Combination of chlorinated cobalt dicarbollide with N,O-donor ligands in extraction systems for separating f-elements.
Gerasimov, Mikhail A.; Koifman, Mikhail I.; Lanin, Leonid O.; Prizhilevskaya, Victoria R.; Kalle, Paulina; Yarenkov, Nikita R.; Zhuravleva, Vasilisa A.; Konopkina, Ekaterina A.; Gopin, Alexander V.; Evsiunina, Mariia V.; Borisova, Nataliya E.; Matveev, Petr I.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10327–10342; doi:10.1039/d5dt01136a

data_7718824
_publ_section_title
;
 Combination of chlorinated cobalt dicarbollide with N,O-donor ligands in
 extraction systems for separating f-elements.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10327
_journal_page_last               10342
_journal_paper_doi               10.1039/d5dt01136a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C34 H43 Eu N4 O7, 3(Cl O4)'
_chemical_formula_sum            'C34 H43 Cl3 Eu N4 O19'
_chemical_formula_weight         1070.03
_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             2025-03-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-03-25 deposited with the CCDC.	2025-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                83.2820(10)
_cell_angle_beta                 75.4480(10)
_cell_angle_gamma                86.1790(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6571(2)
_cell_length_b                   14.7256(4)
_cell_length_c                   18.3204(5)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.370
_cell_measurement_theta_min      2.309
_cell_volume                     2502.51(11)
_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      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21287
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_min         1.900
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed X-ray tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1145 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.7391.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         10180
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+2.8449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8769
_reflns_number_total             10180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01136a2.cif
_cod_data_source_block           eu_phen9
_cod_depositor_comments
'Adding full bibliography for 7718820--7718824.cif.'
_cod_database_code               7718824
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.451
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O21-O24
 2.3 with sigma of 0.01
 Cl13-O28
 1.4 with sigma of 0.007
 O8-O28
 2.3 with sigma of 0.01
 O28-O12
 2.3 with sigma of 0.01
 O28-O29
 2.3 with sigma of 0.01
 Cl1-O24
 1.4 with sigma of 0.01
 C20-C26
 2.5 with sigma of 0.02
 C24-C23 = C26-C25
 1.54 with sigma of 0.02
 C37-C32 = C35-C32
 1.5 with sigma of 0.02
 C38-C37 = C35-C36
 1.54 with sigma of 0.02
 C23-C20 = C25-C20
 1.5 with sigma of 0.02
 Cl1-O22
 1.4 with sigma of 0.02
 Cl1-O23
 1.4 with sigma of 0.02
 Cl2-O18
 1.4 with sigma of 0.01
 O12-O29
 2.3 with sigma of 0.01
 Eu1-H4A \\sim Eu1-H4B
 with sigma of 0.02
 Eu1-H5A \\sim Eu1-H5B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26) = Uanis(C24)
Uanis(C23) = Uanis(C25)
Uanis(C37) = Uanis(C35)
Uanis(O19) = Uanis(O18) = Uanis(O20)
4. Rigid body (RIGU) restrains
 O28, Cl13, O29, O12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl1, O22, O23, O24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Cl2, O15, O16, O17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O11, Cl3, O10, O9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: C25(0.4) H25A(0.4) H25B(0.4) C26(0.4) H26A(0.4) H26B(0.4)
 H26C(0.4) C37(0.65) H37A(0.65) H37B(0.65) C38(0.65) H38A(0.65) H38B(0.65)
 H38C(0.65) C23(0.6) H23A(0.6) H23B(0.6) C24(0.6) H24A(0.6) H24B(0.6) H24C(0.6)
 C35(0.35) H35A(0.35) H35B(0.35) C36(0.35) H36A(0.35) H36B(0.35) H36C(0.35)
 O25(0.8) O26(0.8) O27(0.8) O22(0.2) O23(0.2) O24(0.2) O15(0.7) O16(0.7)
 O17(0.7) O18(0.3) O19(0.3) O20(0.3) O9(0.75) Cl3(0.75) O10(0.75) O11(0.75)
 O12(0.25) Cl13(0.25) O28(0.25) O29(0.25)
6.a Free rotating group:
 O4(H4A,H4B), O5(H5A,H5B)
6.b Rotating group:
 O3(H3A,H3B), O6(H6A,H6B), O7(H7A,H7B)
6.c Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C27(H27A,H27B), C25(H25A,H25B), C37(H37A,H37B), C23(H23A,
 H23B), C35(H35A,H35B)
6.d Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C24(H24A,H24B,H24C)
6.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C18(H18), C19(H19),
 C22(H22), C30(H30), C31(H31), C33(H33), C34(H34)
6.f Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C36(H36A,H36B,
 H36C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19012
_shelx_hkl_checksum              80032
_shelx_fab_checksum              35798
_olex2_submission_special_instructions 'No special instructions were received'