A structural and thermodynamic study of the complexes of U(vi) with azinecarboxylates.
Lv, Lina; Chen, Baihua; Liu, Jun; Chen, Jing; Xu, Chao; Yang, Yanqiu; Dalton transactions (Cambridge, England : 2003) 48 (2019) 566–577; doi:10.1039/c8dt04099k

data_7048247
_publ_section_title
;
 A structural and thermodynamic study of the complexes of U(vi) with
 azinecarboxylates.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              566
_journal_page_last               577
_journal_paper_doi               10.1039/c8dt04099k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C10 H8 N4 O7 U, H2 O'
_chemical_formula_sum            'C10 H10 N4 O8 U'
_chemical_formula_weight         552.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-11-21 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                87.484(5)
_cell_angle_beta                 75.764(6)
_cell_angle_gamma                88.380(6)
_cell_formula_units_Z            2
_cell_length_a                   7.8240(5)
_cell_length_b                   8.0617(6)
_cell_length_c                   11.9538(7)
_cell_measurement_reflns_used    2471
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8770
_cell_measurement_theta_min      3.7110
_cell_volume                     730.01(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -82.00    2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -57.0000   30.0000 84

  2 omega  -25.00   24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -99.0000   60.0000 49

  3 omega  -32.00   49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669   57.0000 -180.0000 81

  4 omega  -58.00  -23.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -38.0000  -30.0000 35

  5 omega  -15.00   19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -99.0000 -180.0000 34

  6 omega  -50.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8419  -77.0000  -60.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0785129000
_diffrn_orient_matrix_UB_12      -0.0448060000
_diffrn_orient_matrix_UB_13      0.0053505000
_diffrn_orient_matrix_UB_21      0.0434953000
_diffrn_orient_matrix_UB_22      -0.0738485000
_diffrn_orient_matrix_UB_23      0.0134430000
_diffrn_orient_matrix_UB_31      -0.0263523000
_diffrn_orient_matrix_UB_32      0.0172473000
_diffrn_orient_matrix_UB_33      0.0595284000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5942
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.904
_refine_diff_density_min         -1.746
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.0245(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2982
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2676
_reflns_number_total             2982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04099k2.cif
_cod_data_source_block           170623_s2_yyq
_cod_depositor_comments
;
Adding full bibliography for 7048244--7048247.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C10 H8 N4 O7 U), 2(H2 O)'
_cod_original_formula_sum        'C20 H20 N8 O16 U2'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1104.50
_cod_database_code               7048247
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3u1
_shelx_estimated_absorpt_t_max   0.135
_shelx_estimated_absorpt_t_min   0.112
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7B
 0.86 with sigma of 0.02
3.a Free rotating group:
 O8(H8A,H8B)
3.b Rotating group:
 O7(H7A)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'