#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:35:44 +0100 (dom 17 de nov de 2019) $
#$Revision: 229137 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/09/7230956.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_7230956
loop_
_publ_author_name
'Carter, Korey P.'
'Kalaj, Mark'
'Kerridge, Andrew'
'Cahill, Christopher L.'
_publ_section_title
;
 Probing hydrogen and halogen-oxo interactions in uranyl coordination
 polymers: a combined crystallographic and computational study
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              4916
_journal_paper_doi               10.1039/C8CE00682B
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C14 H10 O6 U'
_chemical_formula_weight         512.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-04-23 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.791(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.632(6)
_cell_length_b                   17.468(9)
_cell_length_c                   5.313(5)
_cell_measurement_reflns_used    9180
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.360
_cell_measurement_theta_min      4.664
_cell_volume                     704.7(9)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8871
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         2.332
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    11.540
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4227
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.414
_exptl_crystal_description       Plate
_exptl_crystal_F_000             468
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0141
_refine_ls_R_factor_gt           0.0141
_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)+(0.0142P)²+0.6711P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0322
_refine_ls_wR_factor_ref         0.0322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                846
_reflns_number_total             846
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00682b2.cif
_cod_data_source_block           Compound_1
_cod_depositor_comments
'Adding full bibliography for 7230956--7230959.cif.'
_cod_database_code               7230956
_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.
;
_shelxl_version_number           2014-1
_shelx_res_file
;
TITL C2onM_twin in C2/m
CELL  0.71073   7.6320  17.4680   5.3130   90.000   95.791   90.000
ZERR     2.00   0.0060   0.0090   0.0050    0.000    0.007    0.000
LATT   7
SYMM  - X,   Y, - Z
SFAC  C    H    O    U
UNIT  28   20   12   2
MERG   2
FMAP   2
PLAN   5
ACTA  51
BOND  $H
L.S.  24
WGHT    0.014200    0.671100
FVAR       0.12859
U1    4    0.000000    0.000000    0.000000    10.25000    0.04753    0.01522 =
         0.01908    0.00000   -0.00124    0.00000
O1    3    0.226419    0.000000    0.092175    10.50000    0.05600    0.03171 =
         0.05405    0.00000   -0.00342    0.00000
O2    3    0.041815    0.092546   -0.295295    11.00000    0.07758    0.02631 =
         0.03512    0.01020    0.00571   -0.00212
C1    1    0.000000    0.127372   -0.500000    10.50000    0.04496    0.02095 =
         0.02502    0.00000    0.01219    0.00000
C2    1    0.000000    0.211663   -0.500000    10.50000    0.03283    0.01888 =
         0.03130    0.00000    0.01071    0.00000
C3    1    0.078036    0.251427   -0.291993    11.00000    0.04803    0.02979 =
         0.04015   -0.00769    0.00677   -0.00441
AFIX  43
H3    2    0.129935    0.224951   -0.151951    11.00000   -1.20000
AFIX   0
C5    1    0.000000    0.369724   -0.500000    10.50000    0.07390    0.01729 =
         0.11206    0.00000    0.03778    0.00000
AFIX  43
H5    2    0.000001    0.422964   -0.500002    10.50000   -1.20000
AFIX   0
C4    1    0.078298    0.330787   -0.293849    11.00000    0.06587    0.03472 =
         0.07272   -0.02228    0.01902   -0.01538
AFIX  43
H4    2    0.131475    0.357665   -0.155546    11.00000   -1.20000
AFIX   0
HKLF    4

REM  C2onM_twin in C2/m
REM R1 =  0.0141 for     846 Fo > 4sig(Fo)  and  0.0141 for all     846 data
REM     53 parameters refined using      0 restraints

END

WGHT      0.0141      0.6696

REM Highest difference peak  0.647,  deepest hole -0.712,  1-sigma level  0.092
Q1    1   0.0877  0.0000  0.1071  10.50000  0.05    0.65
Q2    1   0.1951  0.0000  0.1909  10.50000  0.05    0.60
Q3    1   0.1694  0.0258  0.0062  11.00000  0.05    0.58
Q4    1   0.1844  0.0000 -0.0223  10.50000  0.05    0.54
Q5    1   0.0000  0.5000 -0.5000  10.25000  0.05    0.54
;
_shelx_res_checksum              53662
loop_
_space_group_symop_operation_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_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
U1 U 0.0000 0.0000 0.0000 0.02759(7) Uani 1 4 d S T P
O1 O 0.2264(4) 0.0000 0.0922(7) 0.0479(8) Uani 1 2 d S T P
O2 O 0.0418(3) 0.09255(12) -0.2953(4) 0.0463(5) Uani 1 1 d . . .
C1 C 0.0000 0.1274(2) -0.5000 0.0297(8) Uani 1 2 d S T P
C2 C 0.0000 0.2117(2) -0.5000 0.0272(7) Uani 1 2 d S T P
C3 C 0.0780(4) 0.25143(17) -0.2920(6) 0.0392(7) Uani 1 1 d . . .
H3 H 0.1299 0.2250 -0.1520 0.047 Uiso 1 1 calc R U .
C5 C 0.0000 0.3697(3) -0.5000 0.0658(17) Uani 1 2 d S T P
H5 H 0.0000 0.4230 -0.5000 0.079 Uiso 1 2 calc R U P
C4 C 0.0783(5) 0.3308(2) -0.2938(8) 0.0570(10) Uani 1 1 d . . .
H4 H 0.1315 0.3577 -0.1555 0.068 Uiso 1 1 calc R U .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.04753(13) 0.01522(10) 0.01908(10) 0.000 -0.00124(8) 0.000
O1 0.0560(19) 0.0317(16) 0.054(2) 0.000 -0.0034(15) 0.000
O2 0.0776(15) 0.0263(10) 0.0351(11) 0.0102(9) 0.0057(10) -0.0021(10)
C1 0.045(2) 0.0209(17) 0.0250(18) 0.000 0.0122(15) 0.000
C2 0.0328(18) 0.0189(17) 0.0313(19) 0.000 0.0107(15) 0.000
C3 0.0480(17) 0.0298(15) 0.0401(16) -0.0077(12) 0.0068(13) -0.0044(12)
C5 0.074(4) 0.017(2) 0.112(5) 0.000 0.038(4) 0.000
C4 0.066(2) 0.0347(18) 0.073(3) -0.0223(18) 0.0190(19) -0.0154(16)
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 U1 O1 180.0 . 5
O1 U1 O2 89.42(11) . 6
O1 U1 O2 90.58(11) 5 6
O1 U1 O2 90.58(11) . 2
O1 U1 O2 89.42(11) 5 2
O2 U1 O2 180.00(14) 6 2
O1 U1 O2 90.58(11) . 5
O1 U1 O2 89.42(11) 5 5
O2 U1 O2 90.55(13) 6 5
O2 U1 O2 89.45(13) 2 5
O1 U1 O2 89.42(11) . .
O1 U1 O2 90.58(11) 5 .
O2 U1 O2 89.45(13) 6 .
O2 U1 O2 90.55(13) 2 .
O2 U1 O2 180.0 5 .
C1 O2 U1 152.81(19) . .
O2 C1 O2 122.2(4) . 2_554
O2 C1 C2 118.90(18) . .
O2 C1 C2 118.90(18) 2_554 .
C3 C2 C3 119.9(4) 2_554 .
C3 C2 C1 120.03(19) 2_554 .
C3 C2 C1 120.04(19) . .
C2 C3 C4 119.7(3) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C4 C5 C4 120.6(4) . 2_554
C4 C5 H5 119.7 . .
C4 C5 H5 119.7 2_554 .
C5 C4 C3 120.0(4) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.748(4) .
U1 O1 1.748(4) 5
U1 O2 2.297(2) 6
U1 O2 2.297(2) 2
U1 O2 2.297(2) 5
U1 O2 2.297(2) .
O2 C1 1.259(3) .
C1 O2 1.259(3) 2_554
C1 C2 1.472(5) .
C2 C3 1.388(4) 2_554
C2 C3 1.388(4) .
C3 C4 1.386(5) .
C3 H3 0.9300 .
C5 C4 1.374(5) .
C5 C4 1.374(5) 2_554
C5 H5 0.9300 .
C4 H4 0.9300 .
