#------------------------------------------------------------------------------
#$Date: 2021-04-15 11:10:23 +0200 (jue 15 de abr de 2021) $
#$Revision: 264198 $
#$URL: svn://www.crystallography.net/cod/cif/1/56/18/1561814.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_1561814
loop_
_publ_author_name
'Gurzhiy, Vladislav V.'
'Kovrugin, Vadim M.'
'Tyumentseva, Olga S.'
'Mikhaylenko, Pavel A.'
'Krivovichev, Sergey V.'
'Tananaev, Ivan G.'
_publ_section_title
;
 Topologically and geometrically flexible structural units in seven new
 organically templated uranyl selenates and selenite--selenates
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              32
_journal_page_last               40
_journal_paper_doi               10.1016/j.jssc.2015.04.040
_journal_volume                  229
_journal_year                    2015
_chemical_formula_moiety         'H2 O11 Se2 U, 2(C2 H8 N)'
_chemical_formula_sum            'C4 H18 N2 O11 Se2 U'
_chemical_formula_weight         666.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5363(7)
_cell_length_b                   12.2021(11)
_cell_length_c                   16.7601(16)
_cell_measurement_reflns_used    5132
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      35.12
_cell_measurement_theta_min      2.96
_cell_volume                     1541.2(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13644
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.064
_exptl_absorpt_coefficient_mu    15.306
_exptl_absorpt_correction_T_max  0.3224
_exptl_absorpt_correction_T_min  0.1779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.871
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.339
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.204
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.188(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4492
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0311
_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)+(0.0280P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4117
_reflns_number_total             4492
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            CompI_last.cif
_cod_data_source_block           compound_I
_cod_database_code               1561814
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.812(14) 0.188(14)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 H11A-H11B
 1.5 with sigma of 0.02
 O11-H11A = O11-H11B
 0.9 with sigma of 0.02
 H11B-U1 = U1-H11A
 2.9 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 N2(H2D,H2E), N1(H1D,H1E)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, 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
U1 U -2.88384(4) 0.65079(3) 0.24285(2) 0.01479(8) Uani 1 1 d D . . . .
Se1 Se -2.78689(10) 0.35665(8) 0.18605(5) 0.01427(16) Uani 1 1 d . . . . .
Se2 Se -3.21320(11) 0.44112(7) 0.31498(5) 0.01546(18) Uani 1 1 d . . . . .
O1 O -2.8609(8) 0.6517(6) 0.3482(3) 0.0234(12) Uani 1 1 d . . . . .
O2 O -2.9073(8) 0.6511(6) 0.1376(3) 0.0244(13) Uani 1 1 d . . . . .
O3 O -2.7582(8) 0.4706(4) 0.2372(5) 0.0277(16) Uani 1 1 d . . . . .
O4 O -2.5940(10) 0.3104(6) 0.1595(4) 0.0318(17) Uani 1 1 d . . . . .
O5 O -2.8711(7) 0.2666(4) 0.2502(4) 0.0196(12) Uani 1 1 d . . . . .
O6 O -2.9181(9) 0.3744(6) 0.1108(4) 0.0297(17) Uani 1 1 d . . . . .
O7 O -3.1244(7) 0.5377(4) 0.2543(3) 0.0110(10) Uani 1 1 d . . . . .
O8 O -3.0866(10) 0.4182(6) 0.3913(4) 0.0283(17) Uani 1 1 d . . . . .
O9 O -3.2381(8) 0.3299(4) 0.2610(4) 0.0259(15) Uani 1 1 d . . . . .
O10 O -3.4083(9) 0.4859(6) 0.3411(5) 0.0349(18) Uani 1 1 d . . . . .
O11 O -2.5535(8) 0.6502(5) 0.2430(4) 0.0294(14) Uani 1 1 d D . . . .
H11A H -2.516(4) 0.588(4) 0.266(6) 0.044 Uiso 1 1 d DR . . . .
H11B H -2.516(4) 0.711(4) 0.267(5) 0.044 Uiso 1 1 d DR . . . .
C1 C -3.7074(18) 0.4699(10) 0.4750(7) 0.044(3) Uani 1 1 d . . . . .
H1A H -3.7201 0.5438 0.4563 0.066 Uiso 1 1 calc GR . . . .
H1B H -3.5949 0.4619 0.5012 0.066 Uiso 1 1 calc GR . . . .
H1C H -3.8011 0.4534 0.5118 0.066 Uiso 1 1 calc GR . . . .
C2 C -3.661(2) 0.2836(10) 0.4261(8) 0.060(5) Uani 1 1 d . . . . .
H2A H -3.6828 0.2370 0.3810 0.090 Uiso 1 1 calc GR . . . .
H2B H -3.7270 0.2572 0.4712 0.090 Uiso 1 1 calc GR . . . .
H2C H -3.5367 0.2831 0.4385 0.090 Uiso 1 1 calc GR . . . .
N2 N -3.2817(13) 0.3830(7) 0.0833(5) 0.030(2) Uani 1 1 d . . . . .
H2D H -3.1663 0.3690 0.1067 0.037 Uiso 1 1 calc R . . . .
H2E H -3.3707 0.3520 0.1185 0.037 Uiso 1 1 calc R . . . .
C3 C -3.3093(19) 0.5024(9) 0.0780(8) 0.046(3) Uani 1 1 d . . . . .
H3A H -3.2319 0.5324 0.0381 0.069 Uiso 1 1 calc GR . . . .
H3B H -3.2836 0.5354 0.1287 0.069 Uiso 1 1 calc GR . . . .
H3C H -3.4304 0.5171 0.0638 0.069 Uiso 1 1 calc GR . . . .
C4 C -3.292(2) 0.3274(9) 0.0055(8) 0.051(3) Uani 1 1 d . . . . .
H4A H -3.1941 0.3503 -0.0273 0.076 Uiso 1 1 calc GR . . . .
H4B H -3.4014 0.3462 -0.0203 0.076 Uiso 1 1 calc GR . . . .
H4C H -3.2866 0.2496 0.0133 0.076 Uiso 1 1 calc GR . . . .
N1 N -3.7165(14) 0.3947(8) 0.4074(6) 0.033(2) Uani 1 1 d . . . . .
H1D H -3.8376 0.3928 0.3878 0.040 Uiso 1 1 calc R . . . .
H1E H -3.6421 0.4227 0.3649 0.040 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
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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 O3 90.4(3) . .
O1 U1 O5 91.4(3) . 4_/55
O1 U1 O7 89.9(3) . .
O1 U1 O9 89.1(3) . 4_/55
O1 U1 O11 84.3(3) . .
O2 U1 O1 179.5(3) . .
O2 U1 O3 90.1(3) . .
O2 U1 O5 88.2(3) . 4_/55
O2 U1 O7 90.3(3) . .
O2 U1 O9 90.5(3) . 4_/55
O2 U1 O11 95.8(3) . .
O3 U1 O11 66.6(2) . .
O5 U1 O3 150.7(2) 4_/55 .
O5 U1 O9 75.49(19) 4_/55 4_/55
O5 U1 O11 142.6(2) 4_/55 .
O7 U1 O3 76.26(19) . .
O7 U1 O5 74.54(17) . 4_/55
O7 U1 O9 150.0(2) . 4_/55
O7 U1 O11 142.28(19) . .
O9 U1 O3 133.7(2) 4_/55 .
O9 U1 O11 67.4(2) 4_/55 .
O3 Se1 O5 105.7(3) . .
O4 Se1 O3 108.6(3) . .
O4 Se1 O5 106.8(3) . .
O6 Se1 O3 111.9(3) . .
O6 Se1 O4 112.4(4) . .
O6 Se1 O5 111.0(3) . .
O8 Se2 O7 111.2(3) . .
O8 Se2 O9 111.1(3) . .
O8 Se2 O10 112.2(4) . .
O9 Se2 O7 106.8(3) . .
O10 Se2 O7 106.6(3) . .
O10 Se2 O9 108.8(3) . .
Se1 O3 U1 138.0(4) . .
Se1 O5 U1 137.4(4) . 4_/45
Se2 O7 U1 141.6(3) . .
Se2 O9 U1 137.1(4) . 4_/45
U1 O11 H11A 109(2) . .
U1 O11 H11B 109(2) . .
H11A O11 H11B 114(4) . .
H1A C1 H1B 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2D N2 H2E 107.7 . .
C3 N2 H2D 108.9 . .
C3 N2 H2E 108.9 . .
C4 N2 H2D 108.9 . .
C4 N2 H2E 108.9 . .
C4 N2 C3 113.3(9) . .
N2 C3 H3A 109.5 . .
N2 C3 H3B 109.5 . .
N2 C3 H3C 109.5 . .
H3A C3 H3B 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N2 C4 H4A 109.5 . .
N2 C4 H4B 109.5 . .
N2 C4 H4C 109.5 . .
H4A C4 H4B 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C1 N1 H1D 108.8 . .
C1 N1 H1E 108.8 . .
C2 N1 C1 114.0(10) . .
C2 N1 H1D 108.8 . .
C2 N1 H1E 108.8 . .
H1D N1 H1E 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.774(5) .
U1 O2 1.772(5) .
U1 O3 2.396(6) .
U1 O5 2.328(5) 4_/55
U1 O7 2.287(5) .
U1 O9 2.372(5) 4_/55
U1 O11 2.489(6) .
Se1 O3 1.647(6) .
Se1 O4 1.622(7) .
Se1 O5 1.663(5) .
Se1 O6 1.617(7) .
Se2 O7 1.694(5) .
Se2 O8 1.621(7) .
Se2 O9 1.642(5) .
Se2 O10 1.628(7) .
O5 U1 2.328(5) 4_/45
O9 U1 2.372(5) 4_/45
O11 H11A 0.89(3) .
O11 H11B 0.89(3) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C1 N1 1.459(13) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C2 N1 1.453(15) .
N2 H2D 0.9700 .
N2 H2E 0.9700 .
N2 C3 1.474(13) .
N2 C4 1.471(14) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
N1 H1D 0.9700 .
N1 H1E 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 Se1 O5 U1 126.9(5) . . . 4_/45
O4 Se1 O3 U1 134.9(5) . . . .
O4 Se1 O5 U1 -117.6(5) . . . 4_/45
O5 Se1 O3 U1 -110.8(6) . . . .
O6 Se1 O3 U1 10.2(7) . . . .
O6 Se1 O5 U1 5.3(6) . . . 4_/45
O7 Se2 O9 U1 113.4(5) . . . 4_/45
O8 Se2 O7 U1 -0.8(6) . . . .
O8 Se2 O9 U1 -8.0(7) . . . 4_/45
O9 Se2 O7 U1 -122.2(5) . . . .
O10 Se2 O7 U1 121.7(5) . . . .
O10 Se2 O9 U1 -131.9(5) . . . 4_/45
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.812(14)
2 0.188(14)

_cod_database_fobs_code 1561814
