Soft-donor dipicolinamide derivatives for selective actinide(III) / lanthanide(III) separation: The role of S- vs. O-donor sites
Lehman-Andino, Ingrid; Su, Jing; Papathanasiou, Konstantinos E.; Eaton, Teresa M.; Jian, Jiwen; Dan, David; Albrecht-Schmitt, Thomas; Dares, Christopher; Batista, Enrique R.; Yang, Ping; Gibson, John K.; Kavallieratos, Konstantinos; Chemical Communications  (2019) –; doi:10.1039/C8CC07683A

data_7122909
_publ_section_title
;
 Soft-donor dipicolinamide derivatives for selective actinide(III) /
 lanthanide(III) separation: The role of S- vs. O-donor sites
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC07683A
_journal_year                    2019
_chemical_formula_moiety         'C81 H93 N9 Nd O6, 3(I), 3(C2 H3 N)'
_chemical_formula_sum            'C87 H102 I3 N12 Nd O6'
_chemical_formula_weight         1936.74
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-01-22 deposited with the CCDC.
2019-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.127(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.754(3)
_cell_length_b                   18.809(3)
_cell_length_c                   25.655(4)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.37
_cell_volume                     8601(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            132485
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.645
_diffrn_reflns_theta_min         2.285
_exptl_absorpt_coefficient_mu    1.739
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       Needles
_exptl_crystal_F_000             3900
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_exptl_crystal_size_min          0.07
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_refine_diff_density_min         -2.769
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         19947
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.305
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+59.9442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17205
_reflns_number_total             19947
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07683a2.cif
_cod_data_source_block           cjw2Nd(3)3
_cod_original_cell_volume        8600(2)
_cod_database_code               7122909
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              2673