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#$Date: 2025-08-21 03:19:08 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301842 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/50/23/4502355.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_4502355
loop_
_publ_author_name
'Biju, A. R.'
'Rajasekharan, M. V.'
_publ_section_title
;
 [Mn(acac)2(HOCH3)2]3[Ce(NO3)6]---Icosahedral Anion Builds a Cubic Network
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              426
_journal_paper_doi               10.1021/cg901027c
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         '3(C12 H22 Mn O6), Ce N6 O18'
_chemical_formula_sum            'C36 H66 Ce Mn3 N6 O36'
_chemical_formula_weight         1463.89
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.5842(3)
_cell_length_b                   16.5842(3)
_cell_length_c                   18.3249(8)
_cell_measurement_reflns_used    9165
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.46
_cell_volume                     4364.8(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16956
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.505
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2235
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2362
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0277P)²+7.6915P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                2284
_reflns_number_total             2362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg901027c_si_002.cif
_cod_data_source_block           mvr181
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4502355
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ce Ce 0.6667 0.3333 0.3333 0.01233(7) Uani 1 6 d S
Mn Mn 0.5000 0.0000 0.0000 0.01576(9) Uani 1 2 d S
O1 O 0.39034(8) -0.02329(8) 0.05175(6) 0.0186(2) Uani 1 1 d .
O2 O 0.49153(9) 0.08665(9) -0.06338(6) 0.0213(3) Uani 1 1 d .
O3 O 0.57899(9) 0.11536(10) 0.07827(7) 0.0257(3) Uani 1 1 d D
O4 O 0.83909(8) 0.45757(8) 0.37455(6) 0.0193(2) Uani 1 1 d .
O5 O 0.61343(8) 0.39529(8) 0.22386(6) 0.0209(2) Uani 1 1 d .
O6 O 0.87211(10) 0.54194(10) 0.47330(7) 0.0346(3) Uani 1 1 d .
N1 N 0.81515(10) 0.48421(10) 0.43076(8) 0.0196(3) Uani 1 1 d .
C1 C 0.27558(12) 0.00267(12) 0.10456(9) 0.0217(3) Uani 1 1 d .
H1A H 0.2161 -0.0454 0.0843 0.032 Uiso 1 1 calc R
H1B H 0.2716 0.0582 0.1163 0.032 Uiso 1 1 calc R
H1C H 0.2896 -0.0209 0.1490 0.032 Uiso 1 1 calc R
C2 C 0.35112(11) 0.02715(11) 0.04976(8) 0.0166(3) Uani 1 1 d .
C3 C 0.37377(11) 0.09868(12) 0.00004(9) 0.0189(3) Uani 1 1 d .
H3 H 0.3420 0.1329 0.0038 0.023 Uiso 1 1 calc R
C4 C 0.43983(11) 0.12318(11) -0.05470(8) 0.0177(3) Uani 1 1 d .
C5 C 0.45426(14) 0.19520(13) -0.11029(9) 0.0253(4) Uani 1 1 d .
H5A H 0.5210 0.2350 -0.1197 0.038 Uiso 1 1 calc R
H5B H 0.4287 0.2333 -0.0919 0.038 Uiso 1 1 calc R
H5C H 0.4225 0.1645 -0.1557 0.038 Uiso 1 1 calc R
C6 C 0.67019(15) 0.19128(15) 0.06714(12) 0.0384(5) Uani 1 1 d .
H6A H 0.7150 0.1692 0.0693 0.058 Uiso 1 1 calc R
H6B H 0.6849 0.2381 0.1052 0.058 Uiso 1 1 calc R
H6C H 0.6738 0.2190 0.0192 0.058 Uiso 1 1 calc R
H31 H 0.558(2) 0.123(2) 0.1115(14) 0.058 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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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
O5 Ce O5 66.92(4) 18_545 17
O5 Ce O5 113.08(4) 18_545 2_655
O5 Ce O5 180.0 17 2_655
O5 Ce O5 180.0 18_545 3_665
O5 Ce O5 113.08(4) 17 3_665
O5 Ce O5 66.91(4) 2_655 3_665
O5 Ce O5 113.09(4) 18_545 .
O5 Ce O5 113.09(4) 17 .
O5 Ce O5 66.91(4) 2_655 .
O5 Ce O5 66.91(4) 3_665 .
O5 Ce O5 66.92(4) 18_545 16_655
O5 Ce O5 66.92(4) 17 16_655
O5 Ce O5 113.08(4) 2_655 16_655
O5 Ce O5 113.08(4) 3_665 16_655
O5 Ce O5 180.0 . 16_655
O5 Ce O4 110.99(4) 18_545 18_545
O5 Ce O4 68.54(4) 17 18_545
O5 Ce O4 111.46(4) 2_655 18_545
O5 Ce O4 69.01(4) 3_665 18_545
O5 Ce O4 48.43(4) . 18_545
O5 Ce O4 131.57(4) 16_655 18_545
O5 Ce O4 68.54(4) 18_545 16_655
O5 Ce O4 131.57(4) 17 16_655
O5 Ce O4 48.43(4) 2_655 16_655
O5 Ce O4 111.46(4) 3_665 16_655
O5 Ce O4 69.01(4) . 16_655
O5 Ce O4 110.99(4) 16_655 16_655
O4 Ce O4 112.30(2) 18_545 16_655
O5 Ce O4 69.01(4) 18_545 3_665
O5 Ce O4 111.46(4) 17 3_665
O5 Ce O4 68.54(4) 2_655 3_665
O5 Ce O4 110.99(4) 3_665 3_665
O5 Ce O4 131.57(4) . 3_665
O5 Ce O4 48.43(4) 16_655 3_665
O4 Ce O4 180.0 18_545 3_665
O4 Ce O4 67.70(2) 16_655 3_665
O5 Ce O4 111.46(4) 18_545 .
O5 Ce O4 48.43(4) 17 .
O5 Ce O4 131.57(4) 2_655 .
O5 Ce O4 68.54(4) 3_665 .
O5 Ce O4 110.99(4) . .
O5 Ce O4 69.01(4) 16_655 .
O4 Ce O4 67.70(2) 18_545 .
O4 Ce O4 180.0 16_655 .
O4 Ce O4 112.30(2) 3_665 .
O5 Ce O4 48.43(4) 18_545 2_655
O5 Ce O4 69.02(4) 17 2_655
O5 Ce O4 110.99(4) 2_655 2_655
O5 Ce O4 131.57(4) 3_665 2_655
O5 Ce O4 68.54(4) . 2_655
O5 Ce O4 111.46(4) 16_655 2_655
O4 Ce O4 67.70(2) 18_545 2_655
O4 Ce O4 67.70(2) 16_655 2_655
O4 Ce O4 112.30(2) 3_665 2_655
O4 Ce O4 112.30(2) . 2_655
O5 Ce O4 131.57(4) 18_545 17
O5 Ce O4 110.98(4) 17 17
O5 Ce O4 69.01(4) 2_655 17
O5 Ce O4 48.43(4) 3_665 17
O5 Ce O4 111.46(4) . 17
O5 Ce O4 68.54(4) 16_655 17
O4 Ce O4 112.30(2) 18_545 17
O4 Ce O4 112.30(2) 16_655 17
O4 Ce O4 67.70(2) 3_665 17
O4 Ce O4 67.70(2) . 17
O4 Ce O4 180.0 2_655 17
O2 Mn O2 180.00(8) . 10_655
O2 Mn O1 88.09(5) . 10_655
O2 Mn O1 91.91(5) 10_655 10_655
O2 Mn O1 91.91(5) . .
O2 Mn O1 88.09(5) 10_655 .
O1 Mn O1 180.00(9) 10_655 .
O2 Mn O3 91.26(5) . 10_655
O2 Mn O3 88.74(5) 10_655 10_655
O1 Mn O3 86.87(5) 10_655 10_655
O1 Mn O3 93.13(5) . 10_655
O2 Mn O3 88.74(5) . .
O2 Mn O3 91.26(5) 10_655 .
O1 Mn O3 93.13(5) 10_655 .
O1 Mn O3 86.87(5) . .
O3 Mn O3 180.00(8) 10_655 .
C2 O1 Mn 126.26(10) . .
C4 O2 Mn 126.78(11) . .
C6 O3 Mn 125.47(11) . .
N1 O4 Ce 95.64(9) . .
N1 O5 Ce 98.50(9) 18_545 .
O6 N1 O4 122.48(15) . .
O6 N1 O5 120.16(15) . 17
O4 N1 O5 117.36(13) . 17
O1 C2 C3 124.22(15) . .
O1 C2 C1 115.49(14) . .
C3 C2 C1 120.28(14) . .
C4 C3 C2 124.08(15) . .
O2 C4 C3 124.56(15) . .
O2 C4 C5 114.51(14) . .
C3 C4 C5 120.92(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce O5 2.6011(12) 18_545
Ce O5 2.6011(12) 17
Ce O5 2.6012(12) 2_655
Ce O5 2.6012(12) 3_665
Ce O5 2.6012(11) .
Ce O5 2.6012(12) 16_655
Ce O4 2.6647(12) 18_545
Ce O4 2.6647(12) 16_655
Ce O4 2.6647(12) 3_665
Ce O4 2.6647(12) .
Ce O4 2.6647(12) 2_655
Ce O4 2.6648(12) 17
Mn O2 1.9068(11) .
Mn O2 1.9068(11) 10_655
Mn O1 1.9113(11) 10_655
Mn O1 1.9113(11) .
Mn O3 2.2197(13) 10_655
Mn O3 2.2197(13) .
O1 C2 1.2917(19) .
O2 C4 1.2832(19) .
O3 C6 1.418(2) .
O4 N1 1.2606(18) .
O5 N1 1.2684(19) 18_545
O6 N1 1.2297(19) .
N1 O5 1.2684(19) 17
C1 C2 1.495(2) .
C2 C3 1.390(2) .
C3 C4 1.388(2) .
C4 C5 1.495(2) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168345028
