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_7719602
_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 N7 O11 Sm'
_chemical_formula_sum            'C22 H26 N7 O11 Sm'
_chemical_formula_weight         714.85
_chemical_name_systematic        Sm_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             2025-01-28
_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                 96.539(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5877(7)
_cell_length_b                   17.4923(13)
_cell_length_c                   15.9192(12)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.981
_cell_measurement_theta_min      2.231
_cell_volume                     2652.5(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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            48428
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         21.999
_diffrn_reflns_theta_min         2.495
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  0.7426
_exptl_absorpt_correction_T_min  0.6835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1174 before and 0.0822 after correction.
The Ratio of minimum to maximum transmission is 0.9204.
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    1.790
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.138
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6595
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0273P)^2^+2.5473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6069
_reflns_number_total             6595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01636c8.cif
_cod_data_source_block           ag_sm_tetdaphen
_cod_depositor_comments
'Adding full bibliography for 7719600--7719609.cif.'
_cod_database_code               7719602
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.737
_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
 C00W-C016 \\sim C00W-C0
 with sigma of 0.02
 C016-H01N \\sim C0-H0A
 with sigma of 0.02
 C016-H01O \\sim C0-H0B
 with sigma of 0.02
 C016-H01P \\sim C0-H0C
 with sigma of 0.02
 C00W-H01N \\sim C00W-H0A
 with sigma of 0.04
 C00W-H01O \\sim C00W-H0B
 with sigma of 0.04
 C00W-H01P \\sim C00W-H0C
 with sigma of 0.04
 H01N-H01O \\sim H0A-H0B
 with sigma of 0.04
 H01N-H01P \\sim H0A-H0C
 with sigma of 0.04
 H01O-H01P \\sim H0B-H0C
 with sigma of 0.04
3. Others
 Sof(H00C)=Sof(H00D)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(H0C)=1-FVAR(1)
 Sof(H00A)=Sof(H00B)=Sof(C016)=Sof(H01N)=Sof(H01O)=Sof(H01P)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C00W(H00A,H00B), C00W(H00C,H00D), C00Z(H00E,H00F), C010(H01A,H01B), C012(H01F,
 H01G)
4.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00N(H00N), C00O(H00O), C00S(H00S), C00V(H00V), C00Y(H00Y)
4.c Idealised Me refined as rotating group:
 C011(H01C,H01D,H01E), C013(H01H,H01I,H01J), C014(H01K,H01L,H01M), C016(H01N,
 H01O,H01P), C0(H0A,H0B,H0C)
;
_olex2_submission_special_instructions 'No special instructions were received'