#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/90/2019033.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019033
loop_
_publ_author_name
'Savchenkov, Anton V.'
'Vologzhanina, Anna V.'
'Serezhkina, Larisa B.'
'Pushkin, Denis V.'
'Serezhkin, Viktor N.'
_publ_section_title
;
 The first uranyl complexes with valerate ions
;
_journal_coeditor_code           FA3320
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              721
_journal_page_last               726
_journal_paper_doi               10.1107/S0108270113014832
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[U (C5 H9 O2)2 O2 (H2 O)2]'
_chemical_formula_moiety         'C10 H22 O8 U'
_chemical_formula_sum            'C10 H22 O8 U'
_chemical_formula_weight         508.31
_chemical_name_common            'uranyl valerate'
_chemical_name_systematic
;
Diaquadioxidobis(n-valerato-κ²O,O')uranium(VI)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.885(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.782(4)
_cell_length_b                   10.802(5)
_cell_length_c                   9.512(5)
_cell_measurement_reflns_used    125
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.49
_cell_volume                     772.8(7)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4876
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    10.531
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.057
_refine_diff_density_min         -2.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0250P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                1187
_reflns_number_total             1187
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fa3320.cif
_cod_data_source_block           I
_cod_original_cell_volume        772.7(7)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2019033
_cod_database_fobs_code          2019033
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
U U1 1.0000 0.0000 1.0000 0.00883(9) Uani d 1
O O1 1.0000 0.2248(5) 1.0000 0.0481(18) Uani d 1
H H1 1.0628 0.2782 0.9704 0.072 Uiso d 1
O O2 1.0290(12) 0.0000 0.8233(10) 0.026(2) Uani d 0.5
O O3 1.1439(13) 0.0000 1.1743(11) 0.042(3) Uani d 0.5
O O4 0.7057(7) -0.1000(6) 0.9038(7) 0.0189(12) Uani d 0.5
O O5 1.2305(8) 0.0995(6) 0.8998(8) 0.0209(13) Uani d 0.5
C C1 0.6208(15) 0.0000 0.8634(12) 0.013(2) Uani d 0.5
C C2 0.4305(8) 0.0000 0.7720(7) 0.0239(13) Uani d 1
H H2 0.3507 0.0095 0.8333 0.029 Uiso d 0.5
H H3 0.4048 -0.0775 0.7215 0.029 Uiso d 0.5
C C3 0.4012(14) 0.1116(9) 0.6565(10) 0.0246(19) Uani d 0.5
H H4 0.4099 0.1916 0.7087 0.029 Uiso calc 0.5
H H5 0.4960 0.1095 0.6043 0.029 Uiso calc 0.5
C C4 0.2191(14) 0.1023(10) 0.5463(11) 0.028(2) Uani d 0.5
H H6 0.2084 0.0203 0.4985 0.033 Uiso calc 0.5
H H7 0.1247 0.1086 0.5986 0.033 Uiso calc 0.5
C C5 0.1909(16) 0.2019(11) 0.4314(12) 0.033(2) Uani d 0.5
H H8 0.0756 0.1920 0.3654 0.050 Uiso d 0.5
H H9 0.1985 0.2817 0.4769 0.050 Uiso d 0.5
H H10 0.2806 0.1952 0.3788 0.050 Uiso d 0.5
C C6 1.2869(14) 0.0000 0.8611(13) 0.014(2) Uani d 0.5
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 U1 O3 . 5_757 180 no
O3 U1 O2 . 5_757 45.4(4) no
O3 U1 O2 5_757 5_757 134.6(4) no
O3 U1 O2 . . 134.5(4) no
O3 U1 O2 5_757 . 45.4(4) no
O2 U1 O2 5_757 . 180 no
O3 U1 O1 . 5_757 90 no
O3 U1 O1 5_757 5_757 90 no
O2 U1 O1 5_757 5_757 90 no
O2 U1 O1 . 5_757 90 no
O3 U1 O1 . . 90 no
O3 U1 O1 5_757 . 90 no
O2 U1 O1 5_757 . 90 no
O2 U1 O1 . . 90 no
O1 U1 O1 5_757 . 180 no
O3 U1 O5 . 5_757 89.2(3) no
O3 U1 O5 5_757 5_757 90.8(3) no
O2 U1 O5 5_757 5_757 49.3(3) no
O2 U1 O5 . 5_757 130.7(3) no
O1 U1 O5 5_757 5_757 64.34(14) no
O1 U1 O5 . 5_757 115.66(14) no
O3 U1 O5 . 6 90.8(3) no
O3 U1 O5 5_757 6 89.2(3) no
O2 U1 O5 5_757 6 130.7(3) no
O2 U1 O5 . 6 49.3(3) no
O1 U1 O5 5_757 6 64.34(14) no
O1 U1 O5 . 6 115.66(14) no
O5 U1 O5 5_757 6 128.7(3) no
O3 U1 O5 . 2_757 89.2(3) no
O3 U1 O5 5_757 2_757 90.8(3) no
O2 U1 O5 5_757 2_757 49.3(3) no
O2 U1 O5 . 2_757 130.7(3) no
O1 U1 O5 5_757 2_757 115.66(14) no
O1 U1 O5 . 2_757 64.34(14) no
O5 U1 O5 5_757 2_757 51.3(3) no
O5 U1 O5 6 2_757 180 no
O3 U1 O5 . . 90.8(3) no
O3 U1 O5 5_757 . 89.2(3) no
O2 U1 O5 5_757 . 130.7(3) no
O2 U1 O5 . . 49.3(3) no
O1 U1 O5 5_757 . 115.66(14) no
O1 U1 O5 . . 64.34(14) no
O5 U1 O5 5_757 . 180 no
O5 U1 O5 6 . 51.3(3) no
O5 U1 O5 2_757 . 128.7(3) no
O3 U1 O4 . . 131.0(3) no
O3 U1 O4 5_757 . 49.0(3) no
O2 U1 O4 5_757 . 91.1(3) no
O2 U1 O4 . . 88.9(3) no
O1 U1 O4 5_757 . 64.24(14) no
O1 U1 O4 . . 115.76(14) no
O5 U1 O4 5_757 . 42.6(2) no
O5 U1 O4 6 . 111.1(2) no
O5 U1 O4 2_757 . 68.9(2) no
O5 U1 O4 . . 137.3(2) no
O3 U1 O4 . 5_757 49.0(3) no
O3 U1 O4 5_757 5_757 131.0(3) no
O2 U1 O4 5_757 5_757 88.9(3) no
O2 U1 O4 . 5_757 91.1(3) no
O1 U1 O4 5_757 5_757 115.76(14) no
O1 U1 O4 . 5_757 64.24(14) no
O5 U1 O4 5_757 5_757 137.4(2) no
O5 U1 O4 6 5_757 68.9(2) no
O5 U1 O4 2_757 5_757 111.1(2) no
O5 U1 O4 . 5_757 42.6(2) no
O4 U1 O4 . 5_757 180 no
U1 O1 H1 . . 132.8 no
O3 O2 U1 5_757 . 67.0(6) no
O2 O3 U1 5_757 . 67.5(6) no
C1 O4 O5 . 5_757 107.1(7) no
C1 O4 U1 . . 95.8(5) no
O5 O4 U1 5_757 . 68.6(3) no
C6 O5 O4 . 5_757 106.4(7) no
C6 O5 U1 . . 94.8(5) no
O4 O5 U1 5_757 . 68.8(3) no
O4 C1 O4 6 . 116.1(11) no
O4 C1 C2 6 . 122.0(5) no
O4 C1 C2 . . 122.0(5) no
O4 C1 U1 6 . 58.4(5) no
O4 C1 U1 . . 58.4(5) no
C2 C1 U1 . . 171.9(7) no
C1 C2 C6 . 1_455 114.8(7) no
C1 C2 C3 . 6 109.8(5) no
C6 C2 C3 1_455 6 111.9(5) no
C1 C2 C3 . . 109.8(5) no
C6 C2 C3 1_455 . 111.9(5) no
C3 C2 C3 6 . 97.2(8) no
C1 C2 H2 . . 110.0 no
C3 C2 H2 6 . 119.6 no
C3 C2 H2 . . 109.5 no
C1 C2 H3 . . 109.6 no
C6 C2 H3 1_455 . 100.6 no
C3 C2 H3 . . 109.7 no
H2 C2 H3 . . 108.2 no
C4 C3 C2 . . 111.2(7) no
C4 C3 H4 . . 109.4 no
C2 C3 H4 . . 109.4 no
C4 C3 H5 . . 109.4 no
C2 C3 H5 . . 109.4 no
H4 C3 H5 . . 108.0 no
C5 C4 C3 . . 112.7(9) no
C5 C4 H6 . . 109.1 no
C3 C4 H6 . . 109.1 no
C5 C4 H7 . . 109.1 no
C3 C4 H7 . . 109.1 no
H6 C4 H7 . . 107.8 no
C4 C5 C5 . 7_556 86.1(9) no
C4 C5 H8 . . 109.5 no
C5 C5 H8 7_556 . 141.6 no
C4 C5 H9 . . 109.5 no
H8 C5 H9 . . 109.5 no
C4 C5 H10 . . 109.5 no
C5 C5 H10 7_556 . 96.9 no
H8 C5 H10 . . 109.5 no
H9 C5 H10 . . 109.5 no
O5 C6 O5 . 6 118.4(10) no
O5 C6 C2 . 1_655 120.8(5) no
O5 C6 C2 6 1_655 120.8(5) no
O5 C6 U1 . . 59.5(5) no
O5 C6 U1 6 . 59.5(5) no
C2 C6 U1 1_655 . 174.9(7) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O3 . 1.746(11) no
U1 O3 5_757 1.746(11) no
U1 O2 5_757 1.752(9) no
U1 O2 . 1.752(9) no
U1 O1 5_757 2.428(5) no
U1 O1 . 2.428(5) no
U1 O5 5_757 2.482(6) no
U1 O5 6 2.482(6) no
U1 O5 2_757 2.482(6) no
U1 O5 . 2.482(6) no
U1 O4 . 2.485(6) no
U1 O4 5_757 2.485(6) no
O1 H1 . 0.8500 no
O2 O3 5_757 1.351(13) no
O3 O2 5_757 1.351(13) no
O4 C1 . 1.273(9) no
O4 O5 5_757 1.806(10) no
O5 C6 . 1.251(8) no
O5 O4 5_757 1.806(10) no
C1 O4 6 1.273(9) no
C1 C2 . 1.512(13) no
C2 C6 1_455 1.567(12) no
C2 C3 6 1.608(10) no
C2 C3 . 1.608(10) no
C2 H2 . 0.9599 no
C2 H3 . 0.9600 no
C3 C4 . 1.534(14) no
C3 H4 . 0.9900 no
C3 H5 . 0.9900 no
C4 C5 . 1.508(14) no
C4 H6 . 0.9900 no
C4 H7 . 0.9900 no
C5 H8 . 0.9600 no
C5 H9 . 0.9599 no
C5 H10 . 0.9601 no
C6 O5 6 1.251(8) no
C6 C2 1_655 1.567(12) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 O4 3_555 0.85 1.93 2.781(7) 180 no
O1 H1 O5 7_757 0.85 2.20 2.808(8) 128 no
