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_7718822
_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         'C18 H32 B18 Cl6 Co Cs'
_chemical_formula_sum            'C18 H32 B18 Cl6 Co Cs'
_chemical_formula_weight         847.55
_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                 124.976(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.204(2)
_cell_length_b                   9.0489(7)
_cell_length_c                   17.1607(13)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      78.345
_cell_measurement_theta_min      3.966
_cell_volume                     3461.4(5)
_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 1.5 (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 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20523
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.333
_diffrn_reflns_theta_min         3.966
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_target            Cu
_diffrn_source_type              'fine-focus sealed X-ray tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    16.320
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.4159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1318 before and 0.0739 after correction.
The Ratio of minimum to maximum transmission is 0.5514.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.500
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3639
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0494P)^2^+37.5752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3487
_reflns_number_total             3639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01136a2.cif
_cod_data_source_block           kmi450
_cod_depositor_comments
'Adding full bibliography for 7718820--7718824.cif.'
_cod_database_code               7718822
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9-C3 = C16-C10
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C4)
Uanis(C6) = Uanis(C3)
Uanis(C8) = Uanis(C5)
Uiso(C16) = Uiso(C10)
4. Others
 Fixed Sof: Cl2(0.75) Cl4(0.25) C3(0.75) C4(0.75) H4(0.75) C5(0.75) H5A(0.75)
 C6(0.75) H6A(0.75) C7(0.75) H7(0.75) C8(0.75) H8(0.75) C9(0.75) H9A(0.75)
 H9B(0.75) H9C(0.75) C10(0.25) C11(0.25) H11(0.25) C12(0.25) H12(0.25)
 C13(0.25) H13(0.25) C14(0.25) H14(0.25) C15(0.25) H15(0.25) C16(0.25)
 H16A(0.25) H16B(0.25) H16C(0.25) H3(0.75) H8A(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5A), C6(H6A), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15)
5.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8), C10(C11,C12,C13,C14,C15)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C16(H16A,H16B,H16C)
5.d Boron cage BH refined with riding coordinates:
 C1(H1), C2(H2), B1(H1A), B3(H3), B4(H4A), B5(H5), B6(H6), B8(H8A), B9(H9)
;
_shelx_res_checksum              15917
_shelx_hkl_checksum              95532
_olex2_submission_special_instructions 'No special instructions were received'