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_7131262
_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         'C54 H50 B2 Eu N12 O2 P2'
_chemical_formula_sum            'C54 H50 B2 Eu N12 O2 P2'
_chemical_formula_weight         1134.58
_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
_audit_creation_date             2022-03-11
_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                74.834(4)
_cell_angle_beta                 89.184(4)
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_cell_formula_units_Z            4
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_cell_length_b                   22.587(3)
_cell_length_c                   23.443(3)
_cell_measurement_reflns_used    6172
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.317
_cell_measurement_theta_min      2.252
_cell_volume                     6229.9(14)
_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)'
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_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 0.984
_diffrn_measured_fraction_theta_max 0.979
_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  0.2120
_diffrn_reflns_av_unetI/netI     0.2354
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            91857
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.453
_diffrn_reflns_theta_min         1.127
_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
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_exptl_absorpt_correction_T_min  0.5936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1421 before and 0.0829 after correction.
The Ratio of minimum to maximum transmission is 0.7964.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.282
_refine_diff_density_min         -1.464
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1315
_refine_ls_number_reflns         25181
_refine_ls_number_restraints     1348
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1782
_refine_ls_R_factor_gt           0.0914
_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^)+(0.0846P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.2154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13263
_reflns_number_total             25181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03189b2.cif
_cod_data_source_block           1_Eu_Ph3PO
_cod_depositor_comments
'Adding full bibliography for 7131257--7131266.cif.'
_cod_original_cell_volume        6230.0(14)
_cod_database_code               7131262
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.818
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 B1(H1A), B2(H2A), B3(H3A), B4(H4A)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C23(H23), C11(H11), C44(H44), C2(H2), C48(H48), C51(H51), C33(H33),
 C45(H45), C28(H28), C32(H32), C18(H18), C8(H8), C3(H3), C53(H53), C27(H27),
 C7(H7), C30(H30), C6(H6), C26(H26), C15(H15), C13(H13), C21(H21), C1(H1),
 C22(H22), C36(H36), C20(H20), C12(H12), C38(H38), C17(H17), C54(H54), C47(H47),
  C24(H24), C35(H35), C34(H34), C39(H39), C29(H29), C14(H14), C9(H9), C42(H42),
 C46(H46), C52(H52), C4(H4), C41(H41), C40(H40), C16(H16), C5(H5), C50(H50),
 C76(H76), C57(H57), C99(H99), C77(H77), C62(H62), C88(H88), C78(H78), C92(H92),
  C61(H61), C58(H58), C83(H83), C60(H60), C74(H74), C94(H94), C90(H90),
 C104(H104), C64(H64), C105(H105), C84(H84), C93(H93), C67(H67), C87(H87),
 C55(H55), C89(H89), C98(H98), C95(H95), C70(H70), C59(H59), C68(H68), C66(H66),
  C81(H81), C106(H106), C56(H56), C82(H82), C101(H101), C100(H100), C107(H107),
 C96(H96), C72(H72), C108(H108), C75(H75), C80(H80), C71(H71), C69(H69),
 C86(H86), C102(H102), C63(H63), C65(H65)
;
_shelx_res_checksum              60738
_shelx_hkl_checksum              19158
_shelx_fab_checksum              82706
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'