Synthesis of bulky hydride ligands: <i>m</i>-terphenylborohydride complexes with trivalent uranium and neodymium.
Zacher, 3rd, Peter A; Unruh, Daniel K.; Daly, Scott R.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9135–9139; doi:10.1039/d5dt01076d

data_7718809
_publ_section_title
;
 Synthesis of bulky hydride ligands: <i>m</i>-terphenylborohydride
 complexes with trivalent uranium and neodymium.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9135
_journal_page_last               9139
_journal_paper_doi               10.1039/d5dt01076d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C68 H96 B2 Li2, 1[C6H14], 0.5[C6H14]'
_chemical_formula_sum            'C77 H117 B2 Li2'
_chemical_formula_weight         1078.20
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2025-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                94.734(2)
_cell_angle_beta                 95.397(2)
_cell_angle_gamma                108.591(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6910(6)
_cell_length_b                   13.2184(8)
_cell_length_c                   27.5291(15)
_cell_measurement_reflns_used    2341
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.374
_cell_measurement_theta_min      2.556
_cell_volume                     3644.8(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture DUO with Photon 3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            90201
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.377
_diffrn_reflns_theta_min         1.879
_exptl_absorpt_coefficient_mu    0.054
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6883
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0770 before and 0.0484 after correction.
The Ratio of minimum to maximum transmission is 0.9230.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.982
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         18108
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0556P)^2^+2.2148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13465
_reflns_number_total             18108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01076d2.cif
_cod_data_source_block           dal_24_52
_cod_depositor_comments
'Adding full bibliography for 7718809--7718812.cif.'
_cod_database_code               7718809
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C61-C64 \\sim C61-C64A
 with sigma of 0.02
 C61-C62 \\sim C61-C62A
 with sigma of 0.02
 C61-C63 \\sim C61-C63A
 with sigma of 0.02
 C47-C49 \\sim C47-C49A
 with sigma of 0.02
 C47-C48 \\sim C47-C48A
 with sigma of 0.02
 C47-C50 \\sim C47-C50A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C64 \\sim C64A \\sim C63 \\sim C63A \\sim C62A \\sim C62: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C61, C63, C63A, C64, C64A, C62, C62A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C64A)=Sof(H64D)=Sof(H64E)=Sof(H64F)=Sof(C63A)=Sof(H63D)=Sof(H63E)=
 Sof(H63F)=Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(1)
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(1)
 Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49A)=Sof(H49D)=Sof(H49E)=
 Sof(H49F)=Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(2)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C12(H12), C22(H22), C24(H24),
 C26(H26), C33(H33), C34(H34), C35(H35), C38(H38), C40(H40), C42(H42), C52(H52),
  C54(H54), C56(H56)
6.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), B1(H1A,
 H1B,H1C), B2(H2A,H2B,H2C), C64(H64A,H64B,H64C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C64A(H64D,H64E,H64F), C63A(H63D,H63E,H63F), C62A(H62D,H62E,H62F),
 C49(H49A,H49B,H49C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C48A(H48D,H48E,
 H48F), C49A(H49D,H49E,H49F), C50A(H50D,H50E,H50F)
;
_shelx_res_checksum              78963
_shelx_hkl_checksum              1934
_shelx_fab_checksum              20239
_olex2_exptl_crystal_mounting_method 'MiTeGen 100 micron MicroLoop'
_olex2_submission_special_instructions 'No special instructions were received'