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_7048245
_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'
_chemical_formula_sum            'C10 H8 N4 O7 U'
_chemical_formula_weight         534.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-04 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.1101(17)
_cell_length_b                   7.7452(5)
_cell_length_c                   6.8023(5)
_cell_measurement_reflns_used    1268
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6100
_cell_measurement_theta_min      3.9850
_cell_volume                     1375.62(16)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.998
_diffrn_measurement_details
;
  1 omega  -82.00  -18.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      -15.1231  -57.0000   30.0000 64

  2 omega   -2.00   24.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      -15.1231  -99.0000  -60.0000 26

  3 omega  -13.00   34.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -       16.8419  -57.0000 -120.0000 47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0244870000
_diffrn_orient_matrix_UB_12      -0.0363073000
_diffrn_orient_matrix_UB_13      0.0183013000
_diffrn_orient_matrix_UB_21      -0.0110153000
_diffrn_orient_matrix_UB_22      0.0836928000
_diffrn_orient_matrix_UB_23      -0.0018986000
_diffrn_orient_matrix_UB_31      -0.0041400000
_diffrn_orient_matrix_UB_32      -0.0079813000
_diffrn_orient_matrix_UB_33      -0.1026324000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3779
_diffrn_reflns_point_group_measured_fraction_full 0.813
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.058
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37301
_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    2.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.729
_refine_diff_density_min         -2.167
_refine_diff_density_rms         0.200
_refine_ls_abs_structure_details
;
 Flack x determined using 503 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.43(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2244
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0412P)^2^+0.3348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.467
_reflns_Friedel_fraction_full    0.592
_reflns_Friedel_fraction_max     0.555
_reflns_number_gt                1862
_reflns_number_total             2244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04099k2.cif
_cod_data_source_block           180613_s2_yyq_u-pz2
_cod_depositor_comments
'Adding full bibliography for 7048244--7048247.cif.'
_cod_original_cell_volume        1375.61(16)
_cod_database_code               7048245
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3u1
_shelx_estimated_absorpt_t_max   0.200
_shelx_estimated_absorpt_t_min   0.088
_reflns_odcompleteness_completeness 99.58
_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,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) =
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10)
Uanis(N1) = Uanis(N2) = Uanis(N3) = Uanis(N4)
3.a Rotating group:
 O7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9)
;
_shelx_res_checksum              37187
_olex2_submission_special_instructions 'No special instructions were received'