#------------------------------------------------------------------------------
#$Date: 2025-01-04 04:37:25 +0200 (Sat, 04 Jan 2025) $
#$Revision: 297060 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023343.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_2023343
loop_
_publ_author_name
'Tsymbal, Liudmyla V.'
'Andriichuk, Irina L.'
'Bahrin, Lucian G.'
'Lampeka, Yaroslaw D.'
_publ_section_title
;
 Syntheses and structures of two coordination polymers formed by
 Ni(cyclam)2+ cations and sulfate anions
;
_journal_coeditor_code           HB8118
_journal_issue                   2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024012337
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          '[Ni (S O4) (C10 H24 N4)]2, C46 H38 O8, 18H2 O'
_chemical_formula_moiety         'C20 H48 N8 Ni2 O8 S2, C46 H38 O8'
_chemical_formula_sum            'C66 H86 N8 Ni2 O16 S2'
_chemical_formula_weight         1428.96
_chemical_name_systematic
;catena-Poly[[[(1,4,8,11-tetraazacyclotetradecane-κ⁴N¹,N⁴,N⁸,N¹¹)nickel(II)]-μ₂-sulfato-κ²O³:O⁴]
hemi[4,4',4'',4'''-(2,2',4,4',6,6'-hexamethyl-[1,1'-biphenyl]-3,3',5,5'-tetrayl)tetrabenzoic acid] nonahydrate]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.777(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1299(5)
_cell_length_b                   18.5163(11)
_cell_length_c                   35.621(2)
_cell_measurement_reflns_used    2340
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.1120
_cell_measurement_theta_min      2.0080
_cell_volume                     7972.7(7)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.1724
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20054
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.043
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       plate
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1881
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0206P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                3223
_reflns_number_total             8085
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb8118.cif
_cod_data_source_block           II
_cod_original_cell_volume        7972.7(8)
_cod_database_code               2023343
_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   0.944
_shelx_estimated_absorpt_t_max   0.994
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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 0.250000 0.750000 0.750000 0.0562(3) Uani d 1 . .
Ni Ni2 0.750000 0.750000 0.750000 0.0628(3) Uani d 1 . .
S S1 0.50054(10) 0.67856(9) 0.75649(4) 0.0648(5) Uani d 1 . .
O O3 0.5194(2) 0.6766(2) 0.79768(10) 0.0784(12) Uani d 1 . .
O O2 0.60695(19) 0.68618(17) 0.73957(8) 0.0637(10) Uani d 1 . .
N N3 0.8460(3) 0.6578(3) 0.74746(15) 0.0723(14) Uani d 1 . .
H H3 0.923074 0.673461 0.747240 0.087 Uiso calc 1 . .
O O1 0.4286(2) 0.74068(18) 0.74571(9) 0.0633(10) Uani d 1 . .
O O4 0.4467(2) 0.6099(2) 0.74284(10) 0.0839(13) Uani d 1 . .
N N1 0.2244(3) 0.6743(3) 0.70776(12) 0.0646(13) Uani d 1 . .
H H1 0.296188 0.651709 0.704761 0.078 Uiso calc 1 . .
N N2 0.2493(3) 0.6758(3) 0.79323(12) 0.0724(15) Uani d 1 . .
H H2 0.322725 0.653431 0.796249 0.087 Uiso calc 1 . .
N N4 0.7455(3) 0.7698(3) 0.69294(12) 0.0752(15) Uani d 1 . .
H H4 0.815571 0.792987 0.688167 0.090 Uiso calc 1 . .
C C30 0.6311(4) 0.1028(2) 0.43972(16) 0.0549(15) Uani d 1 . .
O O6 0.3958(3) 0.6092(2) 0.64754(11) 0.1048(15) Uani d 1 . .
C C11 0.4785(4) 0.5740(3) 0.6510(2) 0.0739(19) Uani d 1 . .
O O8 0.3879(3) -0.0478(2) 0.34768(11) 0.0993(15) Uani d 1 . .
C C18 0.6922(3) 0.4520(2) 0.52586(16) 0.0565(15) Uani d 1 . .
C C15 0.6387(4) 0.4891(3) 0.55700(18) 0.0578(16) Uani d 1 . .
O O5 0.5273(3) 0.5560(3) 0.68365(12) 0.1085(17) Uani d 1 . .
H H5 0.494848 0.574604 0.700454 0.163 Uiso calc 1 . .
C C35 0.6920(4) 0.0749(3) 0.41216(17) 0.0641(17) Uani d 1 . .
H H35 0.767412 0.084687 0.413391 0.077 Uiso calc 1 . .
O O7 0.5501(4) -0.0438(2) 0.32448(15) 0.141(2) Uani d 1 . .
H H7 0.544646 -0.087006 0.319664 0.212 Uiso calc 1 . .
C C24 0.750000 0.2565(4) 0.500000 0.061(2) Uani d 1 . .
C C10 0.8358(4) 0.6201(4) 0.7837(2) 0.099(2) Uani d 1 . .
H H10A 0.894279 0.584556 0.787911 0.118 Uiso calc 1 . .
H H10B 0.765234 0.595217 0.783070 0.118 Uiso calc 1 . .
C C12 0.5369(4) 0.5458(3) 0.61875(18) 0.0632(17) Uani d 1 . .
C C33 0.5339(4) 0.0202(2) 0.37979(15) 0.0549(15) Uani d 1 . .
C C32 0.4706(4) 0.0485(3) 0.40693(17) 0.0667(17) Uani d 1 . .
H H32 0.394832 0.040027 0.405222 0.080 Uiso calc 1 . .
C C29 0.750000 0.0240(3) 0.500000 0.081(3) Uani d 1 . .
H H29A 0.682200 0.006673 0.508860 0.122 Uiso d 0.5 A -1
H H29B 0.811420 0.006673 0.516270 0.122 Uiso d 0.5 A -1
H H29C 0.756370 0.006673 0.474860 0.122 Uiso d 0.5 A -1
C C25 0.6867(4) 0.2198(3) 0.47185(17) 0.0632(16) Uani d 1 . .
C C31 0.5178(4) 0.0887(3) 0.43612(17) 0.0724(18) Uani d 1 . .
H H31 0.473456 0.107060 0.453963 0.087 Uiso calc 1 . .
C C21 0.6887(4) 0.3754(2) 0.52488(16) 0.0598(16) Uani d 1 . .
C C2 0.1792(4) 0.5761(3) 0.7521(2) 0.102(3) Uani d 1 . .
H H2A 0.134603 0.532745 0.752629 0.123 Uiso calc 1 . .
H H2B 0.255789 0.561034 0.751981 0.123 Uiso calc 1 . .
C C14 0.5408(4) 0.5268(3) 0.55178(17) 0.0761(18) Uani d 1 . .
H H14 0.507398 0.533655 0.527591 0.091 Uiso calc 1 . .
C C19 0.750000 0.4897(4) 0.500000 0.059(2) Uani d 1 . .
C C7 0.8269(4) 0.6526(4) 0.67781(18) 0.100(2) Uani d 1 . .
H H7A 0.827753 0.618110 0.657331 0.120 Uiso calc 1 . .
H H7B 0.896294 0.678843 0.679027 0.120 Uiso calc 1 . .
C C1 0.1470(4) 0.6156(3) 0.71504(19) 0.091(2) Uani d 1 . .
H H1A 0.145034 0.581271 0.694445 0.109 Uiso calc 1 . .
H H1B 0.073304 0.635565 0.715824 0.109 Uiso calc 1 . .
C C34 0.6463(4) 0.0332(3) 0.38290(16) 0.0628(16) Uani d 1 . .
H H34 0.690847 0.014029 0.365352 0.075 Uiso calc 1 . .
C C26 0.6144(4) 0.2602(3) 0.44165(17) 0.093(2) Uani d 1 . .
H H26A 0.628524 0.311130 0.443719 0.140 Uiso d 1 . .
H H26B 0.537924 0.251010 0.444999 0.140 Uiso d 1 . .
H H26C 0.630924 0.243690 0.417199 0.140 Uiso d 1 . .
C C28 0.750000 0.1063(3) 0.500000 0.053(2) Uani d 1 . .
C C36 0.4816(5) -0.0268(3) 0.34931(17) 0.0710(18) Uani d 1 . .
C C6 0.8214(4) 0.6113(3) 0.7142(2) 0.093(2) Uani d 1 . .
H H6A 0.748034 0.590791 0.714947 0.112 Uiso calc 1 . .
H H6B 0.874045 0.571789 0.714897 0.112 Uiso calc 1 . .
C C27 0.6889(4) 0.1440(3) 0.47161(16) 0.0581(15) Uani d 1 . .
C C23 0.750000 0.3381(3) 0.500000 0.059(2) Uani d 1 . .
C C4 0.2352(4) 0.7191(4) 0.82776(17) 0.092(2) Uani d 1 . .
H H4A 0.257107 0.690753 0.850039 0.111 Uiso calc 1 . .
H H4B 0.158213 0.732707 0.828578 0.111 Uiso calc 1 . .
C C13 0.4922(4) 0.5543(3) 0.5823(2) 0.077(2) Uani d 1 . .
H H13 0.426278 0.579840 0.578109 0.092 Uiso calc 1 . .
C C17 0.6369(4) 0.5105(3) 0.62374(17) 0.087(2) Uani d 1 . .
H H17 0.671219 0.504953 0.647893 0.105 Uiso calc 1 . .
C C16 0.6867(4) 0.4833(3) 0.5933(2) 0.099(2) Uani d 1 . .
H H16 0.754840 0.460414 0.597436 0.118 Uiso calc 1 . .
C C5 0.1940(4) 0.7144(4) 0.67308(16) 0.089(2) Uani d 1 . .
H H5A 0.116564 0.728053 0.672049 0.106 Uiso calc 1 . .
H H5B 0.204755 0.684329 0.651400 0.106 Uiso calc 1 . .
C C3 0.1672(4) 0.6173(4) 0.7876(2) 0.099(2) Uani d 1 . .
H H3A 0.093417 0.637773 0.786818 0.119 Uiso calc 1 . .
H H3B 0.175758 0.584418 0.808869 0.119 Uiso calc 1 . .
C C9 0.6560(4) 0.8245(4) 0.68479(18) 0.100(2) Uani d 1 . .
H H9A 0.584152 0.801136 0.683389 0.120 Uiso calc 1 . .
H H9B 0.664611 0.847849 0.660847 0.120 Uiso calc 1 . .
C C22 0.6150(4) 0.3346(3) 0.55038(16) 0.096(2) Uani d 1 . .
H H22A 0.652519 0.330370 0.575101 0.144 Uiso d 1 . .
H H22B 0.598969 0.287350 0.540311 0.144 Uiso d 1 . .
H H22C 0.547179 0.360810 0.551891 0.144 Uiso d 1 . .
C C8 0.7330(4) 0.7059(4) 0.66839(17) 0.099(2) Uani d 1 . .
H H8A 0.733069 0.720682 0.642270 0.119 Uiso calc 1 . .
H H8B 0.662777 0.682610 0.671625 0.119 Uiso calc 1 . .
C C20 0.750000 0.5710(3) 0.500000 0.086(3) Uani d 1 . .
H H20A 0.675440 0.588307 0.500220 0.129 Uiso d 0.5 B -1
H H20B 0.781320 0.588307 0.477810 0.129 Uiso d 0.5 B -1
H H20C 0.793240 0.588307 0.521970 0.129 Uiso d 0.5 B -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ni1 O1 . 7_566 180.0 ?
N1 Ni1 O1 7_566 . 90.85(13) ?
N1 Ni1 O1 . 7_566 90.85(13) ?
N1 Ni1 O1 . . 89.15(13) ?
N1 Ni1 O1 7_566 7_566 89.15(13) ?
N1 Ni1 N1 . 7_566 180.0 ?
N1 Ni1 N2 7_566 7_566 94.72(19) ?
N1 Ni1 N2 7_566 . 85.28(19) ?
N1 Ni1 N2 . 7_566 85.28(19) ?
N1 Ni1 N2 . . 94.72(19) ?
N2 Ni1 O1 . 7_566 86.26(12) ?
N2 Ni1 O1 . . 93.74(12) ?
N2 Ni1 O1 7_566 7_566 93.74(12) ?
N2 Ni1 O1 7_566 . 86.26(12) ?
N2 Ni1 N2 . 7_566 180.0 ?
O2 Ni2 O2 7_666 . 180.0 ?
N3 Ni2 O2 7_666 7_666 89.28(14) ?
N3 Ni2 O2 . . 89.28(14) ?
N3 Ni2 O2 7_666 . 90.72(14) ?
N3 Ni2 O2 . 7_666 90.72(14) ?
N3 Ni2 N3 7_666 . 180.0 ?
N4 Ni2 O2 . 7_666 91.61(15) ?
N4 Ni2 O2 7_666 . 91.61(15) ?
N4 Ni2 O2 7_666 7_666 88.39(15) ?
N4 Ni2 O2 . . 88.39(15) ?
N4 Ni2 N3 . 7_666 85.84(19) ?
N4 Ni2 N3 7_666 7_666 94.16(19) ?
N4 Ni2 N3 7_666 . 85.84(19) ?
N4 Ni2 N3 . . 94.16(19) ?
N4 Ni2 N4 7_666 . 180.00(4) ?
O3 S1 O2 . . 110.02(18) ?
O3 S1 O1 . . 108.6(2) ?
O3 S1 O4 . . 109.5(2) ?
O2 S1 O4 . . 108.8(2) ?
O1 S1 O2 . . 109.74(19) ?
O1 S1 O4 . . 110.2(2) ?
S1 O2 Ni2 . . 135.8(2) ?
Ni2 N3 H3 . . 107.2 ?
C10 N3 Ni2 . . 105.2(3) ?
C10 N3 H3 . . 107.2 ?
C6 N3 Ni2 . . 116.0(3) ?
C6 N3 H3 . . 107.2 ?
C6 N3 C10 . . 113.6(5) ?
S1 O1 Ni1 . . 127.61(19) ?
Ni1 N1 H1 . . 106.8 ?
C1 N1 Ni1 . . 115.6(3) ?
C1 N1 H1 . . 106.8 ?
C5 N1 Ni1 . . 106.5(4) ?
C5 N1 H1 . . 106.8 ?
C5 N1 C1 . . 113.8(5) ?
Ni1 N2 H2 . . 107.6 ?
C4 N2 Ni1 . . 105.4(4) ?
C4 N2 H2 . . 107.6 ?
C3 N2 Ni1 . . 115.7(3) ?
C3 N2 H2 . . 107.6 ?
C3 N2 C4 . . 112.6(4) ?
Ni2 N4 H4 . . 107.3 ?
C9 N4 Ni2 . . 105.7(3) ?
C9 N4 H4 . . 107.3 ?
C8 N4 Ni2 . . 115.8(4) ?
C8 N4 H4 . . 107.3 ?
C8 N4 C9 . . 113.1(5) ?
C35 C30 C31 . . 116.6(5) ?
C35 C30 C27 . . 119.2(5) ?
C31 C30 C27 . . 124.2(5) ?
O6 C11 O5 . . 123.1(6) ?
O6 C11 C12 . . 124.2(6) ?
O5 C11 C12 . . 112.8(5) ?
C21 C18 C15 . . 117.5(5) ?
C19 C18 C15 . . 122.3(4) ?
C19 C18 C21 . . 120.1(5) ?
C14 C15 C18 . . 123.7(6) ?
C16 C15 C18 . . 119.0(5) ?
C16 C15 C14 . . 117.3(5) ?
C11 O5 H5 . . 109.5 ?
C30 C35 H35 . . 118.5 ?
C30 C35 C34 . . 123.0(5) ?
C34 C35 H35 . . 118.5 ?
C36 O7 H7 . . 109.5 ?
C25 C24 C25 . 2_656 121.4(7) ?
C25 C24 C23 2_656 . 119.3(4) ?
C25 C24 C23 . . 119.3(4) ?
N3 C10 H10A . . 110.0 ?
N3 C10 H10B . . 110.0 ?
N3 C10 C9 . 7_666 108.7(5) ?
H10A C10 H10B . . 108.3 ?
C9 C10 H10A 7_666 . 110.0 ?
C9 C10 H10B 7_666 . 110.0 ?
C13 C12 C11 . . 120.7(5) ?
C13 C12 C17 . . 116.8(5) ?
C17 C12 C11 . . 122.5(6) ?
C32 C33 C36 . . 120.2(5) ?
C34 C33 C32 . . 118.5(5) ?
C34 C33 C36 . . 121.2(5) ?
C33 C32 H32 . . 119.4 ?
C31 C32 C33 . . 121.1(5) ?
C31 C32 H32 . . 119.4 ?
H29A C29 H29B . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?
C28 C29 H29A . . 109.5 ?
C28 C29 H29B . . 109.5 ?
C28 C29 H29C . . 109.5 ?
C24 C25 C26 . . 121.3(5) ?
C24 C25 C27 . . 118.9(6) ?
C27 C25 C26 . . 119.7(5) ?
C30 C31 H31 . . 119.4 ?
C32 C31 C30 . . 121.3(5) ?
C32 C31 H31 . . 119.4 ?
C18 C21 C22 . . 119.8(4) ?
C23 C21 C18 . . 119.8(5) ?
C23 C21 C22 . . 120.3(4) ?
H2A C2 H2B . . 107.3 ?
C1 C2 H2A . . 108.1 ?
C1 C2 H2B . . 108.1 ?
C3 C2 H2A . . 108.1 ?
C3 C2 H2B . . 108.1 ?
C3 C2 C1 . . 116.8(6) ?
C15 C14 H14 . . 119.9 ?
C15 C14 C13 . . 120.1(6) ?
C13 C14 H14 . . 119.9 ?
C18 C19 C18 . 2_656 119.8(6) ?
C18 C19 C20 2_656 . 120.1(3) ?
C18 C19 C20 . . 120.1(3) ?
H7A C7 H7B . . 107.5 ?
C6 C7 H7A . . 108.4 ?
C6 C7 H7B . . 108.4 ?
C6 C7 C8 . . 115.6(5) ?
C8 C7 H7A . . 108.4 ?
C8 C7 H7B . . 108.4 ?
N1 C1 C2 . . 112.6(5) ?
N1 C1 H1A . . 109.1 ?
N1 C1 H1B . . 109.1 ?
C2 C1 H1A . . 109.1 ?
C2 C1 H1B . . 109.1 ?
H1A C1 H1B . . 107.8 ?
C35 C34 C33 . . 119.5(5) ?
C35 C34 H34 . . 120.3 ?
C33 C34 H34 . . 120.3 ?
C25 C26 H26A . . 109.8 ?
C25 C26 H26B . . 109.3 ?
C25 C26 H26C . . 109.4 ?
H26A C26 H26B . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
C27 C28 C29 2_656 . 120.2(3) ?
C27 C28 C29 . . 120.2(3) ?
C27 C28 C27 2_656 . 119.7(7) ?
O8 C36 O7 . . 123.0(6) ?
O8 C36 C33 . . 124.7(5) ?
O7 C36 C33 . . 112.3(5) ?
N3 C6 C7 . . 111.9(6) ?
N3 C6 H6A . . 109.2 ?
N3 C6 H6B . . 109.2 ?
C7 C6 H6A . . 109.2 ?
C7 C6 H6B . . 109.2 ?
H6A C6 H6B . . 107.9 ?
C25 C27 C30 . . 120.5(5) ?
C28 C27 C30 . . 118.9(5) ?
C28 C27 C25 . . 120.5(6) ?
C21 C23 C24 . . 119.9(3) ?
C21 C23 C24 2_656 . 119.9(3) ?
C21 C23 C21 . 2_656 120.2(6) ?
N2 C4 H4A . . 110.0 ?
N2 C4 H4B . . 110.0 ?
N2 C4 C5 . 7_566 108.6(4) ?
H4A C4 H4B . . 108.3 ?
C5 C4 H4A 7_566 . 110.0 ?
C5 C4 H4B 7_566 . 110.0 ?
C12 C13 C14 . . 122.8(5) ?
C12 C13 H13 . . 118.6 ?
C14 C13 H13 . . 118.6 ?
C12 C17 H17 . . 119.6 ?
C12 C17 C16 . . 120.7(6) ?
C16 C17 H17 . . 119.6 ?
C15 C16 C17 . . 122.1(5) ?
C15 C16 H16 . . 119.0 ?
C17 C16 H16 . . 119.0 ?
N1 C5 C4 . 7_566 109.2(5) ?
N1 C5 H5A . . 109.8 ?
N1 C5 H5B . . 109.8 ?
C4 C5 H5A 7_566 . 109.8 ?
C4 C5 H5B 7_566 . 109.8 ?
H5A C5 H5B . . 108.3 ?
N2 C3 C2 . . 112.1(5) ?
N2 C3 H3A . . 109.2 ?
N2 C3 H3B . . 109.2 ?
C2 C3 H3A . . 109.2 ?
C2 C3 H3B . . 109.2 ?
H3A C3 H3B . . 107.9 ?
N4 C9 C10 . 7_666 108.2(5) ?
N4 C9 H9A . . 110.1 ?
N4 C9 H9B . . 110.1 ?
C10 C9 H9A 7_666 . 110.1 ?
C10 C9 H9B 7_666 . 110.1 ?
H9A C9 H9B . . 108.4 ?
C21 C22 H22A . . 109.3 ?
C21 C22 H22B . . 109.8 ?
C21 C22 H22C . . 109.3 ?
H22A C22 H22B . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
N4 C8 C7 . . 110.6(5) ?
N4 C8 H8A . . 109.5 ?
N4 C8 H8B . . 109.5 ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 108.1 ?
C19 C20 H20A . . 109.5 ?
C19 C20 H20B . . 109.5 ?
C19 C20 H20C . . 109.5 ?
H20A C20 H20B . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 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 O1 . 2.191(2) ?
Ni1 O1 7_566 2.191(2) ?
Ni1 N1 . 2.061(4) ?
Ni1 N1 7_566 2.061(4) ?
Ni1 N2 . 2.065(4) ?
Ni1 N2 7_566 2.065(4) ?
Ni2 O2 . 2.107(3) ?
Ni2 O2 7_666 2.107(3) ?
Ni2 N3 7_666 2.073(4) ?
Ni2 N3 . 2.073(4) ?
Ni2 N4 . 2.062(4) ?
Ni2 N4 7_666 2.062(4) ?
S1 O3 . 1.466(3) ?
S1 O2 . 1.476(3) ?
S1 O1 . 1.476(3) ?
S1 O4 . 1.491(4) ?
N3 H3 . 0.9800 ?
N3 C10 . 1.481(6) ?
N3 C6 . 1.476(6) ?
N1 H1 . 0.9800 ?
N1 C1 . 1.473(6) ?
N1 C5 . 1.462(6) ?
N2 H2 . 0.9800 ?
N2 C4 . 1.490(6) ?
N2 C3 . 1.473(6) ?
N4 H4 . 0.9800 ?
N4 C9 . 1.495(6) ?
N4 C8 . 1.472(6) ?
C30 C35 . 1.377(6) ?
C30 C31 . 1.395(6) ?
C30 C27 . 1.494(7) ?
O6 C11 . 1.194(5) ?
C11 O5 . 1.305(6) ?
C11 C12 . 1.492(7) ?
O8 C36 . 1.198(5) ?
C18 C15 . 1.498(6) ?
C18 C21 . 1.419(6) ?
C18 C19 . 1.391(5) ?
C15 C14 . 1.377(6) ?
C15 C16 . 1.377(7) ?
O5 H5 . 0.8200 ?
C35 H35 . 0.9300 ?
C35 C34 . 1.376(6) ?
O7 H7 . 0.8200 ?
O7 C36 . 1.302(5) ?
C24 C25 2_656 1.389(6) ?
C24 C25 . 1.389(6) ?
C24 C23 . 1.510(9) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C10 C9 7_666 1.519(7) ?
C12 C13 . 1.372(7) ?
C12 C17 . 1.376(6) ?
C33 C32 . 1.386(6) ?
C33 C34 . 1.381(5) ?
C33 C36 . 1.491(6) ?
C32 H32 . 0.9300 ?
C32 C31 . 1.365(6) ?
C29 H29A . 0.9600 ?
C29 H29B . 0.9600 ?
C29 H29C . 0.9602 ?
C29 C28 . 1.524(8) ?
C25 C26 . 1.526(6) ?
C25 C27 . 1.403(6) ?
C31 H31 . 0.9300 ?
C21 C23 . 1.388(5) ?
C21 C22 . 1.526(6) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C2 C1 . 1.530(7) ?
C2 C3 . 1.496(7) ?
C14 H14 . 0.9300 ?
C14 C13 . 1.378(7) ?
C19 C20 . 1.506(8) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C7 C6 . 1.510(7) ?
C7 C8 . 1.523(7) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C34 H34 . 0.9300 ?
C26 H26A . 0.9599 ?
C26 H26B . 0.9601 ?
C26 H26C . 0.9600 ?
C28 C27 2_656 1.391(5) ?
C28 C27 . 1.391(5) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C4 C5 7_566 1.503(7) ?
C13 H13 . 0.9300 ?
C17 H17 . 0.9300 ?
C17 C16 . 1.380(7) ?
C16 H16 . 0.9300 ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C22 H22A . 0.9602 ?
C22 H22B . 0.9600 ?
C22 H22C . 0.9601 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C20 H20A . 0.9600 ?
C20 H20B . 0.9599 ?
C20 H20C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 O4 . 0.98 2.32 3.113(5) 138.0 yes
N2 H2 O3 . 0.98 2.42 3.267(4) 144.1 yes
N4 H4 O3 7_666 0.98 2.10 3.012(5) 154.1 yes
O5 H5 O4 . 0.82 1.79 2.597(5) 169.0 yes
O7 H7 O3 8_554 0.82 1.85 2.654(5) 166.4 yes
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 N1 C1 C2 . . . . -54.6(6) ?
Ni1 N1 C5 C4 . . . 7_566 40.7(4) ?
Ni1 N2 C4 C5 . . . 7_566 -41.7(5) ?
Ni1 N2 C3 C2 . . . . 56.4(6) ?
Ni2 N3 C10 C9 . . . 7_666 -42.8(5) ?
Ni2 N3 C6 C7 . . . . 55.0(5) ?
Ni2 N4 C9 C10 . . . 7_666 41.2(5) ?
Ni2 N4 C8 C7 . . . . -58.2(5) ?
O3 S1 O2 Ni2 . . . . -44.7(3) ?
O3 S1 O1 Ni1 . . . . -75.3(3) ?
O2 S1 O1 Ni1 . . . . 164.4(2) ?
O1 S1 O2 Ni2 . . . . 74.7(3) ?
O4 S1 O2 Ni2 . . . . -164.6(2) ?
O4 S1 O1 Ni1 . . . . 44.6(3) ?
C30 C35 C34 C33 . . . . 2.3(8) ?
O6 C11 C12 C13 . . . . -5.3(9) ?
O6 C11 C12 C17 . . . . 174.5(6) ?
C11 C12 C13 C14 . . . . -177.4(5) ?
C11 C12 C17 C16 . . . . 178.1(6) ?
C18 C15 C14 C13 . . . . 174.6(5) ?
C18 C15 C16 C17 . . . . -174.1(5) ?
C18 C21 C23 C24 . . . . 177.6(3) ?
C18 C21 C23 C21 . . . 2_656 -2.4(3) ?
C15 C18 C21 C23 . . . . -171.0(4) ?
C15 C18 C21 C22 . . . . 10.8(7) ?
C15 C18 C19 C18 . . . 2_656 173.3(5) ?
C15 C18 C19 C20 . . . . -6.7(5) ?
C15 C14 C13 C12 . . . . -0.3(9) ?
O5 C11 C12 C13 . . . . 174.5(6) ?
O5 C11 C12 C17 . . . . -5.7(8) ?
C35 C30 C31 C32 . . . . 0.8(8) ?
C35 C30 C27 C25 . . . . 101.0(6) ?
C35 C30 C27 C28 . . . . -75.5(6) ?
C24 C25 C27 C30 . . . . -173.8(4) ?
C24 C25 C27 C28 . . . . 2.6(7) ?
C10 N3 C6 C7 . . . . 177.0(4) ?
C12 C17 C16 C15 . . . . -1.0(10) ?
C33 C32 C31 C30 . . . . 0.1(9) ?
C32 C33 C34 C35 . . . . -1.3(7) ?
C32 C33 C36 O8 . . . . -6.3(9) ?
C32 C33 C36 O7 . . . . 174.6(5) ?
C29 C28 C27 C30 . . . . -4.9(5) ?
C29 C28 C27 C25 . . . . 178.7(3) ?
C25 C24 C25 C26 2_656 . . . 178.0(5) ?
C25 C24 C25 C27 2_656 . . . -1.3(3) ?
C25 C24 C23 C21 2_656 . . 2_656 102.8(3) ?
C25 C24 C23 C21 . . . . 102.8(3) ?
C25 C24 C23 C21 . . . 2_656 -77.2(3) ?
C25 C24 C23 C21 2_656 . . . -77.2(3) ?
C31 C30 C35 C34 . . . . -2.0(8) ?
C31 C30 C27 C25 . . . . -80.6(7) ?
C31 C30 C27 C28 . . . . 103.0(5) ?
C21 C18 C15 C14 . . . . -107.6(6) ?
C21 C18 C15 C16 . . . . 69.7(7) ?
C21 C18 C19 C18 . . . 2_656 -2.5(3) ?
C21 C18 C19 C20 . . . . 177.5(3) ?
C14 C15 C16 C17 . . . . 3.4(9) ?
C19 C18 C15 C14 . . . . 76.6(6) ?
C19 C18 C15 C16 . . . . -106.1(6) ?
C19 C18 C21 C23 . . . . 5.0(7) ?
C19 C18 C21 C22 . . . . -173.3(4) ?
C1 N1 C5 C4 . . . 7_566 169.2(4) ?
C1 C2 C3 N2 . . . . -70.0(6) ?
C34 C33 C32 C31 . . . . 0.2(8) ?
C34 C33 C36 O8 . . . . 170.1(5) ?
C34 C33 C36 O7 . . . . -9.0(8) ?
C26 C25 C27 C30 . . . . 6.9(8) ?
C26 C25 C27 C28 . . . . -176.8(4) ?
C36 C33 C32 C31 . . . . 176.7(5) ?
C36 C33 C34 C35 . . . . -177.8(5) ?
C6 N3 C10 C9 . . . 7_666 -170.7(4) ?
C6 C7 C8 N4 . . . . 73.2(7) ?
C27 C30 C35 C34 . . . . 176.6(5) ?
C27 C30 C31 C32 . . . . -177.7(5) ?
C27 C28 C27 C30 2_656 . . . 175.1(5) ?
C27 C28 C27 C25 2_656 . . . -1.3(3) ?
C23 C24 C25 C26 . . . . -2.0(5) ?
C23 C24 C25 C27 . . . . 178.7(3) ?
C4 N2 C3 C2 . . . . 177.7(5) ?
C13 C12 C17 C16 . . . . -2.1(9) ?
C17 C12 C13 C14 . . . . 2.8(9) ?
C16 C15 C14 C13 . . . . -2.8(8) ?
C5 N1 C1 C2 . . . . -178.3(5) ?
C3 N2 C4 C5 . . . 7_566 -168.6(4) ?
C3 C2 C1 N1 . . . . 69.3(6) ?
C9 N4 C8 C7 . . . . 179.5(4) ?
C22 C21 C23 C24 . . . . -4.2(5) ?
C22 C21 C23 C21 . . . 2_656 175.7(5) ?
C8 N4 C9 C10 . . . 7_666 169.0(5) ?
C8 C7 C6 N3 . . . . -71.6(7) ?
