Reduction chemistry yields stable and soluble divalent lanthanide tris(pyrazolyl)borate complexes.
Chowdhury, Tajrian; Evans, Matthew J.; Coles, Martyn P.; Bailey, Anna G.; Peveler, William J.; Wilson, Claire; Farnaby, Joy H.; Chemical communications (Cambridge, England) 59 (2023) 2134–2137; doi:10.1039/d2cc03189b

data_7131257
_publ_section_title
;
 Reduction chemistry yields stable and soluble divalent lanthanide
 tris(pyrazolyl)borate complexes.
;
_journal_issue                   15
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2134
_journal_page_last               2137
_journal_paper_doi               10.1039/d2cc03189b
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C36 H40 B4 Eu2 N24, 3(C7 H8)'
_chemical_formula_sum            'C57 H64 B4 Eu2 N24'
_chemical_formula_weight         1432.48
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-03-22 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                81.9420(10)
_cell_angle_beta                 68.6710(10)
_cell_angle_gamma                73.7510(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8751(4)
_cell_length_b                   12.1292(5)
_cell_length_c                   13.2669(4)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.36
_cell_volume                     1563.57(10)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_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_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27534
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.264
_diffrn_reflns_theta_min         2.075
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.046
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0832 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.8957.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       tablet
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7742
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0269P)^2^+2.7950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6832
_reflns_number_total             7742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03189b2.cif
_cod_data_source_block           1_Eu
_cod_depositor_comments
'Adding full bibliography for 7131257--7131266.cif.'
_cod_database_code               7131257
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.777
_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
 C30-C28
 1.51 with sigma of 0.02
 C20-C19 = C24-C19 = C24-C23 = C23-C22 = C22-C21 = C21-C20 = C29-C27 = C30-C29
 = C30-C26_$1 = C27_$1-C26_$1 = C28_$1-C27_$1 = C28_$1-C27
 1.39 with sigma of 0.02
 C25-C19
 1.51 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C30 \\sim C26 \\sim C27 \\sim C28 \\sim C30 \\sim C28 \\sim C29 \\sim C27 \\sim
C29 \\sim C26: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
4. Others
 Fixed Sof: C26(0.5) C28(0.5) C29(0.5)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), B1(H1A), B2(H2A)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              5185
_shelx_hkl_checksum              85184
_olex2_submission_special_instructions 'No special instructions were received'