#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:26:07 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180393 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/62/7206272.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_7206272
loop_
_publ_author_name
'Chen, Haiyan'
'Xiao, Dongrong'
'He, Jianghong'
'Li, Zhifu'
'Zhang, Guangju'
'Sun, Dianzhen'
'Yuan, Ruo'
'Wang, Enbo'
'Luo, Qun-Li'
_publ_section_title
;
 A series of novel entangled coordination frameworks with inherent
 features of self-threading, polyrotaxane and polycatenane
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              4988
_journal_paper_doi               10.1039/c1ce05254c
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C24 H30 N4 Ni O10 S'
_chemical_formula_weight         625.29
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.84(3)
_cell_angle_beta                 79.36(3)
_cell_angle_gamma                86.47(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2542(19)
_cell_length_b                   12.022(2)
_cell_length_c                   13.235(3)
_cell_measurement_reflns_used    8066
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      1.58
_cell_volume                     1427.9(5)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega 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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8066
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.7266
_exptl_absorpt_correction_T_min  0.6681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.42
_refine_diff_density_max         1.345
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5751
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1700P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2130
_reflns_number_gt                4990
_reflns_number_total             5751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05254c.txt
_cod_data_source_block           c2b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7206272
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.47784(4) 0.34180(3) -0.18773(3) 0.02482(19) Uani 1 1 d . . .
S1 S 0.22863(10) -0.11754(8) -0.42763(6) 0.0377(3) Uani 1 1 d . . .
O1 O -0.3022(2) 0.2447(2) -0.24866(18) 0.0326(5) Uani 1 1 d . . .
OW1 O -0.6482(3) 0.4471(2) -0.12667(19) 0.0334(5) Uani 1 1 d D . .
O2 O -0.1077(3) 0.3381(2) -0.2345(2) 0.0437(6) Uani 1 1 d . . .
OW2 O -0.3439(3) 0.4835(2) -0.22458(18) 0.0322(5) Uani 1 1 d D . .
OW3 O -0.9222(4) 0.3623(4) 0.0968(3) 0.0834(12) Uani 1 1 d . . .
O3 O 0.6127(2) -0.3791(2) -0.06759(17) 0.0356(5) Uani 1 1 d . . .
OW4 O 0.0552(4) 0.4219(5) -0.1162(4) 0.0832(13) Uani 1 1 d DU . .
O4 O 0.4133(3) -0.3172(2) 0.03592(17) 0.0339(5) Uani 1 1 d . . .
O5 O 0.1356(3) -0.1996(2) -0.4495(2) 0.0495(7) Uani 1 1 d . . .
O6 O 0.3447(3) -0.0696(3) -0.5076(2) 0.0504(7) Uani 1 1 d . . .
N1 N -0.5906(3) 0.1925(2) -0.1412(2) 0.0316(6) Uani 1 1 d . . .
N2 N -0.7152(4) 0.0534(3) -0.0423(3) 0.0461(8) Uani 1 1 d . . .
N3 N -0.5516(3) 0.3751(2) -0.3295(2) 0.0300(6) Uani 1 1 d . . .
N4 N -0.6831(3) 0.4493(3) -0.4483(2) 0.0333(6) Uani 1 1 d . . .
C1 C 0.1771(4) 0.0896(3) -0.3651(3) 0.0393(8) Uani 1 1 d . . .
H1A H 0.2784 0.0974 -0.3825 0.047 Uiso 1 1 calc R . .
C2 C 0.0864(4) 0.1743(3) -0.3241(3) 0.0362(8) Uani 1 1 d . . .
H2A H 0.1275 0.2391 -0.3131 0.043 Uiso 1 1 calc R . .
C3 C -0.0658(4) 0.1626(3) -0.2993(2) 0.0293(7) Uani 1 1 d . . .
C4 C -0.1264(4) 0.0663(3) -0.3163(3) 0.0342(7) Uani 1 1 d . . .
H4A H -0.2279 0.0594 -0.3016 0.041 Uiso 1 1 calc R . .
C5 C -0.0379(4) -0.0201(3) -0.3549(3) 0.0367(8) Uani 1 1 d . . .
H5A H -0.0785 -0.0858 -0.3641 0.044 Uiso 1 1 calc R . .
C6 C 0.1139(4) -0.0060(3) -0.3796(3) 0.0323(7) Uani 1 1 d . . .
C7 C 0.3077(4) -0.1800(3) -0.3182(3) 0.0343(7) Uani 1 1 d . . .
C8 C 0.2146(4) -0.2340(3) -0.2314(3) 0.0372(8) Uani 1 1 d . . .
H8A H 0.1148 -0.2387 -0.2321 0.045 Uiso 1 1 calc R . .
C9 C 0.2732(4) -0.2807(3) -0.1440(3) 0.0325(7) Uani 1 1 d . . .
H9A H 0.2117 -0.3130 -0.0841 0.039 Uiso 1 1 calc R . .
C10 C 0.4245(4) -0.2791(3) -0.1464(2) 0.0288(7) Uani 1 1 d . . .
C11 C 0.5161(4) -0.2284(3) -0.2357(3) 0.0384(8) Uani 1 1 d . . .
H11A H 0.6172 -0.2299 -0.2379 0.046 Uiso 1 1 calc R . .
C12 C 0.4576(4) -0.1759(3) -0.3213(3) 0.0388(8) Uani 1 1 d . . .
H12A H 0.5180 -0.1389 -0.3794 0.047 Uiso 1 1 calc R . .
C13 C -0.1647(3) 0.2567(3) -0.2569(2) 0.0279(6) Uani 1 1 d . . .
C14 C 0.4877(4) -0.3297(3) -0.0513(2) 0.0298(7) Uani 1 1 d . . .
C15 C -0.6814(4) 0.1610(3) -0.0525(3) 0.0427(9) Uani 1 1 d . . .
H15A H -0.7170 0.2083 -0.0036 0.051 Uiso 1 1 calc R . .
C16 C -0.5676(5) 0.1003(3) -0.1887(3) 0.0507(11) Uani 1 1 d . . .
H16A H -0.5090 0.0969 -0.2533 0.061 Uiso 1 1 calc R . .
C17 C -0.6423(5) 0.0134(4) -0.1284(4) 0.0657(14) Uani 1 1 d . . .
H17A H -0.6435 -0.0596 -0.1432 0.079 Uiso 1 1 calc R . .
C18 C -0.8117(6) -0.0114(5) 0.0469(4) 0.0690(15) Uani 1 1 d . . .
H18A H -0.8391 0.0346 0.1018 0.083 Uiso 1 1 calc R . .
H18B H -0.7576 -0.0777 0.0740 0.083 Uiso 1 1 calc R . .
C19 C -0.9510(6) -0.0479(5) 0.0163(4) 0.0721(15) Uani 1 1 d . . .
H19A H -0.9231 -0.0916 -0.0403 0.087 Uiso 1 1 calc R . .
H19B H -1.0049 -0.0964 0.0750 0.087 Uiso 1 1 calc R . .
C20 C -0.6510(4) 0.4539(3) -0.3539(3) 0.0338(7) Uani 1 1 d . . .
H20A H -0.6933 0.5059 -0.3112 0.041 Uiso 1 1 calc R . .
C21 C -0.5197(4) 0.3175(3) -0.4129(3) 0.0356(7) Uani 1 1 d . . .
H21A H -0.4529 0.2568 -0.4184 0.043 Uiso 1 1 calc R . .
C22 C -0.6007(4) 0.3627(3) -0.4863(3) 0.0386(8) Uani 1 1 d . . .
H22A H -0.5999 0.3389 -0.5499 0.046 Uiso 1 1 calc R . .
C23 C -0.7949(4) 0.5201(3) -0.4974(3) 0.0410(8) Uani 1 1 d . . .
H23A H -0.7607 0.5356 -0.5719 0.049 Uiso 1 1 calc R . .
H23B H -0.8082 0.5915 -0.4709 0.049 Uiso 1 1 calc R . .
C24 C -0.9409(4) 0.4626(3) -0.4759(3) 0.0452(9) Uani 1 1 d . . .
H24A H -0.9736 0.4450 -0.4013 0.054 Uiso 1 1 calc R . .
H24B H -0.9281 0.3923 -0.5041 0.054 Uiso 1 1 calc R . .
HW2A H -0.363(5) 0.531(3) -0.183(3) 0.078(18) Uiso 1 1 d D . .
HW1B H -0.7358(18) 0.440(4) -0.134(2) 0.041(11) Uiso 1 1 d D . .
HW2B H -0.259(2) 0.456(4) -0.223(4) 0.063(15) Uiso 1 1 d D . .
HW1A H -0.643(4) 0.430(3) -0.0632(11) 0.040(11) Uiso 1 1 d D . .
HW4B H 0.028(8) 0.4904(17) -0.126(6) 0.12(3) Uiso 1 1 d D . .
HW4A H 0.012(7) 0.386(4) -0.150(5) 0.11(2) Uiso 1 1 d D . .
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'
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'
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
O1 Ni1 N1 86.60(10) . . ?
O1 Ni1 N3 91.86(10) . . ?
N1 Ni1 N3 93.35(12) . . ?
O1 Ni1 OW1 176.98(9) . . ?
N1 Ni1 OW1 96.31(11) . . ?
N3 Ni1 OW1 88.77(11) . . ?
O1 Ni1 OW2 89.45(9) . . ?
N1 Ni1 OW2 172.99(10) . . ?
N3 Ni1 OW2 92.57(10) . . ?
OW1 Ni1 OW2 87.57(10) . . ?
O1 Ni1 O4 92.54(9) . 2 ?
N1 Ni1 O4 87.75(11) . 2 ?
N3 Ni1 O4 175.52(9) . 2 ?
OW1 Ni1 O4 86.79(10) . 2 ?
OW2 Ni1 O4 86.64(10) . 2 ?
O6 S1 O5 119.80(18) . . ?
O6 S1 C7 108.19(17) . . ?
O5 S1 C7 107.56(17) . . ?
O6 S1 C6 108.72(17) . . ?
O5 S1 C6 108.22(17) . . ?
C7 S1 C6 103.09(16) . . ?
C13 O1 Ni1 130.2(2) . . ?
Ni1 OW1 HW1B 121(3) . . ?
Ni1 OW1 HW1A 99(3) . . ?
HW1B OW1 HW1A 108.4(16) . . ?
Ni1 OW2 HW2A 115(4) . . ?
Ni1 OW2 HW2B 104(3) . . ?
HW2A OW2 HW2B 109.0(17) . . ?
HW4B OW4 HW4A 108.8(18) . . ?
C14 O4 Ni1 129.9(2) . 2 ?
C15 N1 C16 105.2(3) . . ?
C15 N1 Ni1 128.1(2) . . ?
C16 N1 Ni1 126.0(2) . . ?
C15 N2 C17 106.8(3) . . ?
C15 N2 C18 126.8(4) . . ?
C17 N2 C18 126.4(4) . . ?
C20 N3 C21 105.1(3) . . ?
C20 N3 Ni1 125.6(2) . . ?
C21 N3 Ni1 129.0(2) . . ?
C20 N4 C22 107.1(3) . . ?
C20 N4 C23 126.1(3) . . ?
C22 N4 C23 126.6(3) . . ?
C6 C1 C2 118.7(3) . . ?
C6 C1 H1A 120.6 . . ?
C2 C1 H1A 120.6 . . ?
C1 C2 C3 120.4(3) . . ?
C1 C2 H2A 119.8 . . ?
C3 C2 H2A 119.8 . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 C13 120.2(3) . . ?
C2 C3 C13 120.2(3) . . ?
C3 C4 C5 121.0(3) . . ?
C3 C4 H4A 119.5 . . ?
C5 C4 H4A 119.5 . . ?
C4 C5 C6 118.3(3) . . ?
C4 C5 H5A 120.8 . . ?
C6 C5 H5A 120.8 . . ?
C1 C6 C5 122.0(3) . . ?
C1 C6 S1 119.4(3) . . ?
C5 C6 S1 118.6(3) . . ?
C12 C7 C8 121.8(3) . . ?
C12 C7 S1 120.2(3) . . ?
C8 C7 S1 118.0(3) . . ?
C9 C8 C7 119.0(3) . . ?
C9 C8 H8A 120.5 . . ?
C7 C8 H8A 120.5 . . ?
C8 C9 C10 119.8(3) . . ?
C8 C9 H9A 120.1 . . ?
C10 C9 H9A 120.1 . . ?
C9 C10 C11 120.0(3) . . ?
C9 C10 C14 119.7(3) . . ?
C11 C10 C14 120.3(3) . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C7 C12 C11 118.6(3) . . ?
C7 C12 H12A 120.7 . . ?
C11 C12 H12A 120.7 . . ?
O2 C13 O1 125.2(3) . . ?
O2 C13 C3 119.1(3) . . ?
O1 C13 C3 115.7(3) . . ?
O4 C14 O3 126.2(3) . . ?
O4 C14 C10 117.4(3) . . ?
O3 C14 C10 116.4(3) . . ?
N1 C15 N2 111.5(3) . . ?
N1 C15 H15A 124.2 . . ?
N2 C15 H15A 124.2 . . ?
N1 C16 C17 109.9(4) . . ?
N1 C16 H16A 125.0 . . ?
C17 C16 H16A 125.0 . . ?
C16 C17 N2 106.6(4) . . ?
C16 C17 H17A 126.7 . . ?
N2 C17 H17A 126.7 . . ?
N2 C18 C19 112.1(4) . . ?
N2 C18 H18A 109.2 . . ?
C19 C18 H18A 109.2 . . ?
N2 C18 H18B 109.2 . . ?
C19 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C19 C19 C18 113.4(6) 2_355 . ?
C19 C19 H19A 108.9 2_355 . ?
C18 C19 H19A 108.9 . . ?
C19 C19 H19B 108.9 2_355 . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
N3 C20 N4 111.6(3) . . ?
N3 C20 H20A 124.2 . . ?
N4 C20 H20A 124.2 . . ?
C22 C21 N3 109.7(3) . . ?
C22 C21 H21A 125.2 . . ?
N3 C21 H21A 125.2 . . ?
N4 C22 C21 106.5(3) . . ?
N4 C22 H22A 126.8 . . ?
C21 C22 H22A 126.8 . . ?
N4 C23 C24 111.4(3) . . ?
N4 C23 H23A 109.4 . . ?
C24 C23 H23A 109.4 . . ?
N4 C23 H23B 109.4 . . ?
C24 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C23 C24 C24 111.6(4) . 2_364 ?
C23 C24 H24A 109.3 . . ?
C24 C24 H24A 109.3 2_364 . ?
C23 C24 H24B 109.3 . . ?
C24 C24 H24B 109.3 2_364 . ?
H24A C24 H24B 108.0 . . ?
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 O1 2.059(2) . ?
Ni1 N1 2.081(3) . ?
Ni1 N3 2.084(3) . ?
Ni1 OW1 2.086(2) . ?
Ni1 OW2 2.109(2) . ?
Ni1 O4 2.171(2) 2 ?
S1 O6 1.438(3) . ?
S1 O5 1.444(3) . ?
S1 C7 1.781(3) . ?
S1 C6 1.783(3) . ?
O1 C13 1.271(4) . ?
OW1 HW1B 0.843(10) . ?
OW1 HW1A 0.842(10) . ?
O2 C13 1.241(4) . ?
OW2 HW2A 0.843(10) . ?
OW2 HW2B 0.837(10) . ?
O3 C14 1.265(4) . ?
OW4 HW4B 0.845(10) . ?
OW4 HW4A 0.83(6) . ?
O4 C14 1.256(4) . ?
O4 Ni1 2.171(2) 2 ?
N1 C15 1.327(4) . ?
N1 C16 1.347(5) . ?
N2 C15 1.330(5) . ?
N2 C17 1.355(6) . ?
N2 C18 1.484(5) . ?
N3 C20 1.323(4) . ?
N3 C21 1.373(4) . ?
N4 C20 1.347(4) . ?
N4 C22 1.359(5) . ?
N4 C23 1.477(4) . ?
C1 C6 1.375(5) . ?
C1 C2 1.393(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.397(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.384(5) . ?
C3 C13 1.521(5) . ?
C4 C5 1.385(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.397(5) . ?
C5 H5A 0.9300 . ?
C7 C12 1.384(5) . ?
C7 C8 1.397(5) . ?
C8 C9 1.391(5) . ?
C8 H8A 0.9300 . ?
C9 C10 1.396(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.397(5) . ?
C10 C14 1.511(4) . ?
C11 C12 1.390(5) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C15 H15A 0.9300 . ?
C16 C17 1.351(6) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C18 C19 1.529(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C19 1.481(11) 2_355 ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9300 . ?
C21 C22 1.360(5) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C24 1.515(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C24 1.538(7) 2_364 ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
OW2 HW2B O2 0.837(10) 1.93(2) 2.711(4) 154(4) .
OW4 HW4A O2 0.83(6) 1.88(2) 2.702(5) 166(6) .
OW2 HW2A O3 0.843(10) 1.980(14) 2.813(3) 169(4) 1_465
OW1 HW1B OW4 0.843(10) 1.927(14) 2.755(4) 167(3) 1_455
OW1 HW1A O3 0.842(10) 1.809(11) 2.645(3) 172(4) 2
OW1 HW1A O4 0.842(10) 2.50(3) 2.925(4) 112(3) 2
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
N1 Ni1 O1 C13 -147.1(3) . . . . ?
N3 Ni1 O1 C13 119.6(3) . . . . ?
OW1 Ni1 O1 C13 17.5(18) . . . . ?
OW2 Ni1 O1 C13 27.1(3) . . . . ?
O4 Ni1 O1 C13 -59.5(3) 2 . . . ?
O1 Ni1 N1 C15 139.8(3) . . . . ?
N3 Ni1 N1 C15 -128.5(3) . . . . ?
OW1 Ni1 N1 C15 -39.4(3) . . . . ?
OW2 Ni1 N1 C15 84.0(8) . . . . ?
O4 Ni1 N1 C15 47.1(3) 2 . . . ?
O1 Ni1 N1 C16 -28.8(3) . . . . ?
N3 Ni1 N1 C16 62.9(3) . . . . ?
OW1 Ni1 N1 C16 152.0(3) . . . . ?
OW2 Ni1 N1 C16 -84.6(8) . . . . ?
O4 Ni1 N1 C16 -121.5(3) 2 . . . ?
O1 Ni1 N3 C20 -166.1(3) . . . . ?
N1 Ni1 N3 C20 107.2(3) . . . . ?
OW1 Ni1 N3 C20 11.0(3) . . . . ?
OW2 Ni1 N3 C20 -76.6(3) . . . . ?
O4 Ni1 N3 C20 3.1(13) 2 . . . ?
O1 Ni1 N3 C21 19.7(3) . . . . ?
N1 Ni1 N3 C21 -67.0(3) . . . . ?
OW1 Ni1 N3 C21 -163.2(3) . . . . ?
OW2 Ni1 N3 C21 109.3(3) . . . . ?
O4 Ni1 N3 C21 -171.1(11) 2 . . . ?
C6 C1 C2 C3 -0.7(5) . . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
C1 C2 C3 C13 -178.5(3) . . . . ?
C2 C3 C4 C5 1.8(5) . . . . ?
C13 C3 C4 C5 179.9(3) . . . . ?
C3 C4 C5 C6 -2.1(5) . . . . ?
C2 C1 C6 C5 0.3(5) . . . . ?
C2 C1 C6 S1 -177.7(3) . . . . ?
C4 C5 C6 C1 1.1(5) . . . . ?
C4 C5 C6 S1 179.1(3) . . . . ?
O6 S1 C6 C1 -40.4(3) . . . . ?
O5 S1 C6 C1 -172.0(3) . . . . ?
C7 S1 C6 C1 74.3(3) . . . . ?
O6 S1 C6 C5 141.5(3) . . . . ?
O5 S1 C6 C5 9.9(3) . . . . ?
C7 S1 C6 C5 -103.8(3) . . . . ?
O6 S1 C7 C12 0.1(4) . . . . ?
O5 S1 C7 C12 130.9(3) . . . . ?
C6 S1 C7 C12 -114.9(3) . . . . ?
O6 S1 C7 C8 -178.7(3) . . . . ?
O5 S1 C7 C8 -48.0(3) . . . . ?
C6 S1 C7 C8 66.2(3) . . . . ?
C12 C7 C8 C9 2.9(5) . . . . ?
S1 C7 C8 C9 -178.3(3) . . . . ?
C7 C8 C9 C10 -3.9(5) . . . . ?
C8 C9 C10 C11 1.4(5) . . . . ?
C8 C9 C10 C14 179.9(3) . . . . ?
C9 C10 C11 C12 2.3(5) . . . . ?
C14 C10 C11 C12 -176.2(3) . . . . ?
C8 C7 C12 C11 0.7(6) . . . . ?
S1 C7 C12 C11 -178.1(3) . . . . ?
C10 C11 C12 C7 -3.3(6) . . . . ?
Ni1 O1 C13 O2 -5.2(5) . . . . ?
Ni1 O1 C13 C3 175.57(19) . . . . ?
C4 C3 C13 O2 174.3(3) . . . . ?
C2 C3 C13 O2 -7.5(5) . . . . ?
C4 C3 C13 O1 -6.5(4) . . . . ?
C2 C3 C13 O1 171.7(3) . . . . ?
Ni1 O4 C14 O3 13.4(5) 2 . . . ?
Ni1 O4 C14 C10 -165.2(2) 2 . . . ?
C9 C10 C14 O4 -37.0(4) . . . . ?
C11 C10 C14 O4 141.5(3) . . . . ?
C9 C10 C14 O3 144.2(3) . . . . ?
C11 C10 C14 O3 -37.2(5) . . . . ?
C16 N1 C15 N2 0.4(5) . . . . ?
Ni1 N1 C15 N2 -170.0(3) . . . . ?
C17 N2 C15 N1 0.2(5) . . . . ?
C18 N2 C15 N1 179.1(4) . . . . ?
C15 N1 C16 C17 -0.9(5) . . . . ?
Ni1 N1 C16 C17 169.9(3) . . . . ?
N1 C16 C17 N2 1.0(6) . . . . ?
C15 N2 C17 C16 -0.7(6) . . . . ?
C18 N2 C17 C16 -179.6(4) . . . . ?
C15 N2 C18 C19 114.8(5) . . . . ?
C17 N2 C18 C19 -66.4(7) . . . . ?
N2 C18 C19 C19 -64.6(8) . . . 2_355 ?
C21 N3 C20 N4 -0.2(4) . . . . ?
Ni1 N3 C20 N4 -175.5(2) . . . . ?
C22 N4 C20 N3 0.4(4) . . . . ?
C23 N4 C20 N3 176.3(3) . . . . ?
C20 N3 C21 C22 0.0(4) . . . . ?
Ni1 N3 C21 C22 175.1(2) . . . . ?
C20 N4 C22 C21 -0.4(4) . . . . ?
C23 N4 C22 C21 -176.3(3) . . . . ?
N3 C21 C22 N4 0.2(4) . . . . ?
C20 N4 C23 C24 -93.5(4) . . . . ?
C22 N4 C23 C24 81.7(5) . . . . ?
N4 C23 C24 C24 178.3(4) . . . 2_364 ?
