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_7048244
_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         'C15 H11 Cl N6 Na2 O13 U, H2 O'
_chemical_formula_sum            'C15 H13 Cl N6 Na2 O14 U'
_chemical_formula_weight         820.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-21 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.600(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1242(3)
_cell_length_b                   7.06510(10)
_cell_length_c                   23.2973(5)
_cell_measurement_reflns_used    3761
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8400
_cell_measurement_theta_min      3.1330
_cell_volume                     2409.02(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  19.20   0.70    3.50    --  -14.97 -99.00 150.00   56
  2  \w    -37.00  72.20   0.70    3.50    --   16.69   0.00-120.00  156
  3  \w     12.00  85.50   0.70    3.50    --   16.69  38.00 -90.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0107795000
_diffrn_orient_matrix_UB_12      0.0221305000
_diffrn_orient_matrix_UB_13      -0.0271437000
_diffrn_orient_matrix_UB_21      0.0462241000
_diffrn_orient_matrix_UB_22      -0.0251114000
_diffrn_orient_matrix_UB_23      0.0126097000
_diffrn_orient_matrix_UB_31      -0.0097372000
_diffrn_orient_matrix_UB_32      -0.0946909000
_diffrn_orient_matrix_UB_33      -0.0096892000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10946
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.912
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.263
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.842
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4917
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0334
_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/[\s^2^(Fo^2^)+(0.0333P)^2^+2.5865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4089
_reflns_number_total             4917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04099k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7048244--7048247.cif.'
_cod_database_code               7048244
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2u1
_shelx_estimated_absorpt_t_max   0.229
_shelx_estimated_absorpt_t_min   0.194
_reflns_odcompleteness_completeness 99.78
_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. Restrained distances
 O13-H13B = O13-H13A
 0.86 with sigma of 0.02
 O13-H13B
 0.86 with sigma of 0.02
3.a Free rotating group:
 O14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.316
_oxdiff_exptl_absorpt_empirical_full_min 0.782