Rigidified cyclic diglycolamides: coordination and extraction of trivalent f-elements.
Evsiunina, Mariia V.; Kalinin, Mikhail A.; Kalle, Paulina; Iakovlev, Danila A.; Kalmykov, Stepan N.; Matveev, Petr I.; Borisova, Nataliya E.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4638–4656; doi:10.1039/d6dt00275g

data_7720393
_publ_section_title
;
 Rigidified cyclic diglycolamides: coordination and extraction of
 trivalent f-elements.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4638
_journal_page_last               4656
_journal_paper_doi               10.1039/d6dt00275g
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety
'2(C20 H36 La N6 O15), C40 H76 La N5 O11, C H Cl3, 1.8(C2 H3 N)'
_chemical_formula_sum            'C84.6 H154.4 Cl3 La3 N18.8 O41'
_chemical_formula_weight         2614.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-05-01 deposited with the CCDC.	2026-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                69.345(2)
_cell_angle_beta                 66.660(2)
_cell_angle_gamma                85.478(2)
_cell_formula_units_Z            2
_cell_length_a                   17.6599(9)
_cell_length_b                   19.3252(13)
_cell_length_c                   19.5497(10)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    230
_cell_measurement_theta_max      28.855
_cell_measurement_theta_min      2.258
_cell_volume                     5717.8(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      230
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART Photon II'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61554
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.537
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed X-ray tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0768 before and 0.0590 after correction.
The Ratio of minimum to maximum transmission is 0.7557.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             2687
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1389
_refine_ls_number_reflns         22428
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0408P)^2^+1.4115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16861
_reflns_number_total             22428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00275g2.cif
_cod_data_source_block           2198
_cod_depositor_comments          'Adding full bibliography for 7720393.cif.'
_cod_original_formula_sum        'C84.60 H154.40 Cl3 La3 N18.80 O41'
_cod_database_code               7720393
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.744
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 La3-H41A \\sim La3-H41B
 with sigma of 0.02
 La3-H40A \\sim La3-H40B
 with sigma of 0.02
 C55-C56 \\sim C57-C56
 with sigma of 0.02
 C55-C54 \\sim C57-C54
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C55) = Uanis(C57)
4. Others
 Fixed Sof: H54A(0.75) H54B(0.75) H54C(0.25) H54D(0.25) C55(0.75) H55A(0.75)
 H55B(0.75) H56A(0.75) H56B(0.75) H56C(0.25) H56D(0.25) C57(0.25) H57A(0.25)
 H57B(0.25) N19(0.3) N20(0.5) C82(0.5) C83(0.8) H83A(0.5) H83B(0.5) H83C(0.5)
 H83D(0.3) H83E(0.3) H83F(0.3) C84(0.3)
5.a Free rotating group:
 O40(H40A,H40B), O41(H41A,H41B)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,
 H38B), C40(H40C,H40D), C41(H41C,H41D), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
  C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C54(H54C,H54D), C55(H55A,H55B), C56(H56A,H56B),
 C56(H56C,H56D), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B), C62(H62A,H62B),
  C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
 C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B),
  C77(H77A,H77B), C79(H79A,H79B), C81(H81A,H81B)
;
_shelx_res_checksum              13137
_olex2_submission_special_instructions 'No special instructions were received'