#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:40:15 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230561 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/68/7056855.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_7056855
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            'C34 H24 Cl2 N4 O10 U2'
_chemical_formula_weight         1195.53
_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                108.014(4)
_cell_angle_beta                 90.369(2)
_cell_angle_gamma                107.510(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3678(18)
_cell_length_b                   9.0091(19)
_cell_length_c                   12.351(3)
_cell_measurement_reflns_used    5480
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.51
_cell_volume                     839.3(3)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Guagliardi, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       omega
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17817
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.201
_diffrn_reflns_theta_min         1.744
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_exptl_absorpt_coefficient_mu    9.861
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.365
_exptl_crystal_description       Plate
_exptl_crystal_F_000             554
_exptl_crystal_recrystallization_method 'Slow Evaporation/Photolytic'
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0163P)²+2.7446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3269
_reflns_number_total             3739
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj03828c2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7056854--7056861.cif.'
_cod_database_code               7056855
_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.
;
_shelx_estimated_absorpt_t_min   0.298
_shelx_estimated_absorpt_t_max   0.633
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 0.1030(6) 0.4385(6) 0.0914(5) 0.0175(11) Uani 1 1 d . .
H1 H 0.1572 0.3826 0.0354 0.021 Uiso 1 1 calc R U
C2 C -0.0674(7) 0.3664(7) 0.0946(5) 0.0199(12) Uani 1 1 d . .
H2 H -0.1254 0.2638 0.0422 0.024 Uiso 1 1 calc R U
C3 C -0.1501(6) 0.4479(7) 0.1761(5) 0.0206(12) Uani 1 1 d . .
H3 H -0.2651 0.4034 0.1788 0.025 Uiso 1 1 calc R U
C4 C -0.0576(7) 0.5970(7) 0.2534(5) 0.0225(12) Uani 1 1 d . .
H4 H -0.1105 0.6549 0.3093 0.027 Uiso 1 1 calc R U
C5 C 0.1130(6) 0.6615(7) 0.2488(4) 0.0156(11) Uani 1 1 d . .
C6 C 0.2139(6) 0.8222(7) 0.3319(5) 0.0179(11) Uani 1 1 d . .
C7 C 0.1553(7) 0.8899(7) 0.4343(4) 0.0209(12) Uani 1 1 d . .
H7 H 0.0546 0.8310 0.4541 0.025 Uiso 1 1 calc R U
C8 C 0.2461(7) 1.0448(7) 0.5070(4) 0.0204(12) Uani 1 1 d . .
H8 H 0.2094 1.0901 0.5768 0.025 Uiso 1 1 calc R U
C9 C 0.3932(7) 1.1310(7) 0.4735(4) 0.0206(12) Uani 1 1 d . .
H9 H 0.4531 1.2387 0.5174 0.025 Uiso 1 1 calc R U
C10 C 0.4490(7) 1.0525(6) 0.3730(4) 0.0197(12) Uani 1 1 d . .
H10 H 0.5507 1.1089 0.3528 0.024 Uiso 1 1 calc R U
C11 C 0.8309(7) 0.9745(7) 0.1852(5) 0.0188(11) Uani 1 1 d . .
C12 C 1.0030(6) 1.0977(6) 0.2195(4) 0.0164(11) Uani 1 1 d . .
C13 C 1.0336(7) 1.2306(7) 0.3193(5) 0.0210(12) Uani 1 1 d . .
H13 H 0.9469 1.2445 0.3640 0.025 Uiso 1 1 calc R U
C14 C 1.1919(7) 1.3409(7) 0.3514(5) 0.0227(12) Uani 1 1 d . .
C15 C 1.3247(7) 1.3271(7) 0.2840(5) 0.0264(13) Uani 1 1 d . .
H15 H 1.4315 1.4045 0.3063 0.032 Uiso 1 1 calc R U
C16 C 1.2924(7) 1.1960(7) 0.1841(5) 0.0254(13) Uani 1 1 d . .
H16 H 1.3784 1.1849 0.1381 0.031 Uiso 1 1 calc R U
C17 C 1.1327(7) 1.0796(7) 0.1511(5) 0.0208(12) Uani 1 1 d . .
H17 H 1.1124 0.9905 0.0841 0.025 Uiso 1 1 calc R U
N1 N 0.1928(5) 0.5844(5) 0.1651(4) 0.0155(9) Uani 1 1 d . .
N2 N 0.3650(5) 0.8997(5) 0.3028(4) 0.0158(9) Uani 1 1 d . .
O1 O 0.5757(4) 0.6586(4) 0.2447(3) 0.0208(8) Uani 1 1 d . .
O2 O 0.4355(5) 0.8072(5) 0.0418(3) 0.0279(10) Uani 1 1 d . .
O4 O 0.8048(5) 0.8416(5) 0.1028(3) 0.0245(9) Uani 1 1 d . .
O5 O 0.7098(4) 1.0013(4) 0.2409(3) 0.0225(9) Uani 1 1 d . .
Cl1 Cl 1.23336(19) 1.50439(19) 0.48103(13) 0.0342(4) Uani 1 1 d . .
U1 U 0.50732(2) 0.72737(3) 0.13830(2) 0.01537(7) Uani 1 1 d . .
O3 O 0.4126(4) 0.4609(5) 0.0083(4) 0.0371(12) 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'
Cl Cl 0.1484 0.1585 '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 123.0(5) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C3 C2 C1 119.3(5) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
C4 C3 C2 118.0(5) . .
C4 C3 H3 121.0 . .
C2 C3 H3 121.0 . .
C3 C4 C5 120.6(5) . .
C3 C4 H4 119.7 . .
C5 C4 H4 119.7 . .
N1 C5 C4 121.3(5) . .
N1 C5 C6 117.6(4) . .
C4 C5 C6 121.0(5) . .
N2 C6 C7 121.9(5) . .
N2 C6 C5 117.0(4) . .
C7 C6 C5 121.1(5) . .
C8 C7 C6 120.1(5) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
C7 C8 C9 118.4(5) . .
C7 C8 H8 120.8 . .
C9 C8 H8 120.8 . .
C8 C9 C10 118.3(5) . .
C8 C9 H9 120.8 . .
C10 C9 H9 120.8 . .
N2 C10 C9 124.0(5) . .
N2 C10 H10 118.0 . .
C9 C10 H10 118.0 . .
O4 C11 O5 119.5(5) . .
O4 C11 C12 120.8(5) . .
O5 C11 C12 119.7(5) . .
O4 C11 U1 60.4(3) . .
O5 C11 U1 59.4(3) . .
C12 C11 U1 174.2(4) . .
C13 C12 C17 120.1(5) . .
C13 C12 C11 119.7(5) . .
C17 C12 C11 120.2(5) . .
C14 C13 C12 119.5(5) . .
C14 C13 H13 120.3 . .
C12 C13 H13 120.3 . .
C13 C14 C15 121.8(5) . .
C13 C14 Cl1 119.6(4) . .
C15 C14 Cl1 118.6(4) . .
C16 C15 C14 118.3(5) . .
C16 C15 H15 120.9 . .
C14 C15 H15 120.9 . .
C15 C16 C17 120.8(5) . .
C15 C16 H16 119.6 . .
C17 C16 H16 119.6 . .
C16 C17 C12 119.5(5) . .
C16 C17 H17 120.3 . .
C12 C17 H17 120.3 . .
C1 N1 C5 117.7(4) . .
C1 N1 U1 120.8(3) . .
C5 N1 U1 121.3(3) . .
C10 N2 C6 116.9(4) . .
C10 N2 U1 122.6(3) . .
C6 N2 U1 119.3(3) . .
C11 O4 U1 93.4(3) . .
C11 O5 U1 94.4(3) . .
O2 U1 O1 175.47(18) . .
O2 U1 O3 91.95(18) . .
O1 U1 O3 91.79(17) . .
O2 U1 O3 91.97(18) . 2_665
O1 U1 O3 92.56(17) . 2_665
O3 U1 O3 36.75(16) . 2_665
O2 U1 O5 90.40(16) . .
O1 U1 O5 87.14(15) . .
O3 U1 O5 157.25(12) . .
O3 U1 O5 120.56(12) 2_665 .
O2 U1 O4 91.20(15) . .
O1 U1 O4 90.30(14) . .
O3 U1 O4 104.86(12) . .
O3 U1 O4 68.12(12) 2_665 .
O5 U1 O4 52.45(12) . .
O2 U1 N1 89.61(15) . .
O1 U1 N1 89.21(14) . .
O3 U1 N1 70.77(12) . .
O3 U1 N1 107.51(13) 2_665 .
O5 U1 N1 131.89(12) . .
O4 U1 N1 175.58(13) . .
O2 U1 N2 89.16(16) . .
O1 U1 N2 86.42(15) . .
O3 U1 N2 133.13(13) . .
O3 U1 N2 169.85(12) 2_665 .
O5 U1 N2 69.51(12) . .
O4 U1 N2 121.96(12) . .
N1 U1 N2 62.39(13) . .
O2 U1 C11 92.12(16) . .
O1 U1 C11 87.35(16) . .
O3 U1 C11 130.99(13) . .
O3 U1 C11 94.30(14) 2_665 .
O5 U1 C11 26.26(13) . .
O4 U1 C11 26.24(13) . .
N1 U1 C11 158.04(14) . .
N2 U1 C11 95.74(14) . .
O3 O3 U1 71.5(3) 2_665 .
O3 O3 U1 71.8(3) 2_665 2_665
U1 O3 U1 143.25(16) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.334(7) .
C1 C2 1.384(7) .
C1 H1 0.9300 .
C2 C3 1.374(7) .
C2 H2 0.9300 .
C3 C4 1.373(8) .
C3 H3 0.9300 .
C4 C5 1.379(7) .
C4 H4 0.9300 .
C5 N1 1.357(6) .
C5 C6 1.482(7) .
C6 N2 1.358(6) .
C6 C7 1.387(7) .
C7 C8 1.381(8) .
C7 H7 0.9300 .
C8 C9 1.386(7) .
C8 H8 0.9300 .
C9 C10 1.387(7) .
C9 H9 0.9300 .
C10 N2 1.346(7) .
C10 H10 0.9300 .
C11 O4 1.266(6) .
C11 O5 1.269(6) .
C11 C12 1.492(7) .
C11 U1 2.859(5) .
C12 C13 1.384(7) .
C12 C17 1.397(7) .
C13 C14 1.363(8) .
C13 H13 0.9300 .
C14 C15 1.405(8) .
C14 Cl1 1.755(6) .
C15 C16 1.375(8) .
C15 H15 0.9300 .
C16 C17 1.392(8) .
C16 H16 0.9300 .
C17 H17 0.9300 .
N1 U1 2.632(4) .
N2 U1 2.674(4) .
O1 U1 1.773(4) .
O2 U1 1.755(4) .
O4 U1 2.490(4) .
O5 U1 2.467(4) .
U1 O3 2.329(4) .
U1 O3 2.325(4) 2_665
O3 O3 1.467(7) 2_665
O3 U1 2.325(4) 2_665
