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#$Date: 2022-02-09 11:49:22 +0200 (Wed, 09 Feb 2022) $
#$Revision: 272871 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/45/8104551.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_8104551
loop_
_publ_author_name
'Dey, Lucky'
'Rabi, Saswata'
'Begum, Zinnat A.'
'Takase, Tsugiko'
'Rahman, Ismail M.M.'
'Tiekink, Edward R.T.'
'Roy, Tapashi Ghosh'
_publ_section_title
;
 Redetermination of the crystal structure of
 bis[N,N′-ethylenebis(acetylacetoniminato)nickel(II)] sodium
 perchlorate, C24H36ClN4NaNi2O8
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1147
_journal_page_last               1150
_journal_paper_doi               10.1515/ncrs-2021-0254
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C24 H36 Cl N4 Na Ni2 O8'
_chemical_formula_sum            'C24 H36 Cl N4 Na Ni2 O8'
_chemical_formula_weight         684.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 112.0320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5909(11)
_cell_length_b                   10.8023(6)
_cell_length_c                   14.5722(8)
_cell_measurement_reflns_used    13693
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      3.14
_cell_volume                     2858.7(3)
_computing_cell_refinement       'CrystalClear [2]'
_computing_data_collection       'CrystalClear [2]'
_computing_data_reduction        'CrystalClear [2]'
_computing_molecular_graphics    'ORTEP-3 for Windows [5]'
_computing_publication_material  'SHELXL-2018/3 [4]'
_computing_structure_refinement  'SHELXL-2018/3 [4]'
_computing_structure_solution    'SHELXS [3]'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14344
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.373
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB [1]'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0409P)²+2.3767P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3129
_reflns_number_total             3261
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0254_suppl.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               8104551
_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   0.756
_shelx_estimated_absorpt_t_max   0.756
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.67462(2) 0.65612(2) 0.82671(2) 0.01590(8) Uani 1 1 d . . . . .
O1 O 0.60788(5) 0.72456(9) 0.71032(7) 0.0207(2) Uani 1 1 d . . . . .
O2 O 0.58999(5) 0.59640(9) 0.83993(7) 0.0207(2) Uani 1 1 d . . . . .
N1 N 0.75757(6) 0.71569(10) 0.80915(9) 0.0194(2) Uani 1 1 d . . . . .
N2 N 0.73819(6) 0.58926(10) 0.94563(8) 0.0184(2) Uani 1 1 d . . . . .
C1 C 0.62408(8) 0.79199(13) 0.64739(10) 0.0202(3) Uani 1 1 d . . . . .
C2 C 0.69423(8) 0.82287(13) 0.65729(11) 0.0239(3) Uani 1 1 d . . . . .
H2 H 0.699881 0.874073 0.607606 0.029 Uiso 1 1 calc R U . . .
C3 C 0.75898(8) 0.78446(13) 0.73576(11) 0.0219(3) Uani 1 1 d . . . . .
C4 C 0.82698(8) 0.66642(14) 0.88110(12) 0.0252(3) Uani 1 1 d . . . . .
H4A H 0.866150 0.729908 0.896655 0.030 Uiso 1 1 calc R U . . .
H4B H 0.842624 0.593109 0.853181 0.030 Uiso 1 1 calc R U . . .
C5 C 0.81466(7) 0.63091(14) 0.97357(11) 0.0215(3) Uani 1 1 d . . . . .
H5A H 0.848873 0.563636 1.008442 0.026 Uiso 1 1 calc R U . . .
H5B H 0.824057 0.702938 1.018655 0.026 Uiso 1 1 calc R U . . .
C6 C 0.72007(8) 0.52347(13) 1.00862(10) 0.0208(3) Uani 1 1 d . . . . .
C7 C 0.64664(8) 0.48441(14) 0.98815(11) 0.0238(3) Uani 1 1 d . . . . .
H7 H 0.638224 0.430687 1.034448 0.029 Uiso 1 1 calc R U . . .
C8 C 0.58714(8) 0.51861(13) 0.90652(10) 0.0212(3) Uani 1 1 d . . . . .
C9 C 0.55915(9) 0.83626(14) 0.55946(12) 0.0277(3) Uani 1 1 d . . . . .
H9A H 0.520992 0.772111 0.539704 0.042 Uiso 1 1 calc R U . . .
H9B H 0.574860 0.853528 0.504330 0.042 Uiso 1 1 calc R U . . .
H9C H 0.539327 0.911954 0.577096 0.042 Uiso 1 1 calc R U . . .
C10 C 0.83117(9) 0.82580(15) 0.73190(14) 0.0325(4) Uani 1 1 d . . . . .
H10A H 0.855965 0.881642 0.787464 0.049 Uiso 1 1 calc R U . . .
H10B H 0.822188 0.869280 0.669411 0.049 Uiso 1 1 calc R U . . .
H10C H 0.862402 0.753415 0.736296 0.049 Uiso 1 1 calc R U . . .
C11 C 0.77744(8) 0.48404(15) 1.10601(11) 0.0289(3) Uani 1 1 d . . . . .
H11A H 0.810566 0.423580 1.094259 0.043 Uiso 1 1 calc R U . . .
H11B H 0.753314 0.446412 1.147139 0.043 Uiso 1 1 calc R U . . .
H11C H 0.805829 0.556444 1.140091 0.043 Uiso 1 1 calc R U . . .
C12 C 0.51235(8) 0.46434(16) 0.88615(12) 0.0301(3) Uani 1 1 d . . . . .
H12A H 0.475258 0.530180 0.865340 0.045 Uiso 1 1 calc R U . . .
H12B H 0.511615 0.425025 0.946377 0.045 Uiso 1 1 calc R U . . .
H12C H 0.501329 0.402391 0.833417 0.045 Uiso 1 1 calc R U . . .
Na1 Na 0.500000 0.73770(7) 0.750000 0.02234(17) Uani 1 2 d S T P . .
Cl1 Cl 0.500000 1.02255(5) 0.750000 0.02701(12) Uani 1 2 d S T P . .
O3 O 0.54812(6) 0.94232(12) 0.82627(9) 0.0382(3) Uani 1 1 d . . . . .
O4 O 0.54217(9) 1.09586(15) 0.70970(12) 0.0587(4) Uani 1 1 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'
Cl Cl 0.1484 0.1585 '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'
Na Na 0.0362 0.0249 '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
N1 Ni O2 178.17(5) . .
N1 Ni N2 87.02(5) . .
O2 Ni N2 94.61(5) . .
N1 Ni O1 95.10(5) . .
O2 Ni O1 83.29(4) . .
N2 Ni O1 177.38(4) . .
N1 Ni Na1 135.48(4) . .
O2 Ni Na1 43.43(3) . .
N2 Ni Na1 131.85(4) . .
O1 Ni Na1 45.58(3) . .
C1 O1 Ni 126.22(9) . .
C1 O1 Na1 127.44(8) . .
Ni O1 Na1 100.68(4) . .
C8 O2 Ni 126.32(9) . .
C8 O2 Na1 127.46(8) . .
Ni O2 Na1 103.36(4) . .
C3 N1 C4 119.34(12) . .
C3 N1 Ni 126.69(10) . .
C4 N1 Ni 113.60(9) . .
C6 N2 C5 119.23(12) . .
C6 N2 Ni 126.92(10) . .
C5 N2 Ni 113.36(9) . .
O1 C1 C2 124.30(13) . .
O1 C1 C9 115.24(12) . .
C2 C1 C9 120.46(13) . .
C1 C2 C3 125.06(13) . .
C1 C2 H2 117.5 . .
C3 C2 H2 117.5 . .
N1 C3 C2 122.60(12) . .
N1 C3 C10 120.43(13) . .
C2 C3 C10 116.96(13) . .
N1 C4 C5 108.34(12) . .
N1 C4 H4A 110.0 . .
C5 C4 H4A 110.0 . .
N1 C4 H4B 110.0 . .
C5 C4 H4B 110.0 . .
H4A C4 H4B 108.4 . .
N2 C5 C4 108.64(11) . .
N2 C5 H5A 110.0 . .
C4 C5 H5A 110.0 . .
N2 C5 H5B 110.0 . .
C4 C5 H5B 110.0 . .
H5A C5 H5B 108.3 . .
N2 C6 C7 122.24(13) . .
N2 C6 C11 120.76(13) . .
C7 C6 C11 116.99(12) . .
C8 C7 C6 124.64(13) . .
C8 C7 H7 117.7 . .
C6 C7 H7 117.7 . .
O2 C8 C7 124.23(13) . .
O2 C8 C12 114.63(12) . .
C7 C8 C12 121.12(13) . .
C1 C9 H9A 109.5 . .
C1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C1 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C3 C10 H10A 109.5 . .
C3 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C3 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C6 C11 H11A 109.5 . .
C6 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C6 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C8 C12 H12A 109.5 . .
C8 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C8 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O2 Na1 O2 98.08(6) . 2_656
O2 Na1 O1 112.06(4) . 2_656
O2 Na1 O1 63.04(3) 2_656 2_656
O2 Na1 O1 63.04(3) . .
O2 Na1 O1 112.06(4) 2_656 .
O1 Na1 O1 173.20(6) 2_656 .
O2 Na1 O3 155.69(4) . 2_656
O2 Na1 O3 104.49(4) 2_656 2_656
O1 Na1 O3 86.55(4) 2_656 2_656
O1 Na1 O3 99.51(4) . 2_656
O2 Na1 O3 104.49(4) . .
O2 Na1 O3 155.69(4) 2_656 .
O1 Na1 O3 99.51(4) 2_656 .
O1 Na1 O3 86.55(4) . .
O3 Na1 O3 55.25(6) 2_656 .
O2 Na1 Cl1 130.96(3) . .
O2 Na1 Cl1 130.96(3) 2_656 .
O1 Na1 Cl1 93.40(3) 2_656 .
O1 Na1 Cl1 93.40(3) . .
O3 Na1 Cl1 27.62(3) 2_656 .
O3 Na1 Cl1 27.62(3) . .
O2 Na1 Ni 33.21(2) . .
O2 Na1 Ni 119.08(4) 2_656 .
O1 Na1 Ni 143.12(3) 2_656 .
O1 Na1 Ni 33.74(2) . .
O3 Na1 Ni 123.97(3) 2_656 .
O3 Na1 Ni 85.13(3) . .
Cl1 Na1 Ni 105.509(14) . .
O2 Na1 Ni 119.08(4) . 2_656
O2 Na1 Ni 33.21(2) 2_656 2_656
O1 Na1 Ni 33.74(2) 2_656 2_656
O1 Na1 Ni 143.12(3) . 2_656
O3 Na1 Ni 85.13(3) 2_656 2_656
O3 Na1 Ni 123.97(3) . 2_656
Cl1 Na1 Ni 105.508(14) . 2_656
Ni Na1 Ni 148.98(3) . 2_656
O4 Cl1 O4 112.25(15) . 2_656
O4 Cl1 O3 109.84(9) . .
O4 Cl1 O3 109.21(9) 2_656 .
O4 Cl1 O3 109.21(9) . 2_656
O4 Cl1 O3 109.84(9) 2_656 2_656
O3 Cl1 O3 106.32(11) . 2_656
O4 Cl1 Na1 123.87(8) . .
O4 Cl1 Na1 123.87(8) 2_656 .
O3 Cl1 Na1 53.16(5) . .
O3 Cl1 Na1 53.16(5) 2_656 .
Cl1 O3 Na1 99.22(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni N1 1.8527(11) .
Ni O2 1.8552(9) .
Ni N2 1.8592(12) .
Ni O1 1.8625(10) .
Ni Na1 3.2954(3) .
O1 C1 1.3003(16) .
O1 Na1 2.3953(9) .
O2 C8 1.3006(17) .
O2 Na1 2.3285(11) .
N1 C3 1.3110(18) .
N1 C4 1.4704(18) .
N2 C6 1.3107(18) .
N2 C5 1.4680(17) .
C1 C2 1.368(2) .
C1 C9 1.505(2) .
C2 C3 1.414(2) .
C2 H2 0.9500 .
C3 C10 1.5042(19) .
C4 C5 1.505(2) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.419(2) .
C6 C11 1.5041(19) .
C7 C8 1.367(2) .
C7 H7 0.9500 .
C8 C12 1.5008(19) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
Na1 O3 2.4948(15) 2_656
Na1 O3 2.4948(15) .
Na1 Cl1 3.0771(9) .
Cl1 O4 1.4208(14) .
Cl1 O4 1.4208(14) 2_656
Cl1 O3 1.4454(12) .
Cl1 O3 1.4454(12) 2_656
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
N1 Ni O1 C1 -1.35(11) . . . .
O2 Ni O1 C1 179.53(11) . . . .
Na1 Ni O1 C1 154.82(13) . . . .
N1 Ni O1 Na1 -156.17(5) . . . .
O2 Ni O1 Na1 24.71(5) . . . .
N2 Ni O2 C8 -9.18(12) . . . .
O1 Ni O2 C8 172.39(12) . . . .
Na1 Ni O2 C8 -161.87(13) . . . .
N2 Ni O2 Na1 152.69(5) . . . .
O1 Ni O2 Na1 -25.74(5) . . . .
N2 Ni N1 C3 -177.20(12) . . . .
O1 Ni N1 C3 1.27(12) . . . .
Na1 Ni N1 C3 -23.03(15) . . . .
N2 Ni N1 C4 9.93(10) . . . .
O1 Ni N1 C4 -171.60(10) . . . .
Na1 Ni N1 C4 164.10(8) . . . .
N1 Ni N2 C6 -178.75(12) . . . .
O2 Ni N2 C6 0.41(12) . . . .
Na1 Ni N2 C6 25.46(14) . . . .
N1 Ni N2 C5 9.45(9) . . . .
O2 Ni N2 C5 -171.38(9) . . . .
Na1 Ni N2 C5 -146.33(8) . . . .
Ni O1 C1 C2 0.4(2) . . . .
Na1 O1 C1 C2 148.59(12) . . . .
Ni O1 C1 C9 -179.62(9) . . . .
Na1 O1 C1 C9 -31.40(17) . . . .
O1 C1 C2 C3 1.2(2) . . . .
C9 C1 C2 C3 -178.77(14) . . . .
C4 N1 C3 C2 172.27(13) . . . .
Ni N1 C3 C2 -0.2(2) . . . .
C4 N1 C3 C10 -7.5(2) . . . .
Ni N1 C3 C10 179.96(11) . . . .
C1 C2 C3 N1 -1.3(2) . . . .
C1 C2 C3 C10 178.50(15) . . . .
C3 N1 C4 C5 160.54(12) . . . .
Ni N1 C4 C5 -26.01(14) . . . .
C6 N2 C5 C4 161.82(12) . . . .
Ni N2 C5 C4 -25.69(14) . . . .
N1 C4 C5 N2 32.10(15) . . . .
C5 N2 C6 C7 177.39(13) . . . .
Ni N2 C6 C7 6.0(2) . . . .
C5 N2 C6 C11 -3.74(19) . . . .
Ni N2 C6 C11 -175.10(10) . . . .
N2 C6 C7 C8 -5.6(2) . . . .
C11 C6 C7 C8 175.45(14) . . . .
Ni O2 C8 C7 11.8(2) . . . .
Na1 O2 C8 C7 -145.82(12) . . . .
Ni O2 C8 C12 -166.67(10) . . . .
Na1 O2 C8 C12 35.75(17) . . . .
C6 C7 C8 O2 -3.7(2) . . . .
C6 C7 C8 C12 174.66(14) . . . .
O4 Cl1 O3 Na1 -118.04(8) . . . .
O4 Cl1 O3 Na1 118.45(9) 2_656 . . .
O3 Cl1 O3 Na1 0.002(1) 2_656 . . .
