Complexation of Am(III) and Eu(III) with DRAPA (N,N-dialkyl-6-amide-pyridine-2-carboxylic acid
Xu, Chao; Liu, Tingting; Liu, Qian; Yang, Suliang; Li, Dingming; Tian, Guoxin; Dalton Transactions  (2023) –; doi:10.1039/D3DT02319B

data_7713801
_publ_section_title
;
 Complexation of Am(III) and Eu(III) with DRAPA
 (N,N-dialkyl-6-amide-pyridine-2-carboxylic acid
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02319B
_journal_year                    2023
_chemical_formula_moiety         'C27 H27 Eu N6 O9'
_chemical_formula_sum            'C27 H27 Eu N6 O9'
_chemical_formula_weight         731.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-02 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.685(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7029(8)
_cell_length_b                   20.7207(13)
_cell_length_c                   12.2192(7)
_cell_measurement_reflns_used    5505
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.3710
_cell_measurement_theta_min      3.6170
_cell_volume                     3546.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.830
_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    -14.00  15.00   1.00    2.00    --  -11.20 -99.00 -60.00   29
  2  \w     -5.00  21.00   1.00    2.00    --   12.61  37.00 -90.00   26
  3  \w     -3.00  25.00   1.00    2.00    --   12.61  37.00 -60.00   28
  4  \w     27.00  81.00   1.00    2.00    --   12.61  37.00 -60.00   54
  5  \w    -58.00  21.00   1.00    2.00    --   12.61 -37.00 120.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0434846000
_diffrn_orient_matrix_UB_12      0.0035346000
_diffrn_orient_matrix_UB_13      0.0131728000
_diffrn_orient_matrix_UB_21      0.0125012000
_diffrn_orient_matrix_UB_22      0.0322639000
_diffrn_orient_matrix_UB_23      0.0177641000
_diffrn_orient_matrix_UB_31      -0.0227100000
_diffrn_orient_matrix_UB_32      0.0109464000
_diffrn_orient_matrix_UB_33      -0.0567473000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19319
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.799
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.820
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.908
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         8428
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0369P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5842
_reflns_number_total             8428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02319b2.cif
_cod_data_source_block           Eu-DMAPA1-3
_cod_database_code               7713801
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1Eu1
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.712
_diffrn_oxdiff_digest_frames
;
01abdf40b1725b575e98f0ba33978a39c9002282ccd
;
_diffrn_oxdiff_digest_hkl
;
0129d883aab71872b8a9c201b12bc283d96f51
;
_reflns_odcompleteness_completeness 99.72
_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 C(H,H,H) groups
2. Restrained distances
 H17C-H14
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C21(H21), C22(H22),
 C23(H23)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              8586
_shelx_fab_checksum              11657
_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 2.580
_oxdiff_exptl_absorpt_empirical_full_min 0.645