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_7718823
_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 H34 Eu N7 O11, C7 H4 F3 N O2'
_chemical_formula_sum            'C41 H38 Eu F3 N8 O13'
_chemical_formula_weight         1059.75
_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   geom
_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                 102.3910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4141(3)
_cell_length_b                   32.4906(13)
_cell_length_c                   16.5009(7)
_cell_measurement_reflns_used    9306
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.448
_cell_measurement_theta_min      2.557
_cell_volume                     4405.9(3)
_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      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37200
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.573
_diffrn_reflns_theta_min         2.507
_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    1.510
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1353 before and 0.0445 after correction.
The Ratio of minimum to maximum transmission is 0.8238.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       plate
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.692
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 5387 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         13328
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0113P)^2^+5.5037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                12215
_reflns_number_total             13328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01136a2.cif
_cod_data_source_block           gma439
_cod_depositor_comments
'Adding full bibliography for 7718820--7718824.cif.'
_cod_database_code               7718823
_shelx_shelxl_version_number     2018/3
_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
 N9-C44
 1.43 with sigma of 0.015
 C36-C35 \\sim C42-C35
 with sigma of 0.01
 O16-N9 \\sim O14-N8
 with sigma of 0.02
 O15-N9 \\sim O13-N8
 with sigma of 0.02
 O11-N7 \\sim O12-N7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N9 \\sim C44: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
N8 \\sim C38: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C36) = Uanis(C42)
Uanis(C43) = Uanis(C37)
Uanis(O11) = Uanis(O12)
Uanis(O14) = Uanis(O16)
4. Rigid body (RIGU) restrains
 O15, O16, N9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C47, C46, C45, C44, C43, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O11(0.4) O12(0.6) O13(0.6) O14(0.6) O15(0.4) O16(0.4) N8(0.6)
 N9(0.4) C36(0.6) C37(0.6) H37(0.6) C38(0.6) C39(0.6) H39(0.6) C40(0.6)
 H40(0.6) C41(0.6) H41(0.6) C42(0.4) C43(0.4) H43(0.4) C44(0.4) C45(0.4)
 H45(0.4) C46(0.4) H46(0.4) C47(0.4) H47(0.4)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C31(H31A,H31B), C33(H33A,H33B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C16(H16), C17(H17),
 C19(H19), C20(H20), C26(H26), C27(H27), C29(H29), C30(H30), C37(H37), C39(H39),
  C40(H40), C41(H41), C43(H43), C45(H45), C46(H46), C47(H47)
6.c Fitted hexagon refined as free rotating group:
 C36(C37,C38,C39,C40,C41), C42(C43,C44,C45,C46,C47)
6.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C)
;
_shelx_res_checksum              21003
_shelx_hkl_checksum              97638
_olex2_submission_special_instructions 'No special instructions were received'