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#$Date: 2021-04-12 12:07:51 +0300 (Mon, 12 Apr 2021) $
#$Revision: 264055 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/16/1561660.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_1561660
loop_
_publ_author_name
'Kohlgruber, Tsuyoshi A.'
'Mackley, Stephanie A.'
'Bo, Fabrice Dal'
'Aksenov, Sergey M.'
'Burns, Peter C.'
_publ_section_title
;
 The role of 1-ethyl-3-methylimidazolium diethyl phosphate ionic liquid in
 uranyl phosphate compounds
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              120938
_journal_paper_doi               10.1016/j.jssc.2019.120938
_journal_volume                  279
_journal_year                    2019
_chemical_formula_sum            'C2 H5 O2.5 P0.5 U0.25'
_chemical_formula_weight         144.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                105.333(6)
_cell_angle_beta                 90.562(6)
_cell_angle_gamma                98.269(6)
_cell_formula_units_Z            4
_cell_length_a                   5.374(3)
_cell_length_b                   7.674(4)
_cell_length_c                   11.132(6)
_cell_measurement_reflns_used    2716
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.78
_cell_volume                     437.6(4)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5141
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_min         1.899
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    9.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.186
_exptl_crystal_description       blocky
_exptl_crystal_F_000             270
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.015
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6043
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0243
_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)+(0.0241P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0501
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1979
_reflns_number_total             1993
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            chain1_final.cif
_cod_data_source_block           try3_a
_cod_original_formula_sum        'C2 H5 O2.50 P0.50 U0.25'
_cod_database_code               1561660
_shelx_shelxl_version_number     2016/6
_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   0.536
_shelx_estimated_absorpt_t_max   0.871
_diffrn_source_monochromator     'MONTEL Multi-layer'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
U1 U 1.000000 0.500000 0.500000 0.02812(8) Uani 1 2 d S . P . .
P1 P 0.49100(19) 0.46452(15) 0.71276(10) 0.0322(2) Uani 1 1 d . . . . .
O1 O 0.8517(6) 0.2741(4) 0.4362(3) 0.0454(7) Uani 1 1 d . . . . .
O2 O 0.7253(5) 0.5339(5) 0.6578(3) 0.0473(8) Uani 1 1 d . . . . .
O3 O 0.2640(5) 0.4011(4) 0.6238(3) 0.0410(7) Uani 1 1 d . . . . .
O4 O 0.4480(6) 0.6223(4) 0.8279(3) 0.0472(8) Uani 1 1 d . . . . .
O5 O 0.5337(7) 0.3064(5) 0.7716(3) 0.0536(9) Uani 1 1 d . . . . .
C1 C 0.2295(10) 0.6081(8) 0.9020(5) 0.0568(13) Uani 1 1 d . . . . .
H1A H 0.277141 0.582207 0.979947 0.068 Uiso 1 1 calc R U . . .
H1B H 0.101354 0.507892 0.856031 0.068 Uiso 1 1 calc R U . . .
C2 C 0.1273(12) 0.7823(9) 0.9295(7) 0.081(2) Uani 1 1 d . . . . .
H2A H -0.019154 0.773991 0.979039 0.121 Uiso 1 1 calc R U . . .
H2B H 0.254593 0.880770 0.975490 0.121 Uiso 1 1 calc R U . . .
H2C H 0.079329 0.806677 0.851943 0.121 Uiso 1 1 calc R U . . .
C3 C 0.5052(13) 0.1166(8) 0.6987(7) 0.084(2) Uani 1 1 d . . . . .
H3A H 0.372783 0.045222 0.733294 0.100 Uiso 1 1 calc R U . . .
H3B H 0.450070 0.108944 0.613008 0.100 Uiso 1 1 calc R U . . .
C4 C 0.7245(14) 0.0385(9) 0.6958(9) 0.107(3) Uani 1 1 d . . . . .
H4A H 0.691961 -0.087542 0.645717 0.160 Uiso 1 1 calc R U . . .
H4B H 0.855711 0.106216 0.659561 0.160 Uiso 1 1 calc R U . . .
H4C H 0.778337 0.042423 0.779981 0.160 Uiso 1 1 calc R U . . .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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
O1 U1 O1 180.0 2_766 .
O1 U1 O2 90.04(14) 2_766 2_766
O1 U1 O2 89.96(13) . 2_766
O1 U1 O2 89.96(13) 2_766 .
O1 U1 O2 90.04(14) . .
O2 U1 O2 180.0 2_766 .
O1 U1 O3 90.25(13) 2_766 2_666
O1 U1 O3 89.75(13) . 2_666
O2 U1 O3 88.19(12) 2_766 2_666
O2 U1 O3 91.81(12) . 2_666
O1 U1 O3 89.75(13) 2_766 1_655
O1 U1 O3 90.25(13) . 1_655
O2 U1 O3 91.81(12) 2_766 1_655
O2 U1 O3 88.19(12) . 1_655
O3 U1 O3 180.0 2_666 1_655
O2 P1 O3 114.78(18) . .
O2 P1 O4 105.77(19) . .
O3 P1 O4 112.25(18) . .
O2 P1 O5 111.3(2) . .
O3 P1 O5 108.81(19) . .
O4 P1 O5 103.32(19) . .
P1 O2 U1 149.9(2) . .
P1 O3 U1 142.61(19) . 1_455
C1 O4 P1 121.7(3) . .
C3 O5 P1 122.3(4) . .
O4 C1 C2 108.9(5) . .
O4 C1 H1A 109.9 . .
C2 C1 H1A 109.9 . .
O4 C1 H1B 109.9 . .
C2 C1 H1B 109.9 . .
H1A C1 H1B 108.3 . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C4 C3 O5 113.9(6) . .
C4 C3 H3A 108.8 . .
O5 C3 H3A 108.8 . .
C4 C3 H3B 108.8 . .
O5 C3 H3B 108.8 . .
H3A C3 H3B 107.7 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.757(3) 2_766
U1 O1 1.757(3) .
U1 O2 2.292(3) 2_766
U1 O2 2.292(3) .
U1 O3 2.305(3) 2_666
U1 O3 2.305(3) 1_655
P1 O2 1.496(3) .
P1 O3 1.502(3) .
P1 O4 1.558(3) .
P1 O5 1.566(3) .
O4 C1 1.449(6) .
O5 C3 1.454(6) .
C1 C2 1.477(8) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 H2C 0.9700 .
C3 C4 1.394(9) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 H4C 0.9700 .
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
O3 P1 O2 U1 -47.0(5) . . . .
O4 P1 O2 U1 -171.3(4) . . . .
O5 P1 O2 U1 77.1(4) . . . .
O2 P1 O3 U1 -61.5(3) . . . 1_455
O4 P1 O3 U1 59.3(3) . . . 1_455
O5 P1 O3 U1 173.0(3) . . . 1_455
O2 P1 O4 C1 177.0(4) . . . .
O3 P1 O4 C1 51.1(4) . . . .
O5 P1 O4 C1 -66.0(4) . . . .
O2 P1 O5 C3 -86.2(5) . . . .
O3 P1 O5 C3 41.3(5) . . . .
O4 P1 O5 C3 160.7(4) . . . .
P1 O4 C1 C2 -136.4(5) . . . .
P1 O5 C3 C4 118.9(7) . . . .
