#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:40:15 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230561 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/68/7056860.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_7056860
loop_
_publ_author_name
'Ridenour, J. August'
'Cahill, Christopher L.'
_publ_section_title
;
 Synthesis, structural analysis, and supramolecular assembly of a series
 of in situ generated uranyl--peroxide complexes with functionalized
 2,2′-bipyridine and varied carboxylic acid ligands
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1816
_journal_paper_doi               10.1039/C7NJ03828C
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C38 H28 Br4 N4 O14 U2'
_chemical_formula_weight         1560.34
_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_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-06 deposited with the CCDC.
2017-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                95.865(5)
_cell_angle_beta                 105.083(4)
_cell_angle_gamma                116.297(3)
_cell_formula_units_Z            1
_cell_length_a                   10.521(4)
_cell_length_b                   10.766(5)
_cell_length_c                   11.350(4)
_cell_measurement_reflns_used    6789
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.15
_cell_measurement_theta_min      2.27
_cell_volume                     1077.2(8)
_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-2014/7 (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 0.984
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15792
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.277
_diffrn_reflns_theta_min         1.920
_diffrn_source                   Siemens
_exptl_absorpt_coefficient_mu    11.288
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (2015)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.405
_exptl_crystal_description       Plate
_exptl_crystal_F_000             720
_exptl_crystal_recrystallization_method 'Methanol:Acetone - Photolytic'
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.547
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0284P)²+0.7332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5171
_reflns_number_total             5792
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj03828c2.cif
_cod_data_source_block           compound7
_cod_depositor_comments
'Adding full bibliography for 7056854--7056861.cif.'
_cod_database_code               7056860
_shelx_shelxl_version_number     2014/7
_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.
;
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
C1 C 0.7614(4) 0.4067(4) 0.4998(4) 0.0152(7) Uani 1 1 d . .
H1 H 0.8607 0.4381 0.5494 0.018 Uiso 1 1 calc R U
C2 C 0.6593(4) 0.2609(4) 0.4700(4) 0.0158(8) Uani 1 1 d . .
H2 H 0.6886 0.1967 0.4992 0.019 Uiso 1 1 calc R U
C3 C 0.5131(4) 0.2161(4) 0.3955(4) 0.0139(7) Uani 1 1 d . .
C4 C 0.4726(4) 0.3130(4) 0.3508(4) 0.0129(7) Uani 1 1 d . .
H4 H 0.3750 0.2828 0.2977 0.016 Uiso 1 1 calc R U
C5 C 0.5821(4) 0.4569(4) 0.3875(3) 0.0117(7) Uani 1 1 d . .
C6 C 0.5438(4) 0.5652(4) 0.3422(3) 0.0110(7) Uani 1 1 d . .
C7 C 0.3945(4) 0.5286(4) 0.2802(4) 0.0135(7) Uani 1 1 d . .
H7 H 0.3162 0.4372 0.2692 0.016 Uiso 1 1 calc R U
C8 C 0.3651(4) 0.6311(4) 0.2352(4) 0.0144(7) Uani 1 1 d . .
C9 C 0.4811(4) 0.7652(4) 0.2517(4) 0.0181(8) Uani 1 1 d . .
H9 H 0.4628 0.8343 0.2200 0.022 Uiso 1 1 calc R U
C10 C 0.6267(4) 0.7951(4) 0.3171(4) 0.0186(8) Uani 1 1 d . .
H10 H 0.7056 0.8866 0.3297 0.022 Uiso 1 1 calc R U
C11 C 1.1532(4) 0.7569(4) 0.7150(4) 0.0154(7) Uani 1 1 d . .
C12 C 1.2650(4) 0.7305(4) 0.8050(4) 0.0184(8) Uani 1 1 d . .
C13 C 1.2251(5) 0.5892(4) 0.8127(4) 0.0223(9) Uani 1 1 d . .
H13 H 1.1293 0.5145 0.7649 0.027 Uiso 1 1 calc R U
C14 C 1.3307(5) 0.5615(5) 0.8931(4) 0.0273(10) Uani 1 1 d . .
H14 H 1.3044 0.4688 0.9007 0.033 Uiso 1 1 calc R U
C15 C 1.4747(5) 0.6738(5) 0.9612(4) 0.0295(10) Uani 1 1 d . .
H15 H 1.5459 0.6557 1.0127 0.035 Uiso 1 1 calc R U
C16 C 1.5129(5) 0.8132(5) 0.9526(4) 0.0307(10) Uani 1 1 d . .
H16 H 1.6090 0.8880 0.9994 0.037 Uiso 1 1 calc R U
C17 C 1.4084(5) 0.8409(5) 0.8747(4) 0.0252(9) Uani 1 1 d . .
H17 H 1.4348 0.9343 0.8692 0.030 Uiso 1 1 calc R U
C18 C 0.0755(5) 0.1856(5) -0.0111(4) 0.0260(9) Uani 1 1 d . .
C19 C -0.0618(6) 0.1523(6) 0.0239(5) 0.0335(11) Uani 1 1 d . .
H19C H -0.1485 0.1145 -0.0513 0.050 Uiso 1 1 calc R U
H19B H -0.0760 0.0829 0.0730 0.050 Uiso 1 1 calc R U
H19A H -0.0488 0.2382 0.0724 0.050 Uiso 1 1 calc R U
N1 N 0.7261(3) 0.5047(3) 0.4616(3) 0.0117(6) Uani 1 1 d . .
N2 N 0.6600(3) 0.6980(3) 0.3634(3) 0.0133(6) Uani 1 1 d . .
O2 O 0.8545(3) 0.8096(3) 0.6429(3) 0.0220(6) Uani 1 1 d . .
O1 O 1.0015(3) 0.7397(3) 0.4110(3) 0.0205(6) Uani 1 1 d . .
O4 O 1.1855(3) 0.8791(3) 0.6957(3) 0.0172(6) Uani 1 1 d . .
O5 O 1.0230(3) 0.6513(3) 0.6544(3) 0.0208(6) Uani 1 1 d . .
O3 O 1.0740(3) 1.0263(3) 0.5499(3) 0.0325(8) Uani 1 1 d . .
O6 O 0.1986(4) 0.2345(4) 0.0682(3) 0.0445(9) Uani 1 1 d . .
O7 O 0.0533(6) 0.1556(6) -0.1503(5) 0.0860(17) Uani 1 1 d . .
Br1 Br 0.36379(4) 0.02128(4) 0.34837(4) 0.02262(9) Uani 1 1 d . .
Br2 Br 0.16332(4) 0.58566(4) 0.15270(4) 0.02338(9) Uani 1 1 d . .
U1 U 0.93143(2) 0.78234(2) 0.52679(2) 0.01087(4) Uani 1 1 d . .
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'
Br Br -0.2901 2.4595 '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
N1 C1 C2 124.4(3) . .
N1 C1 H1 117.8 . .
C2 C1 H1 117.8 . .
C3 C2 C1 117.0(3) . .
C3 C2 H2 121.5 . .
C1 C2 H2 121.5 . .
C2 C3 C4 120.6(3) . .
C2 C3 Br1 121.2(3) . .
C4 C3 Br1 118.2(3) . .
C3 C4 C5 118.1(3) . .
C3 C4 H4 121.0 . .
C5 C4 H4 121.0 . .
N1 C5 C4 122.8(3) . .
N1 C5 C6 117.1(3) . .
C4 C5 C6 120.1(3) . .
N2 C6 C7 122.5(3) . .
N2 C6 C5 116.9(3) . .
C7 C6 C5 120.6(3) . .
C8 C7 C6 118.5(3) . .
C8 C7 H7 120.8 . .
C6 C7 H7 120.8 . .
C9 C8 C7 120.3(3) . .
C9 C8 Br2 120.2(3) . .
C7 C8 Br2 119.5(3) . .
C8 C9 C10 118.0(3) . .
C8 C9 H9 121.0 . .
C10 C9 H9 121.0 . .
N2 C10 C9 123.5(3) . .
N2 C10 H10 118.3 . .
C9 C10 H10 118.3 . .
O4 C11 O5 119.5(3) . .
O4 C11 C12 122.3(4) . .
O5 C11 C12 118.2(3) . .
O4 C11 U1 61.8(2) . .
O5 C11 U1 57.75(19) . .
C12 C11 U1 174.5(3) . .
C17 C12 C13 119.9(4) . .
C17 C12 C11 121.1(4) . .
C13 C12 C11 118.8(4) . .
C12 C13 C14 119.7(4) . .
C12 C13 H13 120.2 . .
C14 C13 H13 120.2 . .
C15 C14 C13 119.5(4) . .
C15 C14 H14 120.3 . .
C13 C14 H14 120.3 . .
C14 C15 C16 120.3(4) . .
C14 C15 H15 119.8 . .
C16 C15 H15 119.8 . .
C17 C16 C15 120.3(4) . .
C17 C16 H16 119.8 . .
C15 C16 H16 119.8 . .
C12 C17 C16 120.3(4) . .
C12 C17 H17 119.9 . .
C16 C17 H17 119.9 . .
O6 C18 C19 121.5(4) . .
O6 C18 O7 121.4(4) . .
C19 C18 O7 117.1(4) . .
C18 C19 H19C 109.5 . .
C18 C19 H19B 109.5 . .
H19C C19 H19B 109.5 . .
C18 C19 H19A 109.5 . .
H19C C19 H19A 109.5 . .
H19B C19 H19A 109.5 . .
C1 N1 C5 117.1(3) . .
C1 N1 U1 121.7(2) . .
C5 N1 U1 121.2(2) . .
C6 N2 C10 117.2(3) . .
C6 N2 U1 121.5(2) . .
C10 N2 U1 120.1(2) . .
C11 O4 U1 92.0(2) . .
C11 O5 U1 96.0(2) . .
O3 O3 U1 72.0(2) 2_776 .
O3 O3 U1 70.9(2) 2_776 2_776
U1 O3 U1 142.86(13) . 2_776
O1 U1 O2 175.18(13) . .
O1 U1 O3 92.36(13) . .
O2 U1 O3 92.38(14) . .
O1 U1 O3 91.98(13) . 2_776
O2 U1 O3 92.31(13) . 2_776
O3 U1 O3 37.14(13) . 2_776
O1 U1 O5 89.46(12) . .
O2 U1 O5 87.26(12) . .
O3 U1 O5 122.70(10) . .
O3 U1 O5 159.83(10) 2_776 .
O1 U1 O4 90.58(11) . .
O2 U1 O4 90.21(11) . .
O3 U1 O4 70.31(9) . .
O3 U1 O4 107.46(9) 2_776 .
O5 U1 O4 52.40(9) . .
O1 U1 N2 94.46(11) . .
O2 U1 N2 84.97(12) . .
O3 U1 N2 106.89(9) . .
O3 U1 N2 69.90(9) 2_776 .
O5 U1 N2 130.05(9) . .
O4 U1 N2 174.36(9) . .
O1 U1 N1 86.93(11) . .
O2 U1 N1 88.61(12) . .
O3 U1 N1 168.27(9) . .
O3 U1 N1 131.15(10) 2_776 .
O5 U1 N1 69.02(10) . .
O4 U1 N1 121.39(9) . .
N2 U1 N1 61.54(9) . .
O1 U1 C11 89.38(12) . .
O2 U1 C11 89.24(12) . .
O3 U1 C11 96.50(11) . .
O3 U1 C11 133.65(10) 2_776 .
O5 U1 C11 26.22(10) . .
O4 U1 C11 26.19(10) . .
N2 U1 C11 156.08(10) . .
N1 U1 C11 95.20(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.340(5) .
C1 C2 1.393(5) .
C1 H1 0.9300 .
C2 C3 1.377(5) .
C2 H2 0.9300 .
C3 C4 1.384(5) .
C3 Br1 1.889(4) .
C4 C5 1.392(5) .
C4 H4 0.9300 .
C5 N1 1.351(5) .
C5 C6 1.489(5) .
C6 N2 1.351(5) .
C6 C7 1.393(5) .
C7 C8 1.381(5) .
C7 H7 0.9300 .
C8 C9 1.369(5) .
C8 Br2 1.891(4) .
C9 C10 1.387(5) .
C9 H9 0.9300 .
C10 N2 1.353(5) .
C10 H10 0.9300 .
C11 O4 1.263(4) .
C11 O5 1.270(5) .
C11 C12 1.496(5) .
C11 U1 2.859(4) .
C12 C17 1.383(6) .
C12 C13 1.406(6) .
C13 C14 1.407(6) .
C13 H13 0.9300 .
C14 C15 1.389(6) .
C14 H14 0.9300 .
C15 C16 1.392(7) .
C15 H15 0.9300 .
C16 C17 1.385(6) .
C16 H16 0.9300 .
C17 H17 0.9300 .
C18 O6 1.207(5) .
C18 C19 1.497(6) .
C18 O7 1.514(7) .
C19 H19C 0.9600 .
C19 H19B 0.9600 .
C19 H19A 0.9600 .
N1 U1 2.673(3) .
N2 U1 2.650(3) .
O2 U1 1.779(3) .
O1 U1 1.778(3) .
O4 U1 2.522(3) .
O5 U1 2.432(3) .
O3 O3 1.482(5) 2_776
O3 U1 2.320(3) .
O3 U1 2.334(3) 2_776
U1 O3 2.334(3) 2_776
