#------------------------------------------------------------------------------
#$Date: 2022-01-29 01:31:18 +0200 (Sat, 29 Jan 2022) $
#$Revision: 272324 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/43/7244312.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_7244312
loop_
_publ_author_name
'Harrowfield, Jack'
'Atoini, Youssef'
'Thuéry, Pierre'
_publ_section_title
;
 Plumbing the uncertainties of solvothermal synthesis involving uranyl ion
 carboxylate complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01663F
_journal_year                    2022
_chemical_formula_sum            'C11 H13 N O7 U'
_chemical_formula_weight         509.25
_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_update_record
;
2021-12-06 deposited with the CCDC.	2022-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                109.0421(16)
_cell_angle_beta                 92.0632(19)
_cell_angle_gamma                108.7106(17)
_cell_formula_units_Z            2
_cell_length_a                   7.3392(4)
_cell_length_b                   8.7663(4)
_cell_length_c                   11.8187(5)
_cell_measurement_reflns_used    9704
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.1669
_cell_measurement_theta_min      4.3607
_cell_volume                     672.34(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            57490
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.63
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms 70 W'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    12.102
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.073
_refine_diff_density_max         2.004
_refine_diff_density_min         -0.529
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4093
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0142
_refine_ls_R_factor_gt           0.0135
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0156P)²+0.5953P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0325
_refine_ls_wR_factor_ref         0.0328
_reflns_number_gt                3967
_reflns_number_total             4093
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01663f1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7244312
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.65883(2) 0.30952(2) 0.19895(2) 0.01188(3) Uani d . . . 1.0 . .
O O1 0.9101(2) 0.3463(2) 0.19385(13) 0.0178(3) Uani d . . . 1.0 . .
O O2 0.4078(2) 0.2717(2) 0.20517(14) 0.0193(3) Uani d . . . 1.0 . .
O O3 0.5880(2) 0.01134(18) 0.11672(13) 0.0157(3) Uani d . . . 1.0 . .
O O4 0.3815(2) -0.25654(19) 0.01636(13) 0.0162(3) Uani d . . . 1.0 . .
O O5 0.2596(2) -0.50637(19) 0.58603(13) 0.0201(3) Uani d . . . 1.0 . .
O O6 0.3119(3) -0.23211(19) 0.62372(13) 0.0219(3) Uani d . . . 1.0 . .
O O7 0.6980(2) 0.57880(19) 0.19457(15) 0.0207(3) Uani d . . . 1.0 . .
C C1 0.4631(3) -0.1302(2) 0.11321(17) 0.0127(3) Uani d . . . 1.0 . .
C C2 0.4192(3) -0.1430(3) 0.23237(17) 0.0151(3) Uani d . . . 1.0 . .
H H2 0.453092 -0.037605 0.299277 0.018 Uiso calc U . R 1.0 . .
C C3 0.3367(3) -0.2884(3) 0.25492(17) 0.0147(3) Uani d . . . 1.0 . .
H H3 0.287487 -0.396543 0.190101 0.018 Uiso calc U . R 1.0 . .
C C4 0.3230(3) -0.2794(3) 0.37894(17) 0.0156(4) Uani d . . . 1.0 . .
H H4 0.352495 -0.16809 0.438822 0.019 Uiso calc U . R 1.0 . .
C C5 0.2728(3) -0.4132(3) 0.41681(18) 0.0167(4) Uani d . . . 1.0 . .
H H5 0.232158 -0.527467 0.359492 0.02 Uiso calc U . R 1.0 . .
C C6 0.2802(3) -0.3836(3) 0.54738(18) 0.0174(4) Uani d . . . 1.0 . .
N N1A 0.8828(4) 0.8014(3) 0.1463(2) 0.0173(6) Uani d . P . 0.745(5) A 1
C C7A 0.8159(4) 0.7335(4) 0.2268(3) 0.0151(6) Uani d . P . 0.745(5) A 1
C C9A 1.0258(5) 1.0255(4) 0.3358(3) 0.0279(7) Uani d . P . 0.745(5) A 1
H H9A 1.156629 1.051819 0.371999 0.034 Uiso d U P R 0.745(5) A 1
H H9B 0.988189 1.123839 0.371469 0.034 Uiso d U P R 0.745(5) A 1
N N1B 0.8788(10) 0.8535(8) 0.2467(6) 0.0156(16) Uani d . P . 0.255(5) A 2
C C7B 0.8050(11) 0.7007(11) 0.1615(9) 0.0123(16) Uani d U P . 0.255(5) A 2
C C9B 0.9730(13) 0.8972(11) 0.0673(7) 0.0188(17) Uani d . P . 0.255(5) A 2
H H9C 1.094175 0.908562 0.036634 0.023 Uiso d U P R 0.255(5) A 2
H H9D 0.908355 0.955522 0.033464 0.023 Uiso d U P R 0.255(5) A 2
C C8 0.8867(4) 0.8688(4) 0.3572(2) 0.0349(6) Uani d . . . 1.0 . .
H H8A 0.953226 0.829969 0.407217 0.042 Uiso d U P R 0.745(5) A 1
H H8B 0.779674 0.893119 0.393917 0.042 Uiso d U P R 0.745(5) A 1
H H8C 0.787424 0.770269 0.363327 0.052 Uiso d U P R 0.255(5) A 2
H H8D 1.012045 0.874369 0.388637 0.052 Uiso d U P R 0.255(5) A 2
H H8E 0.863754 0.971759 0.403067 0.052 Uiso d U P R 0.255(5) A 2
C C10 1.0138(3) 0.9824(3) 0.2001(2) 0.0209(4) Uani d . . . 1.0 . .
H H10A 0.961541 1.05529 0.174677 0.025 Uiso d U P R 0.745(5) A 1
H H10B 1.140311 0.995871 0.176647 0.025 Uiso d U P R 0.745(5) A 1
H H10C 1.148061 1.008991 0.229807 0.025 Uiso d U P R 0.255(5) A 2
H H10D 0.985821 1.087111 0.223757 0.025 Uiso d U P R 0.255(5) A 2
C C11 0.8471(4) 0.7062(3) 0.0233(3) 0.0353(6) Uani d . . . 1.0 . .
H H11A 0.758078 0.591481 0.008116 0.053 Uiso d U P R 0.745(5) A 1
H H11B 0.791157 0.760831 -0.019404 0.053 Uiso d U P R 0.745(5) A 1
H H11C 0.967248 0.700971 -0.004244 0.053 Uiso d U P R 0.745(5) A 1
H H11D 0.730668 0.679761 -0.030204 0.042 Uiso d U P R 0.255(5) A 2
H H11E 0.917648 0.633211 -0.014784 0.042 Uiso d U P R 0.255(5) 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 U1 O1 . . 179.38(7) ?
O2 U1 O7 . . 89.40(7) ?
O1 U1 O7 . . 91.08(7) ?
O2 U1 O3 . . 89.33(6) ?
O1 U1 O3 . . 90.40(6) ?
O7 U1 O3 . . 155.89(5) ?
O2 U1 O4 . 2_655 93.01(6) ?
O1 U1 O4 . 2_655 87.47(6) ?
O7 U1 O4 . 2_655 77.63(5) ?
O3 U1 O4 . 2_655 78.40(5) ?
O2 U1 O6 . 2_656 90.18(7) ?
O1 U1 O6 . 2_656 89.23(7) ?
O7 U1 O6 . 2_656 127.42(5) ?
O3 U1 O6 . 2_656 76.66(5) ?
O4 U1 O6 2_655 2_656 154.81(5) ?
O2 U1 O5 . 2_656 90.05(6) ?
O1 U1 O5 . 2_656 89.70(6) ?
O7 U1 O5 . 2_656 74.28(5) ?
O3 U1 O5 . 2_656 129.79(5) ?
O4 U1 O5 2_655 2_656 151.70(5) ?
O6 U1 O5 2_656 2_656 53.14(5) ?
C1 O3 U1 . . 141.32(13) ?
C1 O4 U1 . 2_655 137.38(13) ?
C6 O5 U1 . 2_656 92.60(12) ?
C6 O6 U1 . 2_656 94.91(12) ?
C7A O7 U1 . . 144.19(17) ?
C7B O7 U1 . . 143.8(4) ?
O4 C1 O3 . . 123.68(18) ?
O4 C1 C2 . . 120.27(17) ?
O3 C1 C2 . . 116.03(17) ?
C3 C2 C1 . . 126.59(18) ?
C3 C2 H2 . . 116.7 ?
C1 C2 H2 . . 116.7 ?
C2 C3 C4 . . 119.57(18) ?
C2 C3 H3 . . 120.2 ?
C4 C3 H3 . . 120.2 ?
C5 C4 C3 . . 126.06(18) ?
C5 C4 H4 . . 117.0 ?
C3 C4 H4 . . 117.0 ?
C4 C5 C6 . . 120.12(18) ?
C4 C5 H5 . . 119.9 ?
C6 C5 H5 . . 119.9 ?
O5 C6 O6 . . 119.02(18) ?
O5 C6 C5 . . 120.85(18) ?
O6 C6 C5 . . 120.11(18) ?
C7A N1A C11 . . 122.7(3) ?
C7A N1A C10 . . 113.4(2) ?
C11 N1A C10 . . 123.6(2) ?
O7 C7A N1A . . 121.1(3) ?
O7 C7A C8 . . 127.7(3) ?
N1A C7A C8 . . 111.1(2) ?
C10 C9A C8 . . 107.7(2) ?
C10 C9A H9A . . 110.3 ?
C8 C9A H9A . . 110.4 ?
C10 C9A H9B . . 110.0 ?
C8 C9A H9B . . 109.9 ?
H9A C9A H9B . . 108.5 ?
C8 N1B C7B . . 120.2(7) ?
C8 N1B C10 . . 124.2(5) ?
C7B N1B C10 . . 111.3(6) ?
O7 C7B N1B . . 115.9(8) ?
O7 C7B C11 . . 131.4(7) ?
N1B C7B C11 . . 112.2(6) ?
C10 C9B C11 . . 114.1(5) ?
C10 C9B H9C . . 109.0 ?
C11 C9B H9C . . 108.7 ?
C10 C9B H9D . . 108.9 ?
C11 C9B H9D . . 108.6 ?
H9C C9B H9D . . 107.5 ?
C9A C8 C7A . . 102.4(2) ?
C9A C8 H8A . . 111.3 ?
C7A C8 H8A . . 111.1 ?
C9A C8 H8B . . 111.7 ?
C7A C8 H8B . . 111.2 ?
H8A C8 H8B . . 109.2 ?
N1B C8 H8C . . 108.4 ?
N1B C8 H8D . . 110.4 ?
H8C C8 H8D . . 109.5 ?
N1B C8 H8E . . 109.6 ?
H8C C8 H8E . . 109.5 ?
H8D C8 H8E . . 109.4 ?
C9B C10 N1B . . 104.7(4) ?
N1A C10 C9A . . 105.0(2) ?
N1A C10 H10A . . 110.5 ?
C9A C10 H10A . . 111.0 ?
N1A C10 H10B . . 110.8 ?
C9A C10 H10B . . 110.7 ?
H10A C10 H10B . . 108.8 ?
C9B C10 H10C . . 110.6 ?
N1B C10 H10C . . 111.7 ?
C9B C10 H10D . . 110.4 ?
N1B C10 H10D . . 110.6 ?
H10C C10 H10D . . 108.9 ?
C9B C11 C7B . . 96.0(4) ?
N1A C11 H11A . . 109.8 ?
N1A C11 H11B . . 109.1 ?
H11A C11 H11B . . 109.5 ?
N1A C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C9B C11 H11D . . 112.3 ?
C7B C11 H11D . . 113.2 ?
C9B C11 H11E . . 112.3 ?
C7B C11 H11E . . 112.6 ?
H11D C11 H11E . . 110.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O2 . 1.7729(15) ?
U1 O1 . 1.7745(15) ?
U1 O7 . 2.3029(15) ?
U1 O3 . 2.3412(14) ?
U1 O4 2_655 2.4217(14) ?
U1 O6 2_656 2.4266(15) ?
U1 O5 2_656 2.4820(15) ?
O3 C1 . 1.271(2) ?
O4 C1 . 1.262(2) ?
O5 C6 . 1.269(2) ?
O6 C6 . 1.279(3) ?
O7 C7A . 1.273(3) ?
O7 C7B . 1.292(8) ?
C1 C2 . 1.488(3) ?
C2 C3 . 1.342(3) ?
C2 H2 . 0.95 ?
C3 C4 . 1.451(3) ?
C3 H3 . 0.95 ?
C4 C5 . 1.337(3) ?
C4 H4 . 0.95 ?
C5 C6 . 1.475(3) ?
C5 H5 . 0.95 ?
N1A C7A . 1.311(4) ?
N1A C11 . 1.385(4) ?
N1A C10 . 1.471(3) ?
C7A C8 . 1.551(4) ?
C9A C10 . 1.515(4) ?
C9A C8 . 1.529(4) ?
C9A H9A . 0.9603 ?
C9A H9B . 0.9599 ?
N1B C8 . 1.266(7) ?
N1B C7B . 1.310(11) ?
N1B C10 . 1.512(7) ?
C7B C11 . 1.687(10) ?
C9B C10 . 1.473(8) ?
C9B C11 . 1.527(9) ?
C9B H9C . 0.9604 ?
C9B H9D . 0.9598 ?
C8 H8A . 0.9598 ?
C8 H8B . 0.9602 ?
C8 H8C . 0.9607 ?
C8 H8D . 0.9601 ?
C8 H8E . 0.9599 ?
C10 H10A . 0.9598 ?
C10 H10B . 0.9605 ?
C10 H10C . 0.9604 ?
C10 H10D . 0.9598 ?
C11 H11A . 0.9606 ?
C11 H11B . 0.9598 ?
C11 H11C . 0.9604 ?
C11 H11D . 0.9601 ?
C11 H11E . 0.9598 ?
