#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:28:59 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185241 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/48/7224898.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_7224898
loop_
_publ_author_name
'Thuéry, Pierre'
'Harrowfield, Jack'
_publ_section_title
;
 Anchoring flexible uranyl dicarboxylate chains through stacking
 interactions of ancillary ligands on chiral U(vi) centres
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              3905
_journal_paper_doi               10.1039/C6CE00603E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C21 H22 N2 O6 U'
_chemical_formula_weight         636.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-03-14 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                74.294(3)
_cell_angle_beta                 69.809(4)
_cell_angle_gamma                75.184(4)
_cell_formula_units_Z            2
_cell_length_a                   8.9926(5)
_cell_length_b                   10.1782(6)
_cell_length_c                   12.3340(8)
_cell_measurement_reflns_used    57063
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.11
_cell_volume                     1003.39(11)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'2 φ and 13 ω scans with 2° steps (653 frames)'
_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  0.0557
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            57063
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         2.113
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.130
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_description       platelet
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.138
_refine_diff_density_min         -1.712
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0309
_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)+(0.0224P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4698
_reflns_number_total             5177
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce00603e1.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7224895--7224902.cif.'
_cod_database_code               7224898
_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           2014-3
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
U1 U 0.23674(2) 0.11863(2) 0.66600(2) 0.02343(5) Uani 1 1 d . .
O1 O 0.0324(3) 0.1996(2) 0.7150(2) 0.0298(5) Uani 1 1 d . .
O2 O 0.4404(3) 0.0382(2) 0.6187(2) 0.0310(6) Uani 1 1 d . .
O3 O 0.2499(3) 0.2042(2) 0.45464(19) 0.0271(5) Uani 1 1 d . .
O4 O 0.1742(3) 0.0045(2) 0.54369(19) 0.0277(5) Uani 1 1 d . .
O5 O 0.1472(3) 0.8955(2) -0.2324(2) 0.0341(6) Uani 1 1 d . .
O6 O 0.2119(3) 1.0014(2) -0.1277(2) 0.0304(5) Uani 1 1 d . .
N1 N 0.3848(3) 0.2247(3) 0.7687(2) 0.0269(6) Uani 1 1 d . .
N2 N 0.2585(4) 0.3877(3) 0.5969(2) 0.0260(6) Uani 1 1 d . .
C1 C 0.2089(4) 0.0963(3) 0.4493(3) 0.0248(7) Uani 1 1 d . .
C2 C 0.1990(4) 0.0693(3) 0.3381(3) 0.0282(7) Uani 1 1 d . .
H2A H 0.0853 0.0669 0.3490 0.034 Uiso 1 1 calc R U
H2B H 0.2622 -0.0240 0.3277 0.034 Uiso 1 1 calc R U
C3 C 0.2582(4) 0.1731(3) 0.2249(3) 0.0278(7) Uani 1 1 d . .
H3A H 0.2729 0.1324 0.1567 0.033 Uiso 1 1 calc R U
H3B H 0.3647 0.1885 0.2204 0.033 Uiso 1 1 calc R U
C4 C 0.1441(4) 0.3137(3) 0.2150(3) 0.0273(7) Uani 1 1 d . .
H4A H 0.0346 0.2983 0.2275 0.033 Uiso 1 1 calc R U
H4B H 0.1386 0.3597 0.2779 0.033 Uiso 1 1 calc R U
C5 C 0.1990(4) 0.4087(3) 0.0953(3) 0.0285(7) Uani 1 1 d . .
H5A H 0.3134 0.4141 0.0785 0.034 Uiso 1 1 calc R U
H5B H 0.1915 0.3678 0.0335 0.034 Uiso 1 1 calc R U
C6 C 0.0995(4) 0.5553(3) 0.0887(3) 0.0271(7) Uani 1 1 d . .
H6A H 0.0983 0.5930 0.1551 0.033 Uiso 1 1 calc R U
H6B H -0.0129 0.5510 0.0976 0.033 Uiso 1 1 calc R U
C7 C 0.1652(4) 0.6535(3) -0.0275(3) 0.0278(7) Uani 1 1 d . .
H7A H 0.2827 0.6453 -0.0437 0.033 Uiso 1 1 calc R U
H7B H 0.1479 0.6259 -0.0926 0.033 Uiso 1 1 calc R U
C8 C 0.0833(4) 0.8046(3) -0.0235(3) 0.0321(8) Uani 1 1 d . .
H8A H -0.0332 0.8132 -0.0115 0.039 Uiso 1 1 calc R U
H8B H 0.0951 0.8298 0.0448 0.039 Uiso 1 1 calc R U
C9 C 0.1512(4) 0.9043(3) -0.1332(3) 0.0285(7) Uani 1 1 d . .
C10 C 0.4635(4) 0.1403(4) 0.8430(3) 0.0326(8) Uani 1 1 d . .
H10 H 0.4507 0.0460 0.8681 0.039 Uiso 1 1 calc R U
C11 C 0.5642(5) 0.1853(4) 0.8854(3) 0.0384(9) Uani 1 1 d . .
H11 H 0.6205 0.1215 0.9363 0.046 Uiso 1 1 calc R U
C12 C 0.5804(5) 0.3209(4) 0.8532(3) 0.0387(9) Uani 1 1 d . .
H12 H 0.6465 0.3527 0.8828 0.046 Uiso 1 1 calc R U
C13 C 0.4986(4) 0.4145(4) 0.7756(3) 0.0305(7) Uani 1 1 d . .
C14 C 0.4050(4) 0.3595(3) 0.7334(3) 0.0267(7) Uani 1 1 d . .
C15 C 0.3302(4) 0.4475(3) 0.6470(3) 0.0256(7) Uani 1 1 d . .
C16 C 0.3392(4) 0.5900(3) 0.6144(3) 0.0285(7) Uani 1 1 d . .
C17 C 0.4305(5) 0.6424(4) 0.6617(3) 0.0349(8) Uani 1 1 d . .
H17 H 0.4362 0.7383 0.6399 0.042 Uiso 1 1 calc R U
C18 C 0.5090(5) 0.5576(4) 0.7373(3) 0.0362(8) Uani 1 1 d . .
H18 H 0.5725 0.5943 0.7655 0.043 Uiso 1 1 calc R U
C19 C 0.2600(5) 0.6740(3) 0.5312(3) 0.0347(8) Uani 1 1 d . .
H19 H 0.2588 0.7712 0.5093 0.042 Uiso 1 1 calc R U
C20 C 0.1862(5) 0.6141(3) 0.4834(3) 0.0346(8) Uani 1 1 d . .
H20 H 0.1321 0.6690 0.4278 0.042 Uiso 1 1 calc R U
C21 C 0.1901(4) 0.4697(3) 0.5168(3) 0.0316(8) Uani 1 1 d . .
H21 H 0.1413 0.4289 0.4800 0.038 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'
N N 0.0061 0.0033 '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
O2 U1 O1 179.34(9) . .
O2 U1 O4 89.28(10) . .
O1 U1 O4 91.31(10) . .
O2 U1 O6 91.97(10) . 1_546
O1 U1 O6 87.49(9) . 1_546
O4 U1 O6 117.97(8) . 1_546
O2 U1 O5 92.69(11) . 1_546
O1 U1 O5 87.28(10) . 1_546
O4 U1 O5 65.37(8) . 1_546
O6 U1 O5 52.61(8) 1_546 1_546
O2 U1 O3 87.70(9) . .
O1 U1 O3 92.89(9) . .
O4 U1 O3 53.04(8) . .
O6 U1 O3 171.01(8) 1_546 .
O5 U1 O3 118.41(8) 1_546 .
O2 U1 N2 101.82(11) . .
O1 U1 N2 78.14(11) . .
O4 U1 N2 120.20(8) . .
O6 U1 N2 120.06(8) 1_546 .
O5 U1 N2 164.29(9) 1_546 .
O3 U1 N2 68.73(8) . .
O2 U1 N1 76.28(10) . .
O1 U1 N1 103.15(10) . .
O4 U1 N1 165.10(9) . .
O6 U1 N1 66.99(9) 1_546 .
O5 U1 N1 118.20(8) 1_546 .
O3 U1 N1 121.53(8) . .
N2 U1 N1 60.71(8) . .
C1 O3 U1 92.65(19) . .
C1 O4 U1 95.9(2) . .
C9 O5 U1 94.0(2) . 1_564
C9 O6 U1 93.98(19) . 1_564
C10 N1 C14 117.8(3) . .
C10 N1 U1 119.8(2) . .
C14 N1 U1 121.6(2) . .
C21 N2 C15 117.5(3) . .
C21 N2 U1 120.6(2) . .
C15 N2 U1 121.8(2) . .
O3 C1 O4 118.3(3) . .
O3 C1 C2 123.9(3) . .
O4 C1 C2 117.8(3) . .
C1 C2 C3 116.3(3) . .
C1 C2 H2A 108.2 . .
C3 C2 H2A 108.2 . .
C1 C2 H2B 108.2 . .
C3 C2 H2B 108.2 . .
H2A C2 H2B 107.4 . .
C2 C3 C4 113.9(3) . .
C2 C3 H3A 108.8 . .
C4 C3 H3A 108.8 . .
C2 C3 H3B 108.8 . .
C4 C3 H3B 108.8 . .
H3A C3 H3B 107.7 . .
C5 C4 C3 112.2(3) . .
C5 C4 H4A 109.2 . .
C3 C4 H4A 109.2 . .
C5 C4 H4B 109.2 . .
C3 C4 H4B 109.2 . .
H4A C4 H4B 107.9 . .
C6 C5 C4 113.1(3) . .
C6 C5 H5A 109.0 . .
C4 C5 H5A 109.0 . .
C6 C5 H5B 109.0 . .
C4 C5 H5B 109.0 . .
H5A C5 H5B 107.8 . .
C5 C6 C7 112.7(3) . .
C5 C6 H6A 109.1 . .
C7 C6 H6A 109.1 . .
C5 C6 H6B 109.1 . .
C7 C6 H6B 109.1 . .
H6A C6 H6B 107.8 . .
C8 C7 C6 111.7(3) . .
C8 C7 H7A 109.3 . .
C6 C7 H7A 109.3 . .
C8 C7 H7B 109.3 . .
C6 C7 H7B 109.3 . .
H7A C7 H7B 107.9 . .
C9 C8 C7 113.1(3) . .
C9 C8 H8A 109.0 . .
C7 C8 H8A 109.0 . .
C9 C8 H8B 109.0 . .
C7 C8 H8B 109.0 . .
H8A C8 H8B 107.8 . .
O5 C9 O6 118.7(3) . .
O5 C9 C8 121.1(3) . .
O6 C9 C8 120.2(3) . .
N1 C10 C11 122.8(3) . .
N1 C10 H10 118.6 . .
C11 C10 H10 118.6 . .
C12 C11 C10 119.5(3) . .
C12 C11 H11 120.2 . .
C10 C11 H11 120.2 . .
C11 C12 C13 119.8(4) . .
C11 C12 H12 120.1 . .
C13 C12 H12 120.1 . .
C14 C13 C12 117.0(3) . .
C14 C13 C18 119.5(3) . .
C12 C13 C18 123.5(3) . .
N1 C14 C13 123.1(3) . .
N1 C14 C15 117.7(3) . .
C13 C14 C15 119.2(3) . .
N2 C15 C16 122.9(3) . .
N2 C15 C14 117.8(3) . .
C16 C15 C14 119.3(3) . .
C19 C16 C15 117.5(3) . .
C19 C16 C17 122.8(3) . .
C15 C16 C17 119.6(3) . .
C18 C17 C16 120.9(3) . .
C18 C17 H17 119.6 . .
C16 C17 H17 119.6 . .
C17 C18 C13 121.3(3) . .
C17 C18 H18 119.4 . .
C13 C18 H18 119.4 . .
C20 C19 C16 119.2(3) . .
C20 C19 H19 120.4 . .
C16 C19 H19 120.4 . .
C19 C20 C21 119.5(3) . .
C19 C20 H20 120.3 . .
C21 C20 H20 120.3 . .
N2 C21 C20 123.4(3) . .
N2 C21 H21 118.3 . .
C20 C21 H21 118.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.766(2) .
U1 O1 1.775(2) .
U1 O4 2.410(2) .
U1 O6 2.460(2) 1_546
U1 O5 2.464(2) 1_546
U1 O3 2.486(2) .
U1 N2 2.676(3) .
U1 N1 2.680(3) .
O3 C1 1.269(4) .
O4 C1 1.279(4) .
O5 C9 1.264(4) .
O5 U1 2.464(2) 1_564
O6 C9 1.272(4) .
O6 U1 2.460(2) 1_564
N1 C10 1.337(4) .
N1 C14 1.361(4) .
N2 C21 1.327(4) .
N2 C15 1.359(4) .
C1 C2 1.505(4) .
C2 C3 1.525(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.535(4) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.526(4) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.528(4) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.531(4) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.532(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.496(5) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C10 C11 1.405(5) .
C10 H10 0.9500 .
C11 C12 1.360(6) .
C11 H11 0.9500 .
C12 C13 1.414(5) .
C12 H12 0.9500 .
C13 C14 1.413(5) .
C13 C18 1.422(5) .
C14 C15 1.435(4) .
C15 C16 1.413(4) .
C16 C19 1.416(5) .
C16 C17 1.422(5) .
C17 C18 1.348(5) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 C20 1.354(5) .
C19 H19 0.9500 .
C20 C21 1.410(5) .
C20 H20 0.9500 .
C21 H21 0.9500 .
