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#$Date: 2025-08-21 01:01:10 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301838 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/51/4325102.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_4325102
loop_
_publ_author_name
'Kalyan V. Vasudevan'
'Nickolaus A. Smith'
'Brian L. Scott'
'Edward A. McKigney'
'Michael W. Blair'
'John C. Gordon'
'Ross E. Muenchausen'
_publ_section_title
;
 An Ionic Liquid-Mediated Route to Cerium(III) Bromide Solvates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4627
_journal_page_last               4631
_journal_paper_doi               10.1021/ic200353s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C20 H40 Br3 Ce O4'
_chemical_formula_weight         724.37
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 131.149(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.421(9)
_cell_length_b                   9.395(4)
_cell_length_c                   16.657(11)
_cell_measurement_temperature    140(1)
_cell_volume                     2642(2)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω 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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13442
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.281
_exptl_absorpt_correction_T_max  0.5195
_exptl_absorpt_correction_T_min  0.2722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.996
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.435
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3106
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.438
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0359
_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)+(0.0635P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                2374
_reflns_number_total             3106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200353s_si_003.cif
_cod_data_source_block           apx1155a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4325102
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.0000 0.25234(4) 0.2500 0.01608(15) Uani 1 2 d S . .
Br1 Br 0.11840(3) 0.25409(5) 0.48022(4) 0.02877(19) Uani 1 1 d . . .
Br2 Br 0.0000 0.56150(8) 0.2500 0.0340(2) Uani 1 2 d S . .
O1 O 0.0805(2) 0.0317(3) 0.2869(3) 0.0239(8) Uani 1 1 d . . .
O2 O 0.0926(2) 0.3113(4) 0.2182(3) 0.0254(8) Uani 1 1 d . B .
C1 C 0.1584(3) -0.0272(7) 0.3780(5) 0.0336(13) Uani 1 1 d . . .
H1 H 0.1937 0.0511 0.4244 0.040 Uiso 1 1 calc R . .
C2 C 0.1904(4) -0.0979(7) 0.3306(5) 0.0426(16) Uani 1 1 d . . .
H2A H 0.2430 -0.0630 0.3646 0.051 Uiso 1 1 calc R . .
H2B H 0.1926 -0.2004 0.3389 0.051 Uiso 1 1 calc R . .
C3 C 0.1311(4) -0.0561(7) 0.2121(5) 0.0435(16) Uani 1 1 d . . .
H3A H 0.1462 0.0324 0.1998 0.052 Uiso 1 1 calc R . .
H3B H 0.1266 -0.1301 0.1678 0.052 Uiso 1 1 calc R . .
C4 C 0.0558(4) -0.0399(6) 0.1915(5) 0.0382(15) Uani 1 1 d . . .
H4A H 0.0178 0.0173 0.1284 0.046 Uiso 1 1 calc R . .
H4B H 0.0324 -0.1319 0.1825 0.046 Uiso 1 1 calc R . .
C5 C 0.1512(4) -0.1265(7) 0.4401(5) 0.0426(15) Uani 1 1 d . . .
H5A H 0.1307 -0.0764 0.4677 0.064 Uiso 1 1 calc R . .
H5B H 0.2024 -0.1649 0.4982 0.064 Uiso 1 1 calc R . .
H5C H 0.1158 -0.2026 0.3948 0.064 Uiso 1 1 calc R . .
C6 C 0.1741(3) 0.3414(8) 0.3126(5) 0.0444(18) Uani 1 1 d . . .
H6A H 0.1797 0.3401 0.3755 0.053 Uiso 1 1 calc R A 1
H6B H 0.2090 0.2697 0.3211 0.053 Uiso 1 1 calc R A 1
C7 C 0.1941(13) 0.476(3) 0.3003(16) 0.057(8) Uani 0.46(5) 1 d PDU B 1
H7A H 0.2475 0.4753 0.3261 0.069 Uiso 0.50 1 calc PR B 1
H7B H 0.1914 0.5469 0.3403 0.069 Uiso 0.50 1 calc PR B 1
C7' C 0.2075(8) 0.4332(19) 0.2770(11) 0.035(5) Uani 0.54(5) 1 d PU B 2
H7'1 H 0.2317 0.3762 0.2566 0.042 Uiso 0.50 1 calc PR B 2
H7'2 H 0.2464 0.4994 0.3325 0.042 Uiso 0.50 1 calc PR B 2
C8 C 0.1347(4) 0.5109(7) 0.1817(5) 0.0407(16) Uani 1 1 d D . .
H8A H 0.1608 0.5138 0.1530 0.049 Uiso 1 1 calc R B 1
H8B H 0.1102 0.6026 0.1698 0.049 Uiso 1 1 calc R B 1
C9 C 0.0731(3) 0.3937(6) 0.1287(4) 0.0247(12) Uani 1 1 d . B .
H9 H 0.0204 0.4361 0.0884 0.030 Uiso 1 1 calc R . .
C10 C 0.0729(4) 0.2978(7) 0.0568(5) 0.0417(15) Uani 1 1 d . . .
H10A H 0.1254 0.2619 0.0944 0.063 Uiso 1 1 calc R B .
H10B H 0.0559 0.3503 -0.0047 0.063 Uiso 1 1 calc R . .
H10C H 0.0374 0.2197 0.0345 0.063 Uiso 1 1 calc R . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
O2 Ce1 O2 154.59(17) . 2
O2 Ce1 O1 71.22(12) . .
O2 Ce1 O1 132.86(12) 2 .
O2 Ce1 O1 132.87(12) . 2
O2 Ce1 O1 71.22(12) 2 2
O1 Ce1 O1 70.87(16) . 2
O2 Ce1 Br1 83.36(9) . 2
O2 Ce1 Br1 96.50(9) 2 2
O1 Ce1 Br1 102.20(8) . 2
O1 Ce1 Br1 78.34(8) 2 2
O2 Ce1 Br1 96.50(10) . .
O2 Ce1 Br1 83.35(9) 2 .
O1 Ce1 Br1 78.34(8) . .
O1 Ce1 Br1 102.20(8) 2 .
Br1 Ce1 Br1 179.35(2) 2 .
O2 Ce1 Br2 77.30(8) . .
O2 Ce1 Br2 77.30(8) 2 .
O1 Ce1 Br2 144.56(8) . .
O1 Ce1 Br2 144.56(8) 2 .
Br1 Ce1 Br2 89.675(12) 2 .
Br1 Ce1 Br2 89.674(12) . .
C4 O1 C1 107.0(4) . .
C4 O1 Ce1 114.3(3) . .
C1 O1 Ce1 136.6(3) . .
C6 O2 C9 108.5(4) . .
C6 O2 Ce1 116.1(3) . .
C9 O2 Ce1 126.4(3) . .
C5 C1 O1 110.9(5) . .
C5 C1 C2 113.1(5) . .
O1 C1 C2 105.8(5) . .
C3 C2 C1 104.5(5) . .
C4 C3 C2 102.3(5) . .
O1 C4 C3 103.6(5) . .
C7 C6 O2 108.3(8) . .
C7 C6 C7' 29.6(11) . .
O2 C6 C7' 106.5(6) . .
C6 C7 C8 106.9(12) . .
C6 C7' C8 102.6(9) . .
C7' C8 C7 28.4(10) . .
C7' C8 C9 101.6(7) . .
C7 C8 C9 106.5(8) . .
O2 C9 C10 109.7(5) . .
O2 C9 C8 104.1(4) . .
C10 C9 C8 115.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 O2 2.518(3) .
Ce1 O2 2.518(3) 2
Ce1 O1 2.544(3) .
Ce1 O1 2.544(3) 2
Ce1 Br1 2.891(2) 2
Ce1 Br1 2.891(2) .
Ce1 Br2 2.9044(14) .
O1 C4 1.457(7) .
O1 C1 1.474(7) .
O2 C6 1.453(6) .
O2 C9 1.469(6) .
C1 C5 1.479(8) .
C1 C2 1.524(8) .
C2 C3 1.537(9) .
C3 C4 1.493(9) .
C6 C7 1.403(18) .
C6 C7' 1.496(14) .
C7 C8 1.524(16) .
C7' C8 1.519(16) .
C8 C9 1.515(8) .
C9 C10 1.497(8) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139135708
