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_7718820
_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
'C64 H71 N8 Nd O6, 3(Cl O4), 0.5(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C68 H78 Cl3 N10 Nd O18.5'
_chemical_formula_weight         1581.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-12
_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                 132.839(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.0695(16)
_cell_length_b                   18.5034(10)
_cell_length_c                   19.4547(10)
_cell_measurement_reflns_used    9078
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.494
_cell_measurement_theta_min      2.201
_cell_volume                     7409.2(7)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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  0.0342
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48579
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.590
_diffrn_reflns_theta_min         2.094
_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    0.883
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0805 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.7671.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.382(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         21050
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0531P)^2^+14.7813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1131
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.933
_reflns_Friedel_fraction_max     0.856
_reflns_number_gt                19064
_reflns_number_total             21050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01136a2.cif
_cod_data_source_block           ndd91_2
_cod_depositor_comments
'Adding full bibliography for 7718820--7718824.cif.'
_cod_original_formula_sum        'C68 H78 Cl3 N10 Nd O18.50'
_cod_database_code               7718820
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.618(12)
 0.382(12)
2. 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, All O(H,H) groups
3. Restrained distances
 Cl3-O18
 1.44 with sigma of 0.01
 O2-O18A
 3 with sigma of 0.01
 O18A-O17A
 2.5 with sigma of 0.02
 O18A-O16
 2.5 with sigma of 0.02
 O18A-O15
 2.5 with sigma of 0.02
 O16-O17A
 2.5 with sigma of 0.02
 Cl3A-O18A
 1.43 with sigma of 0.005
 O17A-O15
 2.5 with sigma of 0.02
 Cl3A-O17A = Cl3A-O15 = Cl3A-O16
 1.43 with sigma of 0.01
 Cl3-O17
 1.4 with sigma of 0.01
 C44A-C45A
 1.54 with sigma of 0.02
 C45A-N7A
 2.5 with sigma of 0.02
 C52A-C53A
 1.54 with sigma of 0.02
 O18-O17
 2.5 with sigma of 0.02
 O18-O15
 2.5 with sigma of 0.02
 C32A-C31A \\sim C32-C31
 with sigma of 0.02
 C53-C52 \\sim C52A-C53A
 with sigma of 0.02
 C44A-C45A \\sim C45-C44
 with sigma of 0.02
 C52A-C49 \\sim C52-C49
 with sigma of 0.02
 Cl2-O13A \\sim Cl2-O13 \\sim Cl2-O14 \\sim Cl2-O14A
 with sigma of 0.02
 N7-C44 \\sim N7A-C44A
 with sigma of 0.02
 N7-C43 \\sim N7A-C43
 with sigma of 0.02
 N7-C46 \\sim N7A-C46
 with sigma of 0.02
 Nd1-H5A \\sim Nd1-H5B
 with sigma of 0.02
 Nd1-H6A \\sim Nd1-H6B
 with sigma of 0.02
 C28-C31A \\sim C28-C31
 with sigma of 0.02
 C56-C55 \\sim C56A-C55
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C53) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.05
Uiso(O18A) = Uiso(O18)
Uiso(Cl3A) = Uiso(O17A)
5. Rigid body (RIGU) restrains
 C52, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C31
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C55, C56, C56A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: N7(0.75) N7A(0.25) C31(0.65) H31A(0.65) H31B(0.65) C31A(0.35)
 H31C(0.35) H31D(0.35) C32(0.65) H32A(0.65) H32B(0.65) H32C(0.65) C32A(0.35)
 H32D(0.35) H32E(0.35) H32F(0.35) C44(0.75) H44A(0.75) H44B(0.75) C44A(0.25)
 H44C(0.25) H44D(0.25) C45(0.75) H45A(0.75) H45B(0.75) H45C(0.75) C45A(0.25)
 H45D(0.25) H45E(0.25) H45F(0.25) C52(0.55) H52A(0.55) H52B(0.55) C52A(0.45)
 H52C(0.45) H52D(0.45) C53(0.55) H53A(0.55) H53B(0.55) H53C(0.55) C53A(0.45)
 H53D(0.45) H53E(0.45) H53F(0.45) H55C(0.25) H55D(0.25) H55A(0.75) H55B(0.75)
 C56(0.75) H56A(0.75) H56B(0.75) H56C(0.75) C56A(0.25) H56D(0.25) H56E(0.25)
 H56F(0.25) O13(0.6) O13A(0.4) O14(0.6) O14A(0.4) Cl3(0.65) Cl3A(0.35)
 O17(0.65) O17A(0.35) O18(0.65) O18A(0.35) O19(0.5) H19A(0.5) H19B(0.5)
 N10(0.75) C67(0.75) C68(0.75) H68A(0.75) H68B(0.75) H68C(0.75) N11(0.25)
 C69(0.25) C70(0.25) H70A(0.25) H70B(0.25) H70C(0.25)
 Fixed Uiso: C32A(0.05578) C45A(0.05822)
7.a Riding coordinates:
 O19(H19A,H19B), C68(H68A,H68B,H68C)
7.b Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
7.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C20(H20A,H20B), C23(H23A,H23B), C31(H31A,H31B), C31A(H31C,
 H31D), C44(H44A,H44B), C44A(H44C,H44D), C52(H52A,H52B), C52A(H52C,H52D),
 C55(H55C,H55D), C55(H55A,H55B), C63(H63A,H63B)
7.d Me refined with riding coordinates:
 C32A(H32D,H32E,H32F), C53(H53A,H53B,H53C), C56A(H56D,H56E,H56F)
7.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16), C18(H18),
 C19(H19), C26(H26), C27(H27), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36),
  C39(H39), C40(H40), C41(H41), C48(H48), C50(H50), C51(H51), C58(H58),
 C59(H59), C61(H61), C62(H62)
7.f Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C32(H32A,H32B,
 H32C), C45(H45A,H45B,H45C), C45A(H45D,H45E,H45F), C53A(H53D,H53E,H53F),
 C56(H56A,H56B,H56C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C70(H70A,H70B,
 H70C)
;
_shelx_res_checksum              52172
_shelx_hkl_checksum              42275
_olex2_submission_special_instructions 'No special instructions were received'