#------------------------------------------------------------------------------
#$Date: 2020-02-04 22:42:09 +0200 (Tue, 04 Feb 2020) $
#$Revision: 247750 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/31/7703102.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_7703102
loop_
_publ_author_name
'Thuéry, Pierre'
'Atoini, Youssef'
'Harrowfield, Jack'
_publ_section_title
;
 Zero-, mono- and diperiodic uranyl ion complexes with the diphenate
 dianion: influences of transition metal ion coordination and differential
 UVI chelation.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              817
_journal_page_last               828
_journal_paper_doi               10.1039/c9dt04126e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C26 H16 N2 O6 U'
_chemical_formula_weight         690.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.404(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9607(4)
_cell_length_b                   11.8944(9)
_cell_length_c                   18.5400(16)
_cell_measurement_reflns_used    116607
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.80
_cell_volume                     2182.8(3)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'2 φ and 12 ω scans with 2° steps (782 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  0.0346
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            116607
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.797
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.484
_exptl_absorpt_correction_T_max  0.378
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.893
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0314
_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)+(0.0376P)²+0.0773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3322
_reflns_number_total             4137
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04126e1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7703096--7703104.cif.'
_cod_original_cell_volume        2182.9(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7703102
_shelx_shelxl_version_number     2017/1
_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
U1 U 0.30206(2) 0.95154(2) 0.32250(2) 0.02623(8) Uani 1 1 d . .
O1 O 0.4164(3) 0.8395(3) 0.33818(17) 0.0285(8) Uani 1 1 d . .
O2 O 0.1912(3) 1.0669(3) 0.30725(18) 0.0282(8) Uani 1 1 d . .
O3 O 0.4734(3) 1.0869(3) 0.37593(19) 0.0310(9) Uani 1 1 d . .
O4 O 0.4721(3) 1.0497(3) 0.26049(18) 0.0279(8) Uani 1 1 d . .
O5 O 0.2093(3) 1.4186(3) 0.30780(19) 0.0326(9) Uani 1 1 d . .
O6 O 0.3820(3) 1.3524(3) 0.25713(17) 0.0314(8) Uani 1 1 d . .
N1 N 0.1607(4) 0.8112(4) 0.3936(2) 0.0257(10) Uani 1 1 d . .
N2 N 0.2712(4) 0.9973(4) 0.4615(2) 0.0285(10) Uani 1 1 d . .
C1 C 0.6206(5) 1.1954(4) 0.3076(3) 0.0257(11) Uani 1 1 d . .
C2 C 0.6285(5) 1.2948(5) 0.3470(3) 0.0286(12) Uani 1 1 d . .
C3 C 0.7322(5) 1.3708(5) 0.3364(3) 0.0328(13) Uani 1 1 d . .
H3 H 0.738089 1.439611 0.362626 0.039 Uiso 1 1 calc R U
C4 C 0.8259(5) 1.3479(5) 0.2888(3) 0.0333(13) Uani 1 1 d . .
H4 H 0.896245 1.399939 0.282901 0.040 Uiso 1 1 calc R U
C5 C 0.8165(5) 1.2489(5) 0.2498(3) 0.0308(12) Uani 1 1 d . .
H5 H 0.880300 1.232659 0.216774 0.037 Uiso 1 1 calc R U
C6 C 0.7143(5) 1.1731(5) 0.2587(3) 0.0299(12) Uani 1 1 d . .
H6 H 0.707736 1.105452 0.231305 0.036 Uiso 1 1 calc R U
C7 C 0.5361(5) 1.3251(4) 0.4033(3) 0.0273(12) Uani 1 1 d . .
C8 C 0.4013(5) 1.3610(5) 0.3881(3) 0.0278(11) Uani 1 1 d . .
C9 C 0.3300(5) 1.3904(4) 0.4464(3) 0.0276(12) Uani 1 1 d . .
H9 H 0.239195 1.415358 0.436590 0.033 Uiso 1 1 calc R U
C10 C 0.3869(5) 1.3844(5) 0.5174(3) 0.0332(13) Uani 1 1 d . .
H10 H 0.335496 1.403603 0.555812 0.040 Uiso 1 1 calc R U
C11 C 0.5196(5) 1.3502(5) 0.5321(3) 0.0326(12) Uani 1 1 d . .
H11 H 0.560406 1.346145 0.580883 0.039 Uiso 1 1 calc R U
C12 C 0.5936(5) 1.3216(5) 0.4753(3) 0.0320(13) Uani 1 1 d . .
H12 H 0.685296 1.299348 0.485893 0.038 Uiso 1 1 calc R U
C13 C 0.5177(5) 1.1077(5) 0.3157(3) 0.0269(12) Uani 1 1 d . .
C14 C 0.3267(5) 1.3768(5) 0.3138(3) 0.0284(12) Uani 1 1 d . .
C15 C 0.1258(5) 0.7113(5) 0.3650(3) 0.0308(13) Uani 1 1 d . .
H15 H 0.155034 0.692112 0.319562 0.037 Uiso 1 1 calc R U
C16 C 0.0476(5) 0.6328(5) 0.3989(3) 0.0334(13) Uani 1 1 d . .
H16 H 0.026456 0.561484 0.377510 0.040 Uiso 1 1 calc R U
C17 C 0.0027(5) 0.6622(5) 0.4638(3) 0.0325(13) Uani 1 1 d . .
H17 H -0.054276 0.612541 0.486605 0.039 Uiso 1 1 calc R U
C18 C 0.0406(5) 0.7647(5) 0.4962(3) 0.0283(12) Uani 1 1 d . .
C19 C 0.1241(5) 0.8366(5) 0.4604(2) 0.0263(12) Uani 1 1 d . .
C20 C 0.1788(5) 0.9359(4) 0.4951(3) 0.0257(12) Uani 1 1 d . .
C21 C 0.1432(5) 0.9640(4) 0.5642(3) 0.0275(12) Uani 1 1 d . .
C22 C 0.0500(5) 0.8948(5) 0.5977(3) 0.0311(13) Uani 1 1 d . .
H22 H 0.021991 0.916494 0.643057 0.037 Uiso 1 1 calc R U
C23 C 0.0017(5) 0.7991(5) 0.5655(3) 0.0321(13) Uani 1 1 d . .
H23 H -0.058947 0.753633 0.588784 0.039 Uiso 1 1 calc R U
C24 C 0.2038(5) 1.0603(5) 0.5986(3) 0.0309(12) Uani 1 1 d . .
H24 H 0.181067 1.082725 0.644908 0.037 Uiso 1 1 calc R U
C25 C 0.2941(5) 1.1203(4) 0.5653(3) 0.0281(12) Uani 1 1 d . .
H25 H 0.335690 1.185091 0.587910 0.034 Uiso 1 1 calc R U
C26 C 0.3258(5) 1.0858(5) 0.4967(3) 0.0303(12) Uani 1 1 d . .
H26 H 0.390300 1.128494 0.474336 0.036 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
O1 U1 O2 178.34(16) . .
O1 U1 O5 89.98(14) . 2_545
O2 U1 O5 90.40(14) . 2_545
O1 U1 O4 88.29(13) . .
O2 U1 O4 90.42(14) . .
O5 U1 O4 64.48(12) 2_545 .
O1 U1 O3 91.28(15) . .
O2 U1 O3 87.11(15) . .
O5 U1 O3 117.10(11) 2_545 .
O4 U1 O3 52.72(11) . .
O1 U1 O6 99.08(14) . 2_545
O2 U1 O6 82.42(15) . 2_545
O5 U1 O6 52.61(11) 2_545 2_545
O4 U1 O6 116.44(11) . 2_545
O3 U1 O6 165.02(12) . 2_545
O1 U1 N1 78.97(14) . .
O2 U1 N1 102.31(14) . .
O5 U1 N1 115.25(12) 2_545 .
O4 U1 N1 167.26(12) . .
O3 U1 N1 126.63(12) . .
O6 U1 N1 66.49(11) 2_545 .
O1 U1 N2 97.85(14) . .
O2 U1 N2 81.93(14) . .
O5 U1 N2 170.48(12) 2_545 .
O4 U1 N2 120.90(13) . .
O3 U1 N2 68.36(12) . .
O6 U1 N2 120.29(12) 2_545 .
N1 U1 N2 61.48(13) . .
C13 O3 U1 93.8(3) . .
C13 O4 U1 94.9(3) . .
C14 O5 U1 95.2(3) . 2
C14 O6 U1 91.3(3) . 2
C15 N1 C19 118.4(4) . .
C15 N1 U1 119.8(3) . .
C19 N1 U1 121.8(3) . .
C26 N2 C20 117.2(4) . .
C26 N2 U1 123.4(3) . .
C20 N2 U1 118.8(3) . .
C2 C1 C6 120.0(5) . .
C2 C1 C13 123.1(4) . .
C6 C1 C13 116.9(5) . .
C1 C2 C3 118.4(5) . .
C1 C2 C7 124.3(5) . .
C3 C2 C7 117.2(5) . .
C4 C3 C2 121.5(5) . .
C4 C3 H3 119.3 . .
C2 C3 H3 119.3 . .
C5 C4 C3 119.5(5) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
C4 C5 C6 120.1(5) . .
C4 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C5 C6 C1 120.5(5) . .
C5 C6 H6 119.7 . .
C1 C6 H6 119.7 . .
C12 C7 C8 118.8(5) . .
C12 C7 C2 116.0(4) . .
C8 C7 C2 125.0(4) . .
C9 C8 C7 118.3(5) . .
C9 C8 C14 115.8(4) . .
C7 C8 C14 125.8(4) . .
C10 C9 C8 122.4(5) . .
C10 C9 H9 118.8 . .
C8 C9 H9 118.8 . .
C9 C10 C11 119.2(5) . .
C9 C10 H10 120.4 . .
C11 C10 H10 120.4 . .
C10 C11 C12 119.8(5) . .
C10 C11 H11 120.1 . .
C12 C11 H11 120.1 . .
C7 C12 C11 121.4(5) . .
C7 C12 H12 119.3 . .
C11 C12 H12 119.3 . .
O3 C13 O4 118.2(5) . .
O3 C13 C1 122.6(5) . .
O4 C13 C1 119.2(4) . .
O5 C14 O6 119.9(4) . .
O5 C14 C8 119.1(4) . .
O6 C14 C8 120.9(4) . .
N1 C15 C16 123.2(5) . .
N1 C15 H15 118.4 . .
C16 C15 H15 118.4 . .
C17 C16 C15 118.2(5) . .
C17 C16 H16 120.9 . .
C15 C16 H16 120.9 . .
C16 C17 C18 120.0(5) . .
C16 C17 H17 120.0 . .
C18 C17 H17 120.0 . .
C17 C18 C19 118.4(5) . .
C17 C18 C23 123.0(5) . .
C19 C18 C23 118.6(5) . .
N1 C19 C18 121.6(5) . .
N1 C19 C20 117.8(4) . .
C18 C19 C20 120.5(4) . .
N2 C20 C21 122.4(5) . .
N2 C20 C19 118.5(4) . .
C21 C20 C19 119.0(5) . .
C20 C21 C24 117.7(5) . .
C20 C21 C22 120.0(5) . .
C24 C21 C22 122.2(5) . .
C23 C22 C21 120.5(5) . .
C23 C22 H22 119.7 . .
C21 C22 H22 119.7 . .
C22 C23 C18 121.1(5) . .
C22 C23 H23 119.4 . .
C18 C23 H23 119.4 . .
C25 C24 C21 119.6(5) . .
C25 C24 H24 120.2 . .
C21 C24 H24 120.2 . .
C24 C25 C26 119.2(5) . .
C24 C25 H25 120.4 . .
C26 C25 H25 120.4 . .
N2 C26 C25 123.9(5) . .
N2 C26 H26 118.0 . .
C25 C26 H26 118.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.756(3) .
U1 O2 1.764(3) .
U1 O5 2.438(3) 2_545
U1 O4 2.447(3) .
U1 O3 2.472(4) .
U1 O6 2.516(3) 2_545
U1 N1 2.631(4) .
U1 N2 2.684(4) .
O3 C13 1.270(6) .
O4 C13 1.275(6) .
O5 C14 1.265(6) .
O6 C14 1.272(6) .
N1 C15 1.331(7) .
N1 C19 1.363(6) .
N2 C26 1.324(7) .
N2 C20 1.377(6) .
C1 C2 1.387(7) .
C1 C6 1.397(7) .
C1 C13 1.481(7) .
C2 C3 1.403(7) .
C2 C7 1.511(7) .
C3 C4 1.382(7) .
C3 H3 0.9500 .
C4 C5 1.380(8) .
C4 H4 0.9500 .
C5 C6 1.383(7) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C12 1.393(7) .
C7 C8 1.408(7) .
C8 C9 1.403(7) .
C8 C14 1.502(7) .
C9 C10 1.375(7) .
C9 H9 0.9500 .
C10 C11 1.382(7) .
C10 H10 0.9500 .
C11 C12 1.393(7) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C15 C16 1.408(7) .
C15 H15 0.9500 .
C16 C17 1.375(7) .
C16 H16 0.9500 .
C17 C18 1.392(7) .
C17 H17 0.9500 .
C18 C19 1.409(7) .
C18 C23 1.442(7) .
C19 C20 1.424(7) .
C20 C21 1.406(7) .
C21 C24 1.413(7) .
C21 C22 1.434(7) .
C22 C23 1.349(8) .
C22 H22 0.9500 .
C23 H23 0.9500 .
C24 C25 1.351(7) .
C24 H24 0.9500 .
C25 C26 1.405(7) .
C25 H25 0.9500 .
C26 H26 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C15 H15 O4 0.95 2.50 3.091(6) 120.3 2_545 yes
C16 H16 O4 0.95 2.56 3.101(6) 116.1 2_545 yes
C26 H26 O3 0.95 2.14 2.813(6) 126.3 . yes
