C33 C34 H34 . . 120.4 ?
C33 C34 C35 . . 119.14(13) ?
C35 C34 H34 . . 120.4 ?
N31 C35 C34 . . 122.78(12) ?
N31 C35 H35 . . 118.6 ?
C34 C35 H35 . . 118.6 ?
C32 C36 H36A . . 109.5 ?
C32 C36 H36B . . 109.5 ?
C32 C36 H36C . . 109.5 ?
H36A C36 H36B . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
C41 N41 Ni1 . . 121.14(9) ?
C41 N41 C45 . . 117.88(11) ?
C45 N41 Ni1 . . 120.95(9) ?
N41 C41 H41 . . 118.1 ?
N41 C41 C42 . . 123.82(13) ?
C42 C41 H41 . . 118.1 ?
C41 C42 C43 . . 117.17(13) ?
C41 C42 C46 . . 121.06(14) ?
C43 C42 C46 . . 121.76(13) ?
C42 C43 H43 . . 120.1 ?
C44 C43 C42 . . 119.85(13) ?
C44 C43 H43 . . 120.1 ?
C43 C44 H44 . . 120.6 ?
C43 C44 C45 . . 118.89(13) ?
C45 C44 H44 . . 120.6 ?
N41 C45 C44 . . 122.38(13) ?
N41 C45 H45 . . 118.8 ?
C44 C45 H45 . . 118.8 ?
C42 C46 H46A . . 109.5 ?
C42 C46 H46B . . 109.5 ?
C42 C46 H46C . . 109.5 ?
H46A C46 H46B . . 109.5 ?
H46A C46 H46C . . 109.5 ?
H46B C46 H46C . . 109.5 ?
C52 O1 C53 . . 113.17(12) ?
H51A C51 H51B . . 109.5 ?
H51A C51 H51C . . 109.5 ?
H51B C51 H51C . . 109.5 ?
C52 C51 H51A . . 109.5 ?
C52 C51 H51B . . 109.5 ?
C52 C51 H51C . . 109.5 ?
O1 C52 C51 . . 108.25(12) ?
O1 C52 H52A . . 110.0 ?
O1 C52 H52B . . 110.0 ?
C51 C52 H52A . . 110.0 ?
C51 C52 H52B . . 110.0 ?
H52A C52 H52B . . 108.4 ?
O1 C53 H53A . . 110.0 ?
O1 C53 H53B . . 110.0 ?
O1 C53 C54 . . 108.46(13) ?
H53A C53 H53B . . 108.4 ?
C54 C53 H53A . . 110.0 ?
C54 C53 H53B . . 110.0 ?
C53 C54 H54A . . 109.5 ?
C53 C54 H54B . . 109.5 ?
C53 C54 H54C . . 109.5 ?
H54A C54 H54B . . 109.5 ?
H54A C54 H54C . . 109.5 ?
H54B C54 H54C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 . 2.0517(11) y
Ni1 N2 . 2.0552(11) y
Ni1 N11 . 2.1358(10) y
Ni1 N21 . 2.1266(10) y
Ni1 N31 . 2.1523(11) y
Ni1 N41 . 2.1291(11) y
N1 C1 . 1.1643(17) ?
C1 S1 . 1.6254(13) ?
N2 C2 . 1.1546(18) ?
C2 S2 . 1.6366(13) ?
N11 C11 . 1.3413(16) ?
N11 C15 . 1.3437(16) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.3912(17) ?
C12 C13 . 1.3898(19) ?
C12 C16 . 1.5050(18) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.387(2) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.3855(18) ?
C15 H15 . 0.9500 ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
N21 C21 . 1.3400(16) ?
N21 C25 . 1.3436(16) ?
C21 H21 . 0.9500 ?
C21 C22 . 1.3907(18) ?
C22 C23 . 1.3927(19) ?
C22 C26 . 1.5045(19) ?
C23 H23 . 0.9500 ?
C23 C24 . 1.3841(19) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.3864(18) ?
C25 H25 . 0.9500 ?
C26 H26A . 0.9800 ?
C26 H26B . 0.9800 ?
C26 H26C . 0.9800 ?
N31 C31 . 1.3452(16) ?
N31 C35 . 1.3437(17) ?
C31 H31 . 0.9500 ?
C31 C32 . 1.3926(18) ?
C32 C33 . 1.3928(19) ?
C32 C36 . 1.5047(18) ?
C33 H33 . 0.9500 ?
C33 C34 . 1.382(2) ?
C34 H34 . 0.9500 ?
C34 C35 . 1.3858(19) ?
C35 H35 . 0.9500 ?
C36 H36A . 0.9800 ?
C36 H36B . 0.9800 ?
C36 H36C . 0.9800 ?
N41 C41 . 1.3409(17) ?
N41 C45 . 1.3423(17) ?
C41 H41 . 0.9500 ?
C41 C42 . 1.3894(18) ?
C42 C43 . 1.391(2) ?
C42 C46 . 1.508(2) ?
C43 H43 . 0.9500 ?
C43 C44 . 1.380(2) ?
C44 H44 . 0.9500 ?
C44 C45 . 1.3872(19) ?
C45 H45 . 0.9500 ?
C46 H46A . 0.9800 ?
C46 H46B . 0.9800 ?
C46 H46C . 0.9800 ?
O1 C52 . 1.4195(19) ?
O1 C53 . 1.4202(19) ?
C51 H51A . 0.9800 ?
C51 H51B . 0.9800 ?
C51 H51C . 0.9800 ?
C51 C52 . 1.497(2) ?
C52 H52A . 0.9900 ?
C52 H52B . 0.9900 ?
C53 H53A . 0.9900 ?
C53 H53B . 0.9900 ?
C53 C54 . 1.503(2) ?
C54 H54A . 0.9800 ?
C54 H54B . 0.9800 ?
C54 H54C . 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ni1 N11 C11 C12 . . . . -179.71(9) ?
Ni1 N11 C15 C14 . . . . 179.93(10) ?
Ni1 N21 C21 C22 . . . . -170.21(10) ?
Ni1 N21 C25 C24 . . . . 170.56(10) ?
Ni1 N31 C31 C32 . . . . -175.46(9) ?
Ni1 N31 C35 C34 . . . . 177.39(10) ?
Ni1 N41 C41 C42 . . . . -177.75(10) ?
Ni1 N41 C45 C44 . . . . 177.81(10) ?
N11 C11 C12 C13 . . . . -0.29(19) ?
N11 C11 C12 C16 . . . . -179.46(12) ?
C11 N11 C15 C14 . . . . -0.57(18) ?
C11 C12 C13 C14 . . . . -0.44(19) ?
C12 C13 C14 C15 . . . . 0.6(2) ?
C13 C14 C15 N11 . . . . -0.1(2) ?
C15 N11 C11 C12 . . . . 0.79(18) ?
C16 C12 C13 C14 . . . . 178.71(13) ?
N21 C21 C22 C23 . . . . -0.3(2) ?
N21 C21 C22 C26 . . . . 179.49(14) ?
C21 N21 C25 C24 . . . . -1.63(18) ?
C21 C22 C23 C24 . . . . -1.4(2) ?
C22 C23 C24 C25 . . . . 1.5(2) ?
C23 C24 C25 N21 . . . . 0.0(2) ?
C25 N21 C21 C22 . . . . 1.80(19) ?
C26 C22 C23 C24 . . . . 178.84(14) ?
N31 C31 C32 C33 . . . . -1.89(19) ?
N31 C31 C32 C36 . . . . 178.29(12) ?
C31 N31 C35 C34 . . . . 0.66(19) ?
C31 C32 C33 C34 . . . . 0.66(19) ?
C32 C33 C34 C35 . . . . 1.1(2) ?
C33 C34 C35 N31 . . . . -1.8(2) ?
C35 N31 C31 C32 . . . . 1.23(19) ?
C36 C32 C33 C34 . . . . -179.52(13) ?
N41 C41 C42 C43 . . . . -0.1(2) ?
N41 C41 C42 C46 . . . . 179.09(14) ?
C41 N41 C45 C44 . . . . -0.3(2) ?
C41 C42 C43 C44 . . . . -0.2(2) ?
C42 C43 C44 C45 . . . . 0.2(2) ?
C43 C44 C45 N41 . . . . 0.0(2) ?
C45 N41 C41 C42 . . . . 0.4(2) ?
C46 C42 C43 C44 . . . . -179.38(15) ?
C52 O1 C53 C54 . . . . 174.86(13) ?
C53 O1 C52 C51 . . . . 176.55(12) ?

_cod_database_fobs_code 2244209
