#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:32:11 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232884 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/83/4348349.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_4348349
loop_
_publ_author_name
'Carter, Korey P.'
'Cahill, Christopher L.'
_publ_section_title
;
 Combining coordination and supramolecular chemistry to explore uranyl
 assembly in the solid state
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              141
_journal_paper_doi               10.1039/C4QI00183D
_journal_volume                  2
_journal_year                    2015
_chemical_formula_sum            'C26 H16 Br4 N2 O7 U'
_chemical_formula_weight         1026.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.259(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2282(8)
_cell_length_b                   6.5817(4)
_cell_length_c                   16.1780(9)
_cell_measurement_reflns_used    18307
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.151
_cell_measurement_theta_min      5.029
_cell_volume                     1370.15(15)
_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 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18291
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.603
_diffrn_reflns_theta_min         1.392
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    11.805
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5319
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.487
_exptl_crystal_description       Plate
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.971
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3465
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0279
_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)+(0.0192P)²+1.0033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2976
_reflns_number_total             3465
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4qi00183d2.cif
_cod_data_source_block           Compound_3
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4348349
_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           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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 0.74127(2) 0.7500 0.67332(2) 0.00778(6) Uani 1 2 d S T P
Br3 Br 0.65818(5) 0.7500 1.03232(4) 0.01887(15) Uani 1 2 d S T P
Br2 Br 0.96884(5) 0.7500 1.20907(4) 0.01941(15) Uani 1 2 d S T P
Br1 Br 1.29063(5) 0.7500 1.09320(4) 0.01886(15) Uani 1 2 d S T P
Br4 Br 0.22333(5) 0.7500 0.81702(5) 0.02428(17) Uani 1 2 d S T P
O3 O 0.7949(3) 0.7500 0.8380(3) 0.0118(9) Uani 1 2 d S T P
O1 O 0.7429(2) 0.4807(4) 0.67093(19) 0.0111(6) Uani 1 1 d . . .
O4 O 0.5849(3) 0.7500 0.6748(3) 0.0129(9) Uani 1 2 d S T P
O5 O 0.4134(3) 0.7500 0.5907(3) 0.0151(9) Uani 1 2 d S T P
O2 O 0.9193(3) 0.7500 0.7917(3) 0.0123(9) Uani 1 2 d S T P
OW1 O 0.8025(3) 0.2500 0.5233(3) 0.0214(11) Uani 1 2 d S T P
N2 N 0.6413(4) 0.7500 0.5004(3) 0.0098(10) Uani 1 2 d S T P
C2 C 1.0194(5) 0.7500 0.5778(4) 0.0142(13) Uani 1 2 d S T P
H2 H 1.0915 0.7500 0.6092 0.017 Uiso 1 2 calc R U P
N1 N 0.8536(4) 0.7500 0.5848(3) 0.0122(11) Uani 1 2 d S T P
C19 C 0.9372(4) 0.7500 1.0237(4) 0.0092(12) Uani 1 2 d S T P
H19 H 0.8669 0.7500 1.0106 0.011 Uiso 1 2 calc R U P
C11 C 0.6951(4) 0.7500 0.4470(4) 0.0090(12) Uani 1 2 d S T P
C8 C 0.5349(5) 0.7500 0.3105(4) 0.0129(13) Uani 1 2 d S T P
H8 H 0.4989 0.7500 0.2471 0.016 Uiso 1 2 calc R U P
C3 C 0.9728(5) 0.7500 0.4848(4) 0.0145(13) Uani 1 2 d S T P
H3 H 1.0126 0.7500 0.4517 0.017 Uiso 1 2 calc R U P
C4 C 0.8637(5) 0.7500 0.4394(4) 0.0128(13) Uani 1 2 d S T P
C20 C 0.4894(4) 0.7500 0.6650(4) 0.0107(12) Uani 1 2 d S T P
C22 C 0.5600(5) 0.7500 0.8378(4) 0.0121(13) Uani 1 2 d S T P
H22 H 0.6275 0.7500 0.8426 0.015 Uiso 1 2 calc R U P
C7 C 0.6440(4) 0.7500 0.3514(4) 0.0103(12) Uani 1 2 d S T P
C6 C 0.7033(5) 0.7500 0.2993(4) 0.0165(14) Uani 1 2 d S T P
H6 H 0.6697 0.7500 0.2358 0.020 Uiso 1 2 calc R U P
C5 C 0.8089(5) 0.7500 0.3422(5) 0.0191(14) Uani 1 2 d S T P
H5 H 0.8464 0.7500 0.3071 0.023 Uiso 1 2 calc R U P
C26 C 0.3747(5) 0.7500 0.7463(4) 0.0152(13) Uani 1 2 d S T P
H26 H 0.3177 0.7500 0.6895 0.018 Uiso 1 2 calc R U P
C12 C 0.8061(4) 0.7500 0.4915(4) 0.0092(12) Uani 1 2 d S T P
C13 C 0.8909(5) 0.7500 0.8562(4) 0.0095(12) Uani 1 2 d S T P
C23 C 0.5428(5) 0.7500 0.9148(4) 0.0121(13) Uani 1 2 d S T P
C16 C 1.1470(4) 0.7500 1.0639(4) 0.0119(13) Uani 1 2 d S T P
C9 C 0.4813(5) 0.7500 0.3631(4) 0.0115(13) Uani 1 2 d S T P
H9 H 0.4090 0.7500 0.3365 0.014 Uiso 1 2 calc R U P
C15 C 1.0748(5) 0.7500 0.9732(4) 0.0096(12) Uani 1 2 d S T P
H15 H 1.0963 0.7500 0.9264 0.012 Uiso 1 2 calc R U P
C25 C 0.3606(5) 0.7500 0.8248(4) 0.0154(14) Uani 1 2 d S T P
C14 C 0.9695(4) 0.7500 0.9536(4) 0.0084(12) Uani 1 2 d S TU P
C21 C 0.4755(5) 0.7500 0.7519(4) 0.0107(12) Uani 1 2 d S T P
C24 C 0.4429(5) 0.7500 0.9109(5) 0.0166(14) Uani 1 2 d S T P
H24 H 0.4321 0.7500 0.9637 0.020 Uiso 1 2 calc R U P
C10 C 0.5379(5) 0.7500 0.4580(4) 0.0131(13) Uani 1 2 d S T P
H10 H 0.5012 0.7500 0.4937 0.016 Uiso 1 2 calc R U P
C17 C 1.1170(4) 0.7500 1.1350(4) 0.0097(12) Uani 1 2 d S T P
H17 H 1.1660 0.7500 1.1956 0.012 Uiso 1 2 calc R U P
C18 C 1.0112(5) 0.7500 1.1125(4) 0.0105(12) Uani 1 2 d S TU P
C1 C 0.9577(4) 0.7500 0.6254(4) 0.0140(13) Uani 1 2 d S T P
H1 H 0.9906 0.7500 0.6889 0.017 Uiso 1 2 calc R U P
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
O1 U1 O1 176.57(18) 4_575
O1 U1 O4 91.30(9) 4_575
O1 U1 O4 91.30(9) .
O1 U1 O3 91.32(9) 4_575
O1 U1 O3 91.32(9) .
O4 U1 O3 80.64(14) .
O1 U1 O2 89.90(9) 4_575
O1 U1 O2 89.90(9) .
O4 U1 O2 134.18(14) .
O3 U1 O2 53.55(13) .
O1 U1 N2 88.99(9) 4_575
O1 U1 N2 88.99(9) .
O4 U1 N2 85.39(15) .
O3 U1 N2 166.02(14) .
O2 U1 N2 140.43(14) .
O1 U1 N1 88.31(9) 4_575
O1 U1 N1 88.31(9) .
O4 U1 N1 150.19(16) .
O3 U1 N1 129.18(15) .
O2 U1 N1 75.63(15) .
N2 U1 N1 64.80(16) .
O1 U1 C13 90.68(9) 4_575
O1 U1 C13 90.68(9) .
O4 U1 C13 107.37(16) .
O3 U1 C13 26.73(15) .
O2 U1 C13 26.82(15) .
N2 U1 C13 167.25(16) .
N1 U1 C13 102.45(17) .
C13 O3 U1 93.4(3) .
C20 O4 U1 173.1(4) .
C13 O2 U1 93.2(3) .
C10 N2 C11 117.6(5) .
C10 N2 U1 123.0(4) .
C11 N2 U1 119.4(4) .
C3 C2 C1 119.1(6) .
C3 C2 H2 120.5 .
C1 C2 H2 120.5 .
C1 N1 C12 117.6(5) .
C1 N1 U1 123.3(4) .
C12 N1 U1 119.1(4) .
C18 C19 C14 118.7(5) .
C18 C19 H19 120.7 .
C14 C19 H19 120.7 .
N2 C11 C7 121.8(5) .
N2 C11 C12 118.3(5) .
C7 C11 C12 119.8(5) .
C9 C8 C7 120.4(6) .
C9 C8 H8 119.8 .
C7 C8 H8 119.8 .
C2 C3 C4 119.1(6) .
C2 C3 H3 120.4 .
C4 C3 H3 120.4 .
C12 C4 C3 118.9(6) .
C12 C4 C5 118.5(5) .
C3 C4 C5 122.6(6) .
O5 C20 O4 123.9(6) .
O5 C20 C21 120.4(5) .
O4 C20 C21 115.8(5) .
C23 C22 C21 119.5(6) .
C23 C22 H22 120.3 .
C21 C22 H22 120.3 .
C11 C7 C8 118.0(5) .
C11 C7 C6 119.6(5) .
C8 C7 C6 122.4(6) .
C5 C6 C7 120.2(6) .
C5 C6 H6 119.9 .
C7 C6 H6 119.9 .
C6 C5 C4 121.8(6) .
C6 C5 H5 119.1 .
C4 C5 H5 119.1 .
C25 C26 C21 119.5(6) .
C25 C26 H26 120.2 .
C21 C26 H26 120.2 .
N1 C12 C4 121.6(5) .
N1 C12 C11 118.4(5) .
C4 C12 C11 120.0(5) .
O3 C13 O2 119.8(5) .
O3 C13 C14 119.6(5) .
O2 C13 C14 120.6(5) .
O3 C13 U1 59.9(3) .
O2 C13 U1 59.9(3) .
C14 C13 U1 179.5(4) .
C22 C23 C24 122.2(6) .
C22 C23 Br3 119.6(5) .
C24 C23 Br3 118.1(5) .
C17 C16 C15 121.7(6) .
C17 C16 Br1 118.3(4) .
C15 C16 Br1 120.0(5) .
C8 C9 C10 118.2(6) .
C8 C9 H9 120.9 .
C10 C9 H9 120.9 .
C16 C15 C14 118.8(6) .
C16 C15 H15 120.6 .
C14 C15 H15 120.6 .
C26 C25 C24 122.5(6) .
C26 C25 Br4 119.5(5) .
C24 C25 Br4 118.0(5) .
C19 C14 C15 120.7(5) .
C19 C14 C13 119.9(5) .
C15 C14 C13 119.3(5) .
C22 C21 C26 119.3(6) .
C22 C21 C20 122.0(5) .
C26 C21 C20 118.7(6) .
C25 C24 C23 117.0(6) .
C25 C24 H24 121.5 .
C23 C24 H24 121.5 .
N2 C10 C9 124.0(6) .
N2 C10 H10 118.0 .
C9 C10 H10 118.0 .
C16 C17 C18 117.7(5) .
C16 C17 H17 121.1 .
C18 C17 H17 121.1 .
C19 C18 C17 122.4(5) .
C19 C18 Br2 119.3(4) .
C17 C18 Br2 118.2(4) .
N1 C1 C2 123.7(6) .
N1 C1 H1 118.1 .
C2 C1 H1 118.1 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.773(3) 4_575
U1 O1 1.773(3) .
U1 O4 2.235(4) .
U1 O3 2.438(4) .
U1 O2 2.438(4) .
U1 N2 2.540(5) .
U1 N1 2.561(5) .
U1 C13 2.813(6) .
Br3 C23 1.909(6) .
Br2 C18 1.899(6) .
Br1 C16 1.890(6) .
Br4 C25 1.903(6) .
O3 C13 1.267(7) .
O4 C20 1.299(7) .
O5 C20 1.227(7) .
O2 C13 1.271(7) .
N2 C10 1.332(7) .
N2 C11 1.378(7) .
C2 C3 1.361(9) .
C2 C1 1.393(8) .
C2 H2 0.9300 .
N1 C1 1.340(7) .
N1 C12 1.366(7) .
C19 C18 1.371(8) .
C19 C14 1.395(8) .
C19 H19 0.9300 .
C11 C7 1.400(8) .
C11 C12 1.430(8) .
C8 C9 1.364(8) .
C8 C7 1.404(8) .
C8 H8 0.9300 .
C3 C4 1.406(8) .
C3 H3 0.9300 .
C4 C12 1.404(8) .
C4 C5 1.426(9) .
C20 C21 1.501(8) .
C22 C23 1.370(8) .
C22 C21 1.397(8) .
C22 H22 0.9300 .
C7 C6 1.424(8) .
C6 C5 1.360(9) .
C6 H6 0.9300 .
C5 H5 0.9300 .
C26 C25 1.369(8) .
C26 C21 1.397(8) .
C26 H26 0.9300 .
C13 C14 1.493(8) .
C23 C24 1.395(8) .
C16 C17 1.388(8) .
C16 C15 1.386(8) .
C9 C10 1.396(8) .
C9 H9 0.9300 .
C15 C14 1.392(8) .
C15 H15 0.9300 .
C25 C24 1.386(9) .
C24 H24 0.9300 .
C10 H10 0.9300 .
C17 C18 1.389(8) .
C17 H17 0.9300 .
C1 H1 0.9300 .
