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_7719603
_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         'C22 H26 Gd N7 O11'
_chemical_formula_sum            'C22 H26 Gd N7 O11'
_chemical_formula_weight         721.75
_chemical_name_systematic        Gd_TEtDAPhen
_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     dual
_audit_creation_date             2025-02-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-12 deposited with the CCDC.	2025-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.412(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5653(10)
_cell_length_b                   17.4897(19)
_cell_length_c                   15.9187(18)
_cell_measurement_reflns_used    9106
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.970
_cell_measurement_theta_min      2.263
_cell_volume                     2646.4(5)
_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 0.971
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56149
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         21.969
_diffrn_reflns_theta_min         2.624
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1224 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.8433.
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    1.811
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6434
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+2.5937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6103
_reflns_number_total             6434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01636c8.cif
_cod_data_source_block           ag_gd_tetdaphen
_cod_depositor_comments
'Adding full bibliography for 7719600--7719609.cif.'
_cod_database_code               7719603
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.542
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19-C015 \\sim C19-C20
 with sigma of 0.02
 C015-H01A \\sim C20-H20A
 with sigma of 0.02
 C015-H01B \\sim C20-H20B
 with sigma of 0.02
 C015-H01C \\sim C20-H20C
 with sigma of 0.02
 C19-H01A \\sim C19-H20A
 with sigma of 0.04
 C19-H01B \\sim C19-H20B
 with sigma of 0.04
 C19-H01C \\sim C19-H20C
 with sigma of 0.04
 H01A-H01B \\sim H20A-H20B
 with sigma of 0.04
 H01A-H01C \\sim H20A-H20C
 with sigma of 0.04
 H01B-H01C \\sim H20B-H20C
 with sigma of 0.04
 C19-N4 \\sim N4-C21
 with sigma of 0.01
 C015-C19 \\sim C19-C20
 with sigma of 0.01
3. Others
 Sof(H19C)=Sof(H19D)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-FVAR(1)
 Sof(H19A)=Sof(H19B)=Sof(C015)=Sof(H01A)=Sof(H01B)=Sof(H01C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C19(H19C,H19D), C21(H21A,H21B), C14(H14A,H14B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C5(H5), C6(H6), C3(H3), C10(H10), C2(H2)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C015(H01A,H01B,
 H01C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'