#------------------------------------------------------------------------------
#$Date: 2025-07-05 13:10:14 +0300 (Sat, 05 Jul 2025) $
#$Revision: 300370 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573865.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_1573865
loop_
_publ_author_name
'Pfeiffer, Maximilian'
'Stöger, Berthold'
'Weil, Matthias'
_publ_section_title
;
 Poly[[bis(\m4-acetato-\k4
 O:O:O&#x2032;:O&#x2032;)tetrakis(\m3-acetato-\k3
 O:O:O&#x2032;)bis(\m2-acetato-\k2
 O:O′)bis(μ3-hydroxido)pentanickel(II)] 2.60-hydrate]
;
_journal_coeditor_code           BT4163
_journal_issue                   2
_journal_name_full               IUCrData
_journal_page_first              x250082
_journal_paper_doi               10.1107/S2414314625000823
_journal_volume                  10
_journal_year                    2025
_chemical_formula_iupac          '[Ni5 (C2 H3 O2)8 (O H)2], 2.60H2O'
_chemical_formula_moiety         'C16 H26 Ni5 O18, 2.60(H2O)'
_chemical_formula_sum            'C16 H31.2 Ni5 O20.6'
_chemical_formula_weight         846.80
_chemical_name_systematic
'Poly[[bis(μ₄-acetato-κ⁴O:O:O':O')tetrakis(μ₃-acetato-κ³O:O:O')bis(μ₂-acetato-κ²O:O')bis(μ₃-hydroxido)pentanickel(II)] 2.60-hydrate]'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.3025(11)
_cell_length_b                   23.3025(11)
_cell_length_c                   11.2648(5)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.92
_cell_measurement_theta_min      1.75
_cell_volume                     6116.9(5)
_computing_cell_refinement
;
X-Area (Stoe & Cie, 2024)
;
_computing_data_collection
;
X-Area (Stoe & Cie, 2024)
;
_computing_data_reduction
;
X-Area (Stoe & Cie, 2024)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL  (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT  (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'Eiger2 1M CdTe'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.1234
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20999
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.511
_diffrn_reflns_theta_min         2.008
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    3.103
_exptl_absorpt_correction_T_max  0.7097
_exptl_absorpt_correction_T_min  0.5809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(LANA; Koziskova et al., 2016)
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_size_rad          0.040
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.911
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         5145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0376
_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)+(0.0260P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                2744
_reflns_number_total             5145
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            bt4163.cif
_cod_data_source_block           I
_cod_original_cell_volume        6116.9(6)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C16 H31.20 Ni5 O20.60'
_cod_database_code               1573865
#BEGIN Tags that were not found in dictionaries:
_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   0.576
_shelx_estimated_absorpt_t_max   0.860
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 1.000000 0.500000 0.500000 0.01941(13) Uani d 1 . .
Ni Ni2 0.87305(2) 0.53890(2) 0.49712(3) 0.01354(8) Uani d 1 . .
Ni Ni3 0.77923(2) 0.44682(2) 0.52555(3) 0.01217(8) Uani d 1 . .
O O1 0.90748(9) 0.59881(9) 0.60134(16) 0.0211(5) Uani d 1 . .
O O2 1.00011(9) 0.57249(10) 0.59387(17) 0.0284(5) Uani d 1 . .
O O3 0.94065(8) 0.53418(9) 0.37833(14) 0.0183(5) Uani d 1 . .
O O4 0.88695(8) 0.53130(9) 0.21325(15) 0.0214(5) Uani d 1 . .
O O5 0.92122(8) 0.47408(9) 0.57859(15) 0.0191(5) Uani d 1 . .
O O6 0.84795(8) 0.42100(8) 0.63759(14) 0.0134(4) Uani d 1 . .
O O7 0.70649(8) 0.46180(8) 0.42844(15) 0.0178(4) Uani d 1 . .
O O8 0.72147(8) 0.54712(8) 0.34548(14) 0.0136(4) Uani d 1 . .
O O9 0.83183(8) 0.47852(8) 0.40476(14) 0.0122(4) Uani d 1 . .
H H9 0.858792 0.448659 0.373873 0.018 Uiso calc 1 . .
O OW1 0.8698(2) 0.37614(17) 0.2711(4) 0.0573(14) Uani d 0.699(5) A 1
O OW2 0.8781(4) 0.3908(4) 0.0907(8) 0.070(4) Uani d 0.301(5) . .
O OW3 0.8977(4) 0.3816(4) 0.3396(8) 0.041(3) Uani d 0.301(5) A 2
C C1 0.97488(17) 0.65457(18) 0.7052(4) 0.0710(15) Uani d 1 . .
H H1A 0.965806 0.690456 0.663914 0.106 Uiso calc 1 . .
H H1B 1.015970 0.653458 0.723552 0.106 Uiso calc 1 . .
H H1C 0.952762 0.652406 0.779061 0.106 Uiso calc 1 . .
C C2 0.95967(16) 0.60452(16) 0.6271(3) 0.0316(8) Uani d 1 . .
C C3 0.98514(14) 0.51384(18) 0.1903(3) 0.0435(11) Uani d 1 . .
H H3A 0.994597 0.547377 0.141613 0.065 Uiso calc 1 . .
H H3B 0.976865 0.481045 0.138644 0.065 Uiso calc 1 . .
H H3C 1.017715 0.504596 0.241930 0.065 Uiso calc 1 . .
C C4 0.93369(12) 0.52682(13) 0.2648(2) 0.0205(6) Uani d 1 . .
C C5 0.94067(13) 0.37866(14) 0.6475(3) 0.0338(9) Uani d 1 . .
H H5A 0.938084 0.369374 0.732144 0.051 Uiso calc 1 . .
H H5B 0.980102 0.389891 0.628096 0.051 Uiso calc 1 . .
H H5C 0.929924 0.344947 0.600447 0.051 Uiso calc 1 . .
C C6 0.90074(13) 0.42727(13) 0.6195(2) 0.0183(7) Uani d 1 . .
C C7 0.62615(14) 0.52147(16) 0.4064(3) 0.0487(11) Uani d 1 . .
H H7A 0.618561 0.561801 0.387364 0.073 Uiso calc 1 . .
H H7B 0.614544 0.513707 0.488435 0.073 Uiso calc 1 . .
H H7C 0.604258 0.496792 0.352400 0.073 Uiso calc 1 . .
C C8 0.68878(12) 0.50943(13) 0.3925(2) 0.0167(6) Uani d 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'
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'
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
O2 Ni1 O2 9_766 . 180.0 ?
O2 Ni1 O3 . . 91.47(8) ?
O2 Ni1 O3 . 9_766 88.53(8) ?
O2 Ni1 O3 9_766 . 88.53(8) ?
O2 Ni1 O3 9_766 9_766 91.47(8) ?
O2 Ni1 O5 . . 91.20(8) ?
O2 Ni1 O5 . 9_766 88.80(8) ?
O2 Ni1 O5 9_766 9_766 91.20(8) ?
O2 Ni1 O5 9_766 . 88.80(8) ?
O3 Ni1 O3 . 9_766 180.0 ?
O3 Ni1 O5 9_766 . 100.88(7) ?
O3 Ni1 O5 . . 79.12(7) ?
O3 Ni1 O5 9_766 9_766 79.12(7) ?
O3 Ni1 O5 . 9_766 100.89(7) ?
O5 Ni1 O5 . 9_766 180.0 ?
O1 Ni2 O3 . . 96.42(8) ?
O1 Ni2 O5 . . 91.80(8) ?
O1 Ni2 O6 . 7_544 94.78(7) ?
O1 Ni2 O8 . 8_454 96.25(8) ?
O1 Ni2 O9 . . 174.04(8) ?
O3 Ni2 O5 . . 80.62(7) ?
O3 Ni2 O6 . 7_544 91.54(7) ?
O3 Ni2 O8 . 8_454 167.29(7) ?
O5 Ni2 O6 . 7_544 170.29(7) ?
O5 Ni2 O8 . 8_454 97.89(7) ?
O8 Ni2 O6 8_454 7_544 88.49(7) ?
O9 Ni2 O3 . . 89.53(7) ?
O9 Ni2 O5 . . 88.74(7) ?
O9 Ni2 O6 . 7_544 85.46(7) ?
O9 Ni2 O8 . 8_454 77.80(7) ?
O4 Ni3 O6 8_454 . 85.24(7) ?
O4 Ni3 O8 8_454 8_454 166.95(8) ?
O7 Ni3 O4 . 8_454 89.94(8) ?
O7 Ni3 O6 . . 171.54(7) ?
O7 Ni3 O8 . 8_454 102.12(7) ?
O8 Ni3 O6 8_454 . 83.37(7) ?
O9 Ni3 O4 8_454 8_454 86.88(7) ?
O9 Ni3 O4 . 8_454 95.99(7) ?
O9 Ni3 O6 . . 92.72(7) ?
O9 Ni3 O6 8_454 . 85.30(7) ?
O9 Ni3 O7 . . 94.70(7) ?
O9 Ni3 O7 8_454 . 87.50(7) ?
O9 Ni3 O8 . 8_454 78.25(7) ?
O9 Ni3 O8 8_454 8_454 98.49(7) ?
O9 Ni3 O9 . 8_454 176.38(9) ?
C2 O1 Ni2 . . 126.8(2) ?
C2 O2 Ni1 . . 131.2(2) ?
Ni2 O3 Ni1 . . 95.69(7) ?
C4 O3 Ni1 . . 132.29(19) ?
C4 O3 Ni2 . . 123.22(18) ?
C4 O4 Ni3 . 7_544 131.83(17) ?
Ni2 O5 Ni1 . . 94.33(7) ?
C6 O5 Ni1 . . 135.72(19) ?
C6 O5 Ni2 . . 125.03(18) ?
Ni2 O6 Ni3 8_454 . 89.64(7) ?
C6 O6 Ni2 . 8_454 142.11(18) ?
C6 O6 Ni3 . . 127.48(17) ?
C8 O7 Ni3 . . 126.65(19) ?
Ni2 O8 Ni3 7_544 7_544 94.22(7) ?
C8 O8 Ni2 . 7_544 136.79(19) ?
C8 O8 Ni3 . 7_544 123.99(18) ?
Ni2 O9 H9 . . 111.7 ?
Ni3 O9 Ni2 . . 101.72(7) ?
Ni3 O9 Ni2 7_544 . 97.13(8) ?
Ni3 O9 Ni3 . 7_544 121.18(9) ?
Ni3 O9 H9 . . 111.7 ?
Ni3 O9 H9 7_544 . 111.7 ?
H1A C1 H1B . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
O1 C2 O2 . . 126.4(3) ?
O1 C2 C1 . . 116.4(3) ?
O2 C2 C1 . . 117.2(3) ?
H3A C3 H3B . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C4 C3 H3A . . 109.5 ?
C4 C3 H3B . . 109.5 ?
C4 C3 H3C . . 109.5 ?
O3 C4 C3 . . 118.6(3) ?
O4 C4 O3 . . 124.0(3) ?
O4 C4 C3 . . 117.4(2) ?
H5A C5 H5B . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
C6 C5 H5A . . 109.5 ?
C6 C5 H5B . . 109.5 ?
C6 C5 H5C . . 109.5 ?
O5 C6 C5 . . 119.3(3) ?
O6 C6 O5 . . 121.6(3) ?
O6 C6 C5 . . 119.1(3) ?
H7A C7 H7B . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C8 C7 H7A . . 109.5 ?
C8 C7 H7B . . 109.5 ?
C8 C7 H7C . . 109.5 ?
O7 C8 O8 . . 123.2(3) ?
O7 C8 C7 . . 117.0(3) ?
O8 C8 C7 . . 119.8(3) ?
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 O2 9_766 1.993(2) ?
Ni1 O2 . 1.993(2) y
Ni1 O3 9_766 2.1037(18) ?
Ni1 O3 . 2.1037(18) y
Ni1 O5 . 2.1257(19) y
Ni1 O5 9_766 2.1257(19) ?
Ni2 O1 . 1.993(2) y
Ni2 O9 . 1.9962(18) y
Ni2 O3 . 2.0698(18) y
Ni2 O5 . 2.0937(19) y
Ni2 O8 8_454 2.1016(18) y
Ni2 O6 7_544 2.1140(18) y
Ni3 O9 . 1.9747(18) y
Ni3 O9 8_454 1.9902(17) y
Ni3 O7 . 2.0474(19) y
Ni3 O4 8_454 2.0750(19) y
Ni3 O8 8_454 2.1023(19) y
Ni3 O6 . 2.1259(18) y
O1 C2 . 1.257(4) ?
O2 C2 . 1.259(4) ?
O3 C4 . 1.301(3) ?
O4 C4 . 1.238(3) ?
O5 C6 . 1.277(3) ?
O6 C6 . 1.255(3) ?
O7 C8 . 1.251(3) ?
O8 C8 . 1.278(3) ?
O9 H9 . 1.0000 ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C1 C2 . 1.503(5) ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C3 C4 . 1.494(4) ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C5 H5C . 0.9800 ?
C5 C6 . 1.499(4) ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C7 C8 . 1.495(4) ?
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
O9 H9 OW1 . 1.00 2.06 2.957(4) 147.4 yes
O9 H9 OW3 . 1.00 1.85 2.827(8) 165.9 yes
O7 . OW2 7_544 . . 2.87 . yes
OW2 . OW3 1_555 . . 2.85 . 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 O2 C2 O1 . . . . -4.1(5) ?
Ni1 O2 C2 C1 . . . . 175.8(2) ?
Ni1 O3 C4 O4 . . . . 151.5(2) ?
Ni1 O3 C4 C3 . . . . -30.4(4) ?
Ni1 O5 C6 O6 . . . . -164.02(18) ?
Ni1 O5 C6 C5 . . . . 16.4(4) ?
Ni2 O1 C2 O2 . . . . -1.8(5) ?
Ni2 O1 C2 C1 . . . . 178.3(2) ?
Ni2 O3 C4 O4 . . . . 12.4(4) ?
Ni2 O3 C4 C3 . . . . -169.5(2) ?
Ni2 O5 C6 O6 . . . . -15.7(4) ?
Ni2 O5 C6 C5 . . . . 164.8(2) ?
Ni2 O6 C6 O5 8_454 . . . -150.4(2) ?
Ni2 O6 C6 C5 8_454 . . . 29.1(5) ?
Ni2 O8 C8 O7 7_544 . . . 166.11(17) ?
Ni2 O8 C8 C7 7_544 . . . -13.8(4) ?
Ni3 O4 C4 O3 7_544 . . . -18.6(5) ?
Ni3 O4 C4 C3 7_544 . . . 163.2(2) ?
Ni3 O6 C6 O5 . . . . 43.1(4) ?
Ni3 O6 C6 C5 . . . . -137.4(2) ?
Ni3 O7 C8 O8 . . . . 44.2(3) ?
Ni3 O7 C8 C7 . . . . -135.9(2) ?
Ni3 O8 C8 O7 7_544 . . . 18.2(4) ?
Ni3 O8 C8 C7 7_544 . . . -161.7(2) ?
