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_7713802
_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 N6 O9 Am'
_chemical_formula_sum            'C27 H27 Am N6 O9'
_chemical_formula_weight         820.61
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-09-29
_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                 109.682(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7061(12)
_cell_length_b                   19.4040(10)
_cell_length_c                   12.2732(9)
_cell_measurement_reflns_used    12523
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8960
_cell_measurement_theta_min      3.4950
_cell_volume                     3297.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.794
_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    -19.00  38.00   0.50    2.00    --    4.33 -99.00-120.00  114
  2  \w     49.00  78.00   0.50    2.00    --    4.33  37.00-180.00   58
  3  \w     43.00  79.00   0.50    2.00    --    4.33  29.00-134.00   72
  4  \w     -7.00  28.00   0.50    2.00    --    4.33  29.00-134.00   70
  5  \w    -42.00  14.00   0.50    2.00    --    4.33 -29.00  64.00  112
  6  \w    -29.00   2.00   0.50    2.00    --   -5.89 -37.00  30.00   62
  7  \w    -20.00  25.00   0.50    2.00    --   -5.89 -99.00  30.00   90
  8  \w    -74.00 -49.00   0.50    2.00    --   -5.89 -37.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0373800000
_diffrn_orient_matrix_UB_12      -0.0116106000
_diffrn_orient_matrix_UB_13      0.0501255000
_diffrn_orient_matrix_UB_21      -0.0289645000
_diffrn_orient_matrix_UB_22      0.0079818000
_diffrn_orient_matrix_UB_23      0.0342566000
_diffrn_orient_matrix_UB_31      -0.0197918000
_diffrn_orient_matrix_UB_32      -0.0336923000
_diffrn_orient_matrix_UB_33      -0.0091679000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34461
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.893
_diffrn_reflns_theta_min         3.332
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.752
_refine_diff_density_min         -2.230
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         8262
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0497
_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/[\s^2^(Fo^2^)+(0.0667P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5407
_reflns_number_total             8262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02319b2.cif
_cod_data_source_block           202209Am-DMAPA1-3
_cod_original_formula_sum        'C27 H27 N6 O9 Am'
_cod_database_code               7713802
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1OAm1
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.941
_diffrn_oxdiff_digest_frames
;
01970f8ea99cd45ba3f5b38967cbf6369100628fdea
;
_diffrn_oxdiff_digest_hkl
;
01b8a74f37555ff2258b8962b6bd4b7537fb71
;
_reflns_odcompleteness_completeness 99.63
_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. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.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)
3.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              55737
_shelx_fab_checksum              99098
_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 1.707
_oxdiff_exptl_absorpt_empirical_full_min 0.744