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_7718821
_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         'C32 H34 Cl3 N4 Nd O14'
_chemical_formula_sum            'C32 H34 Cl3 N4 Nd O14'
_chemical_formula_weight         949.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-12 deposited with the CCDC.	2025-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.658(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8218(8)
_cell_length_b                   11.6485(7)
_cell_length_c                   24.5579(15)
_cell_measurement_reflns_used    8677
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.430
_cell_measurement_theta_min      2.362
_cell_volume                     3666.3(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 0.998
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            16975
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.561
_diffrn_reflns_theta_min         2.363
_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    1.708
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0978 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.7345.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.268
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5604
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0107P)^2^+22.3295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4888
_reflns_number_total             5604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01136a2.cif
_cod_data_source_block           gma424
_cod_depositor_comments
'Adding full bibliography for 7718820--7718824.cif.'
_cod_database_code               7718821
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.772
_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
2. Restrained distances
 Cl2-O8 \\sim Cl2-O7
 with sigma of 0.02
3. Others
 Fixed Sof: Cl2(0.5) O7(0.5) O8(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              47481
_shelx_hkl_checksum              84888
_olex2_submission_special_instructions 'No special instructions were received'