#------------------------------------------------------------------------------
#$Date: 2020-02-04 22:42:09 +0200 (Tue, 04 Feb 2020) $
#$Revision: 247750 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/31/7703100.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_7703100
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            'C44 H52 Cu N6 O18 U2'
_chemical_formula_weight         1492.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                82.508(5)
_cell_angle_beta                 73.613(5)
_cell_angle_gamma                67.945(4)
_cell_formula_units_Z            1
_cell_length_a                   9.4464(8)
_cell_length_b                   9.6422(10)
_cell_length_c                   15.0190(12)
_cell_measurement_reflns_used    56007
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.66
_cell_volume                     1215.92(19)
_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 (737 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  0.1037
_diffrn_reflns_av_unetI/netI     0.1166
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56007
_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         25.679
_diffrn_reflns_theta_min         2.660
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.157
_exptl_absorpt_correction_T_max  0.606
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_description       platelet
_exptl_crystal_F_000             715
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.546
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4604
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0393
_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)+(0.0049P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3761
_reflns_number_total             4604
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04126e1.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7703096--7703104.cif.'
_cod_original_cell_volume        1215.9(2)
_cod_database_code               7703100
_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, -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
_atom_site_refinement_flags_occupancy
U1 U 0.04625(3) 0.51040(3) 0.81900(2) 0.03275(9) Uani 1 1 d . . .
Cu1 Cu 0.500000 0.500000 0.500000 0.0321(3) Uani 1 2 d S . P
O1 O 0.1629(4) 0.5957(4) 0.8445(4) 0.0319(11) Uani 1 1 d . . .
O2 O -0.0710(4) 0.4269(4) 0.7914(3) 0.0351(11) Uani 1 1 d . . .
O3 O 0.0997(4) 0.3471(4) 0.9414(3) 0.0314(11) Uani 1 1 d . . .
O4 O 0.1809(5) 0.3653(4) 1.0638(4) 0.0367(12) Uani 1 1 d . . .
O5 O 0.2638(4) 0.3435(4) 0.7256(4) 0.0342(12) Uani 1 1 d . . .
O6 O 0.3188(5) 0.1781(5) 0.6180(4) 0.0383(12) Uani 1 1 d . . .
O7 O 0.0837(5) 0.6381(4) 0.6603(4) 0.0393(12) Uani 1 1 d . . .
O8 O -0.1082(5) 0.7715(4) 0.7649(4) 0.0371(12) Uani 1 1 d . . .
O9 O -0.0335(5) 0.8762(5) 0.6315(4) 0.0418(13) Uani 1 1 d . . .
N1 N -0.0223(6) 0.7683(6) 0.6841(5) 0.0372(15) Uani 1 1 d . . .
N2 N 0.7030(6) 0.3491(5) 0.5270(4) 0.0298(13) Uani 1 1 d D . .
H2 H 0.756(6) 0.365(6) 0.4635(15) 0.036 Uiso 1 1 d D U .
N3 N 0.4711(6) 0.3212(5) 0.4619(5) 0.0334(14) Uani 1 1 d D . .
H3 H 0.398(5) 0.308(6) 0.519(2) 0.040 Uiso 1 1 d D U .
C1 C 0.3761(6) 0.2649(6) 0.9274(5) 0.0303(16) Uani 1 1 d . . .
C2 C 0.4257(7) 0.1520(6) 0.8629(5) 0.0336(16) Uani 1 1 d . . .
C3 C 0.5819(7) 0.1049(7) 0.8130(5) 0.0361(17) Uani 1 1 d . . .
H3A H 0.619327 0.025855 0.770934 0.043 Uiso 1 1 calc R U .
C4 C 0.6850(7) 0.1684(7) 0.8222(5) 0.0387(17) Uani 1 1 d . . .
H4 H 0.790737 0.134700 0.785176 0.046 Uiso 1 1 calc R U .
C5 C 0.6374(7) 0.2793(7) 0.8837(5) 0.0352(17) Uani 1 1 d . . .
H5 H 0.708649 0.323900 0.889008 0.042 Uiso 1 1 calc R U .
C6 C 0.4822(7) 0.3262(6) 0.9387(5) 0.0354(17) Uani 1 1 d . . .
H6 H 0.448791 0.399923 0.983855 0.043 Uiso 1 1 calc R U .
C7 C 0.3164(7) 0.0785(6) 0.8551(5) 0.0315(16) Uani 1 1 d . . .
C8 C 0.2550(7) 0.1008(6) 0.7769(5) 0.0318(17) Uani 1 1 d . . .
C9 C 0.1566(7) 0.0286(6) 0.7721(5) 0.0361(17) Uani 1 1 d . . .
H9 H 0.116914 0.042314 0.718879 0.043 Uiso 1 1 calc R U .
C10 C 0.1151(7) -0.0653(6) 0.8460(6) 0.0355(17) Uani 1 1 d . . .
H10 H 0.043018 -0.111278 0.844010 0.043 Uiso 1 1 calc R U .
C11 C 0.1774(7) -0.0909(7) 0.9205(6) 0.043(2) Uani 1 1 d . . .
H11 H 0.151317 -0.157669 0.969086 0.051 Uiso 1 1 calc R U .
C12 C 0.2785(7) -0.0208(6) 0.9267(5) 0.0372(17) Uani 1 1 d . . .
H12 H 0.321702 -0.039879 0.978960 0.045 Uiso 1 1 calc R U .
C13 C 0.2083(7) 0.3287(7) 0.9819(5) 0.0323(16) Uani 1 1 d . . .
C14 C 0.2845(7) 0.2088(7) 0.6983(6) 0.0343(17) Uani 1 1 d . . .
C15 C 0.6865(7) 0.2014(6) 0.5347(5) 0.0336(17) Uani 1 1 d . . .
H15A H 0.615341 0.189879 0.595416 0.040 Uiso 1 1 calc R U .
H15B H 0.790844 0.120783 0.530096 0.040 Uiso 1 1 calc R U .
C16 C 0.6201(7) 0.1907(6) 0.4579(6) 0.0388(19) Uani 1 1 d . . .
H16A H 0.696595 0.191034 0.397322 0.047 Uiso 1 1 calc R U .
H16B H 0.598782 0.096373 0.464818 0.047 Uiso 1 1 calc R U .
C17 C 0.3998(7) 0.3402(6) 0.3817(6) 0.0327(17) Uani 1 1 d . . .
C18 C 0.2378(6) 0.4653(6) 0.4046(5) 0.0299(15) Uani 1 1 d . . .
H18A H 0.177712 0.458024 0.362091 0.036 Uiso 1 1 calc R U .
H18B H 0.181029 0.445718 0.468370 0.036 Uiso 1 1 calc R U .
C19 C 0.2329(7) 0.6262(6) 0.3988(5) 0.0322(16) Uani 1 1 d . . .
H19 H 0.298525 0.645219 0.336820 0.039 Uiso 1 1 calc R U .
C20 C 0.3757(7) 0.1972(6) 0.3677(6) 0.0430(19) Uani 1 1 d . . .
H20A H 0.475384 0.112248 0.362652 0.065 Uiso 1 1 calc R U .
H20B H 0.341004 0.207850 0.310747 0.065 Uiso 1 1 calc R U .
H20C H 0.295228 0.179896 0.420829 0.065 Uiso 1 1 calc R U .
C21 C 0.5098(7) 0.3788(7) 0.2933(6) 0.0432(19) Uani 1 1 d . . .
H21A H 0.549307 0.451569 0.307661 0.065 Uiso 1 1 calc R U .
H21B H 0.451219 0.421649 0.245809 0.065 Uiso 1 1 calc R U .
H21C H 0.598910 0.287657 0.270196 0.065 Uiso 1 1 calc R U .
C22 C 0.0602(6) 0.7347(6) 0.4098(6) 0.0382(18) Uani 1 1 d . . .
H22A H -0.005026 0.715224 0.469968 0.057 Uiso 1 1 calc R U .
H22B H 0.019985 0.719356 0.359871 0.057 Uiso 1 1 calc R U .
H22C H 0.056335 0.838205 0.406466 0.057 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'
Cu Cu 0.3201 1.2651 '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 178.9(2) . .
O1 U1 O5 91.02(16) . .
O2 U1 O5 88.84(16) . .
O1 U1 O3 86.93(18) . .
O2 U1 O3 94.17(18) . .
O5 U1 O3 87.36(15) . .
O1 U1 O4 94.26(17) . 2_567
O2 U1 O4 86.10(17) . 2_567
O5 U1 O4 167.21(14) . 2_567
O3 U1 O4 81.30(15) . 2_567
O1 U1 O7 87.23(19) . .
O2 U1 O7 91.66(19) . .
O5 U1 O7 74.23(15) . .
O3 U1 O7 160.57(13) . .
O4 U1 O7 117.62(14) 2_567 .
O1 U1 O8 85.21(16) . .
O2 U1 O8 93.94(16) . .
O5 U1 O8 123.99(16) . .
O3 U1 O8 147.73(15) . .
O4 U1 O8 68.17(16) 2_567 .
O7 U1 O8 49.79(14) . .
N3 Cu1 N3 180.0 2_666 .
N3 Cu1 N2 94.7(2) 2_666 .
N3 Cu1 N2 85.3(2) . .
N3 Cu1 N2 85.3(2) 2_666 2_666
N3 Cu1 N2 94.7(2) . 2_666
N2 Cu1 N2 180.0(2) . 2_666
C13 O3 U1 125.9(4) . .
C13 O4 U1 136.2(4) . 2_567
C14 O5 U1 129.5(4) . .
N1 O7 U1 97.3(4) . .
N1 O8 U1 97.7(4) . .
O9 N1 O8 124.2(6) . .
O9 N1 O7 121.5(6) . .
O8 N1 O7 114.3(6) . .
C15 N2 C19 113.4(5) . 2_666
C15 N2 Cu1 106.0(3) . .
C19 N2 Cu1 121.4(4) 2_666 .
C15 N2 H2 108(3) . .
C19 N2 H2 117(3) 2_666 .
Cu1 N2 H2 88(3) . .
C16 N3 C17 115.6(6) . .
C16 N3 Cu1 107.9(4) . .
C17 N3 Cu1 118.3(4) . .
C16 N3 H3 106(3) . .
C17 N3 H3 110(4) . .
Cu1 N3 H3 97(4) . .
C6 C1 C2 120.4(6) . .
C6 C1 C13 117.8(6) . .
C2 C1 C13 121.7(5) . .
C3 C2 C1 117.3(5) . .
C3 C2 C7 121.8(6) . .
C1 C2 C7 120.7(6) . .
C4 C3 C2 122.2(6) . .
C4 C3 H3A 118.9 . .
C2 C3 H3A 118.9 . .
C5 C4 C3 120.8(6) . .
C5 C4 H4 119.6 . .
C3 C4 H4 119.6 . .
C4 C5 C6 119.0(6) . .
C4 C5 H5 120.5 . .
C6 C5 H5 120.5 . .
C1 C6 C5 120.1(6) . .
C1 C6 H6 119.9 . .
C5 C6 H6 119.9 . .
C12 C7 C8 119.1(5) . .
C12 C7 C2 118.6(6) . .
C8 C7 C2 122.3(6) . .
C9 C8 C7 120.2(6) . .
C9 C8 C14 116.9(7) . .
C7 C8 C14 122.9(5) . .
C8 C9 C10 119.9(7) . .
C8 C9 H9 120.1 . .
C10 C9 H9 120.1 . .
C11 C10 C9 120.3(6) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
C10 C11 C12 121.0(7) . .
C10 C11 H11 119.5 . .
C12 C11 H11 119.5 . .
C11 C12 C7 119.5(7) . .
C11 C12 H12 120.3 . .
C7 C12 H12 120.3 . .
O4 C13 O3 123.4(6) . .
O4 C13 C1 118.5(6) . .
O3 C13 C1 118.0(6) . .
O6 C14 O5 123.0(7) . .
O6 C14 C8 122.7(6) . .
O5 C14 C8 114.2(6) . .
N2 C15 C16 108.4(5) . .
N2 C15 H15A 110.0 . .
C16 C15 H15A 110.0 . .
N2 C15 H15B 110.0 . .
C16 C15 H15B 110.0 . .
H15A C15 H15B 108.4 . .
N3 C16 C15 108.4(5) . .
N3 C16 H16A 110.0 . .
C15 C16 H16A 110.0 . .
N3 C16 H16B 110.0 . .
C15 C16 H16B 110.0 . .
H16A C16 H16B 108.4 . .
N3 C17 C20 110.9(5) . .
N3 C17 C18 107.8(6) . .
C20 C17 C18 108.1(5) . .
N3 C17 C21 109.1(5) . .
C20 C17 C21 109.6(6) . .
C18 C17 C21 111.4(6) . .
C19 C18 C17 117.8(4) . .
C19 C18 H18A 107.9 . .
C17 C18 H18A 107.9 . .
C19 C18 H18B 107.9 . .
C17 C18 H18B 107.9 . .
H18A C18 H18B 107.2 . .
N2 C19 C18 110.2(5) 2_666 .
N2 C19 C22 110.1(5) 2_666 .
C18 C19 C22 109.1(4) . .
N2 C19 H19 109.1 2_666 .
C18 C19 H19 109.1 . .
C22 C19 H19 109.1 . .
C17 C20 H20A 109.5 . .
C17 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C17 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C17 C21 H21A 109.5 . .
C17 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C17 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C19 C22 H22A 109.5 . .
C19 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C19 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.742(4) .
U1 O2 1.750(4) .
U1 O5 2.293(4) .
U1 O3 2.299(5) .
U1 O4 2.372(4) 2_567
U1 O7 2.532(5) .
U1 O8 2.551(4) .
Cu1 N3 2.019(5) 2_666
Cu1 N3 2.019(5) .
Cu1 N2 2.037(5) .
Cu1 N2 2.037(5) 2_666
O3 C13 1.281(7) .
O4 C13 1.252(8) .
O5 C14 1.340(7) .
O6 C14 1.203(9) .
O7 N1 1.295(6) .
O8 N1 1.252(7) .
O9 N1 1.211(7) .
N2 C15 1.476(7) .
N2 C19 1.490(8) 2_666
N2 H2 0.968(10) .
N3 C16 1.486(7) .
N3 C17 1.499(9) .
N3 H3 0.964(10) .
C1 C6 1.396(8) .
C1 C2 1.406(8) .
C1 C13 1.492(8) .
C2 C3 1.380(8) .
C2 C7 1.491(8) .
C3 C4 1.374(8) .
C3 H3A 0.9500 .
C4 C5 1.364(8) .
C4 H4 0.9500 .
C5 C6 1.397(8) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C12 1.405(9) .
C7 C8 1.410(9) .
C8 C9 1.375(8) .
C8 C14 1.506(9) .
C9 C10 1.401(9) .
C9 H9 0.9500 .
C10 C11 1.361(10) .
C10 H10 0.9500 .
C11 C12 1.389(8) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C15 C16 1.490(9) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C20 1.527(7) .
C17 C18 1.530(7) .
C17 C21 1.537(9) .
C18 C19 1.527(7) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C22 1.548(7) .
C19 H19 1.0000 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
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
N2 H2 O7 0.968(10) 2.033(18) 2.981(7) 166(5) 2_666 yes
N3 H3 O6 0.964(10) 1.98(3) 2.866(7) 151(5) . yes
