#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:40:15 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230561 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/68/7056856.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_7056856
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_moiety         'C34 H24 I2 N4 O10 U2'
_chemical_formula_sum            'C34 H24 I2 N4 O10 U2'
_chemical_formula_weight         1378.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 100.432(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8501(8)
_cell_length_b                   12.5730(10)
_cell_length_c                   14.8854(11)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.65
_cell_volume                     1813.0(2)
_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    'SIR 92 (Guagliardi, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33526
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.476
_diffrn_reflns_theta_min         2.102
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              Siemens
_exptl_absorpt_coefficient_mu    10.686
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.525
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1252
_exptl_crystal_recrystallization_method 'Slow Evaporation/Photolytic'
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.098
_refine_diff_density_max         2.568
_refine_diff_density_min         -2.913
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3728
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0433
_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)+(0.0564P)²+25.4557P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3320
_reflns_number_total             3728
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj03828c2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7056854--7056861.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7056856
_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   0.125
_shelx_estimated_absorpt_t_max   0.421
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0600(9) 0.4578(7) 0.3418(5) 0.0298(17) Uani 1 1 d . . . . .
H1 H -0.0682 0.5136 0.3815 0.036 Uiso 1 1 calc R U . . .
C2 C -0.1803(9) 0.4129(7) 0.2930(6) 0.0331(18) Uani 1 1 d . . . . .
H2 H -0.2662 0.4409 0.2974 0.040 Uiso 1 1 calc R U . . .
C3 C -0.1701(9) 0.3267(7) 0.2383(6) 0.0358(19) Uani 1 1 d . . . . .
H3 H -0.2488 0.2945 0.2056 0.043 Uiso 1 1 calc R U . . .
C4 C -0.0403(9) 0.2886(6) 0.2328(5) 0.0295(17) Uani 1 1 d . . . . .
H4 H -0.0308 0.2291 0.1973 0.035 Uiso 1 1 calc R U . . .
C5 C 0.0764(8) 0.3394(6) 0.2805(5) 0.0234(15) Uani 1 1 d . . . . .
C6 C 0.2171(8) 0.3012(6) 0.2744(5) 0.0239(15) Uani 1 1 d . . . . .
C7 C 0.2400(10) 0.2225(7) 0.2138(6) 0.0346(19) Uani 1 1 d . . . . .
H7 H 0.1678 0.1908 0.1738 0.042 Uiso 1 1 calc R U . . .
C8 C 0.3813(8) 0.1925(6) 0.2159(5) 0.0246(15) Uani 1 1 d . U . . .
H8 H 0.4009 0.1385 0.1775 0.030 Uiso 1 1 calc R U . . .
C9 C 0.4766(10) 0.2360(8) 0.2670(7) 0.045(2) Uani 1 1 d . . . . .
H9 H 0.5671 0.2155 0.2663 0.054 Uiso 1 1 calc R U . . .
C10 C 0.4503(10) 0.3160(9) 0.3263(7) 0.049(3) Uani 1 1 d . . . . .
H10 H 0.5244 0.3476 0.3646 0.059 Uiso 1 1 calc R U . . .
C11 C 0.1554(10) 0.6926(6) 0.4970(5) 0.0295(17) Uani 1 1 d . . . . .
C12 C 0.0853(10) 0.7845(6) 0.5327(5) 0.0323(19) Uani 1 1 d . . . . .
C13 C 0.1670(13) 0.8611(8) 0.5860(6) 0.046(2) Uani 1 1 d . . . . .
H13 H 0.2627 0.8549 0.5973 0.055 Uiso 1 1 calc R U . . .
C14 C 0.1042(15) 0.9458(8) 0.6218(7) 0.055(3) Uani 1 1 d . . . . .
H14 H 0.1575 0.9962 0.6579 0.066 Uiso 1 1 calc R U . . .
C15 C -0.0408(16) 0.9553(8) 0.6032(7) 0.058(3) Uani 1 1 d . . . . .
H15 H -0.0833 1.0128 0.6259 0.070 Uiso 1 1 calc R U . . .
C16 C -0.1200(13) 0.8785(8) 0.5508(7) 0.051(3) Uani 1 1 d . . . . .
C17 C -0.0573(12) 0.7927(7) 0.5161(6) 0.045(2) Uani 1 1 d . . . . .
H17 H -0.1109 0.7409 0.4818 0.054 Uiso 1 1 calc R U . . .
N1 N 0.0666(7) 0.4249(5) 0.3345(4) 0.0240(13) Uani 1 1 d . . . . .
N2 N 0.3221(7) 0.3494(6) 0.3303(5) 0.0316(15) Uani 1 1 d . . . . .
O1 O 0.3202(12) 0.5870(7) 0.3409(7) 0.098(4) Uani 1 1 d . . . . .
O2 O 0.2419(9) 0.4356(5) 0.5215(4) 0.055(2) Uani 1 1 d . . . . .
O4 O 0.2821(7) 0.6774(6) 0.5236(5) 0.0480(18) Uani 1 1 d . . . . .
O5 O 0.0868(6) 0.6286(4) 0.4401(4) 0.0313(13) Uani 1 1 d . . . . .
I1 I -0.33402(10) 0.89548(7) 0.52178(6) 0.0709(3) Uani 1 1 d . . . . .
U1 U 0.28765(3) 0.51181(3) 0.43370(2) 0.03438(13) Uani 1 1 d . . . . .
O3A O 0.4982(12) 0.4192(12) 0.5047(9) 0.035(5) Uani 0.46(2) 1 d . . P A 1
O3B O 0.5166(14) 0.4837(10) 0.4436(10) 0.044(5) Uani 0.54(2) 1 d . . P A 2
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'
I I -0.4742 1.8119 '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 123.4(8) . .
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C3 C2 C1 119.0(8) . .
C3 C2 H2 120.5 . .
C1 C2 H2 120.5 . .
C2 C3 C4 118.5(8) . .
C2 C3 H3 120.7 . .
C4 C3 H3 120.7 . .
C3 C4 C5 119.8(7) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
N1 C5 C4 121.8(7) . .
N1 C5 C6 117.4(7) . .
C4 C5 C6 120.9(7) . .
N2 C6 C7 121.7(8) . .
N2 C6 C5 116.0(6) . .
C7 C6 C5 122.3(7) . .
C6 C7 C8 116.4(8) . .
C6 C7 H7 121.8 . .
C8 C7 H7 121.8 . .
C9 C8 C7 121.8(7) . .
C9 C8 H8 119.1 . .
C7 C8 H8 119.1 . .
C8 C9 C10 120.4(9) . .
C8 C9 H9 119.8 . .
C10 C9 H9 119.8 . .
N2 C10 C9 122.6(9) . .
N2 C10 H10 118.7 . .
C9 C10 H10 118.7 . .
O4 C11 O5 119.6(7) . .
O4 C11 C12 120.2(8) . .
O5 C11 C12 120.2(8) . .
O4 C11 U1 59.8(4) . .
O5 C11 U1 59.8(4) . .
C12 C11 U1 178.0(5) . .
C17 C12 C13 120.5(9) . .
C17 C12 C11 121.0(8) . .
C13 C12 C11 118.5(9) . .
C14 C13 C12 119.6(11) . .
C14 C13 H13 120.2 . .
C12 C13 H13 120.2 . .
C13 C14 C15 119.8(10) . .
C13 C14 H14 120.1 . .
C15 C14 H14 120.1 . .
C16 C15 C14 119.8(10) . .
C16 C15 H15 120.1 . .
C14 C15 H15 120.1 . .
C15 C16 C17 120.4(12) . .
C15 C16 I1 119.3(8) . .
C17 C16 I1 120.2(9) . .
C12 C17 C16 119.8(10) . .
C12 C17 H17 120.1 . .
C16 C17 H17 120.1 . .
C1 N1 C5 117.4(7) . .
C1 N1 U1 121.0(5) . .
C5 N1 U1 121.4(5) . .
C10 N2 C6 117.1(7) . .
C10 N2 U1 119.6(5) . .
C6 N2 U1 123.1(5) . .
C11 O4 U1 94.3(5) . .
C11 O5 U1 93.9(5) . .
O2 U1 O1 175.5(5) . .
O2 U1 O3B 104.8(5) . .
O1 U1 O3B 79.2(6) . .
O2 U1 O3A 104.5(5) . 3_666
O1 U1 O3A 80.0(6) . 3_666
O2 U1 O3B 74.0(5) . 3_666
O1 U1 O3B 110.5(5) . 3_666
O3B U1 O3B 45.6(6) . 3_666
O2 U1 O3A 74.2(4) . .
O1 U1 O3A 109.6(6) . .
O3A U1 O3A 50.6(7) 3_666 .
O2 U1 O5 88.9(3) . .
O1 U1 O5 88.4(4) . .
O3B U1 O5 152.0(3) . .
O3A U1 O5 116.1(3) 3_666 .
O3B U1 O5 119.5(3) 3_666 .
O3A U1 O5 152.3(3) . .
O2 U1 O4 91.3(3) . .
O1 U1 O4 89.9(3) . .
O3B U1 O4 102.4(3) . .
O3A U1 O4 65.1(3) 3_666 .
O3B U1 O4 70.4(3) 3_666 .
O3A U1 O4 105.4(3) . .
O5 U1 O4 52.2(2) . .
O2 U1 N2 95.2(3) . .
O1 U1 N2 84.0(3) . .
O3B U1 N2 71.5(3) . .
O3A U1 N2 108.6(3) 3_666 .
O3B U1 N2 107.0(3) 3_666 .
O3A U1 N2 72.1(3) . .
O5 U1 N2 132.4(2) . .
O4 U1 N2 172.0(2) . .
O2 U1 N1 83.9(3) . .
O1 U1 N1 91.9(4) . .
O3B U1 N1 133.2(3) . .
O3A U1 N1 168.4(4) 3_666 .
O3B U1 N1 154.5(4) 3_666 .
O3A U1 N1 126.5(3) . .
O5 U1 N1 71.52(19) . .
O4 U1 N1 123.6(2) . .
N2 U1 N1 61.9(2) . .
O2 U1 C11 89.7(2) . .
O1 U1 C11 89.4(3) . .
O3B U1 C11 127.6(3) . .
O3A U1 C11 90.5(4) 3_666 .
O3B U1 C11 94.7(3) 3_666 .
O3A U1 C11 129.5(3) . .
O5 U1 C11 26.3(2) . .
O4 U1 C11 25.9(2) . .
N2 U1 C11 158.2(2) . .
N1 U1 C11 97.7(2) . .
U1 O3A U1 129.4(7) 3_666 .
O3B O3B U1 71.4(8) 3_666 .
O3B O3B U1 63.0(8) 3_666 3_666
U1 O3B U1 134.4(6) . 3_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.337(11) .
C1 C2 1.393(12) .
C1 H1 0.9300 .
C2 C3 1.370(12) .
C2 H2 0.9300 .
C3 C4 1.382(13) .
C3 H3 0.9300 .
C4 C5 1.392(11) .
C4 H4 0.9300 .
C5 N1 1.356(9) .
C5 C6 1.485(11) .
C6 N2 1.348(10) .
C6 C7 1.386(11) .
C7 C8 1.437(12) .
C7 H7 0.9300 .
C8 C9 1.225(13) .
C8 H8 0.9300 .
C9 C10 1.394(12) .
C9 H9 0.9300 .
C10 N2 1.341(12) .
C10 H10 0.9300 .
C11 O4 1.253(11) .
C11 O5 1.270(10) .
C11 C12 1.493(11) .
C11 U1 2.862(8) .
C12 C17 1.385(15) .
C12 C13 1.406(13) .
C13 C14 1.385(14) .
C13 H13 0.9300 .
C14 C15 1.410(19) .
C14 H14 0.9300 .
C15 C16 1.388(17) .
C15 H15 0.9300 .
C16 C17 1.388(13) .
C16 I1 2.085(13) .
C17 H17 0.9300 .
N1 U1 2.636(6) .
N2 U1 2.616(6) .
O1 U1 1.750(9) .
O2 U1 1.744(7) .
O4 U1 2.481(6) .
O5 U1 2.479(6) .
U1 O3B 2.261(13) .
U1 O3A 2.311(12) 3_666
U1 O3B 2.404(13) 3_666
U1 O3A 2.445(13) .
O3A U1 2.311(12) 3_666
O3B O3B 1.81(3) 3_666
O3B U1 2.404(13) 3_666
