Unveiling the interplay: comparing solvent extraction, structure, and stability constants in a phenanthroline diamide system with trivalent lanthanides.
Archer, Emma M.; Vigil, Correy R.; Galley, Shane S.; Jackson, Jessica A.; Shafer, Jenifer C.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16086–16094; doi:10.1039/d5dt01636c

data_7719609
_publ_section_title
;
 Unveiling the interplay: comparing solvent extraction, structure, and
 stability constants in a phenanthroline diamide system with trivalent
 lanthanides.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16086
_journal_page_last               16094
_journal_paper_doi               10.1039/d5dt01636c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '0.5(C44 H52 La N11 O13), C2 H3 N'
_chemical_formula_sum            'C24 H29 La0.5 N6.5 O6.5'
_chemical_formula_weight         581.99
_chemical_name_systematic        LaTEtDAPhen
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-13 deposited with the CCDC.	2025-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.248(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.5844(8)
_cell_length_b                   20.8564(15)
_cell_length_c                   20.0610(14)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.000
_cell_measurement_theta_min      2.211
_cell_volume                     5210.9(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            131723
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         22.337
_diffrn_reflns_theta_min         2.429
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.6666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1301 before and 0.0899 after correction.
The Ratio of minimum to maximum transmission is 0.8950.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       prism
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.511
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.469(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1392
_refine_ls_number_reflns         26970
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0306P)^2^+1.0676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                25728
_reflns_number_total             26970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01636c8.cif
_cod_data_source_block           ag_la_tetdaphen_3
_cod_depositor_comments
'Adding full bibliography for 7719600--7719609.cif.'
_cod_original_formula_sum        'C24 H29 La0.50 N6.50 O6.50'
_cod_database_code               7719609
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.531(14)
 0.469(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H03D,H03E,H03F} of C039, {H35A,H35B,H35C} of C35, {H3AA,
  H3AB,H3AC} of C3A, All C(H,H) groups
 At 1.5 times of:
  {H10A,H10B,H10C} of C10B, {H86A,H86B,H86C} of C86, {H19A,H19B,H19C} of C19,
  {H63A,H63B,H63C} of C63, {H60A,H60B,H60C} of C60, {H50A,H50B,H50C} of C50,
  {H21A,H21B,H21C} of C21, {H65A,H65B,H65C} of C65, {H42A,H42B,H42C} of C42,
  {H37A,H37B,H37C} of C37, {H84A,H84B,H84C} of C84, {H16A,H16B,H16C} of C16,
  {H79A,H79B,H79C} of C79, {H81A,H81B,H81C} of C81, {H44A,H44B,H44C} of C44,
  {H39A,H39B,H39C} of C39, {H03A,H03B,H03C} of C03R, {H58A,H58B,H58C} of C58
3. Others
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(H10C)=1-FVAR(1)
 Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=Sof(C85)=Sof(H85A)=Sof(H85B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C38(H38A,H38B), C57(H57A,H57B), C59(H59A,
 H59B), C36(H36A,H36B), C80(H80A,H80B), C78(H78A,H78B), C64(H64A,H64B),
 C18(H18A,H18B), C62(H62A,H62B), C20(H20A,H20B), C43(H43A,H43B), C41(H41A,H41B),
  C83(H83A,H83B), C85(H85A,H85B), C8B(H8BA,H8BB)
4.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C10(H10), C5(H5), C70(H70), C14(H14), C23(H23), C2(H2), C47(H47),
 C24(H24), C6(H6), C3(H3), C27(H27), C53(H53), C67(H67), C68(H68), C71(H71),
 C46(H46), C54(H54), C26(H26), C31(H31), C9(H9), C32(H32), C76(H76), C75(H75)
4.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C65(H65A,H65B,H65C), C19(H19A,H19B,H19C), C50(H50A,H50B,
 H50C), C039(H03D,H03E,H03F), C63(H63A,H63B,H63C), C60(H60A,H60B,H60C),
 C21(H21A,H21B,H21C), C42(H42A,H42B,H42C), C16(H16A,H16B,H16C), C79(H79A,H79B,
 H79C), C37(H37A,H37B,H37C), C03R(H03A,H03B,H03C), C44(H44A,H44B,H44C),
 C81(H81A,H81B,H81C), C39(H39A,H39B,H39C), C84(H84A,H84B,H84C), C35(H35A,H35B,
 H35C), C3A(H3AA,H3AB,H3AC), C86(H86A,H86B,H86C), C10B(H10A,H10B,H10C)
;
_olex2_submission_original_sample_id LaTEtDAPhen
_olex2_submission_special_instructions 'No special instructions were received'