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_7131260
_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 H35 B2 N12 O P Yb'
_chemical_formula_sum            'C36 H35 B2 N12 O P Yb'
_chemical_formula_weight         877.39
_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             2022-03-08
_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                73.4450(10)
_cell_angle_beta                 83.8410(10)
_cell_angle_gamma                65.6540(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7840(4)
_cell_length_b                   12.0768(4)
_cell_length_c                   14.8349(5)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.14
_cell_measurement_theta_min      2.39
_cell_volume                     1843.60(11)
_computing_cell_refinement       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0983
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52538
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.290
_diffrn_reflns_theta_min         1.897
_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    2.628
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1098 before and 0.0753 after correction.
The Ratio of minimum to maximum transmission is 0.8734.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       rod
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         9157
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0340P)^2^+0.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7065
_reflns_number_total             9157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03189b2.cif
_cod_data_source_block           1_Yb_Ph3PO
_cod_depositor_comments
'Adding full bibliography for 7131257--7131266.cif.'
_cod_database_code               7131260
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.571
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2. Restrained distances
 C32-C31 = C32A-C31 = C33-C32 = C33A-C32A = C34-C33 = C34-C33A = C35A-C34 =
 C35-C34 = C36A-C35A = C36-C35 = C36A-C31 = C36-C31
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C32 \\sim C32A \\sim C33 \\sim C33A \\sim C35A \\sim C35 \\sim C36A \\sim C36:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
4. Others
 Sof(H34A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36A)=1-FVAR(1)
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=
 Sof(H36)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34A),
 C34(H34), C35(H35), C36(H36), C32A(H32A), C33A(H33A), C35A(H35A), C36A(H36A)
;
_shelx_res_checksum              77047
_shelx_hkl_checksum              84114
_olex2_submission_special_instructions 'No special instructions were received'