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_7718812
_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         'C110 H160 B3 O2 U'
_chemical_formula_sum            'C110 H160 B3 O2 U'
_chemical_formula_weight         1784.83
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-05-06
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7221)
;
_audit_update_record
;
2025-05-07 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4250(5)
_cell_length_b                   30.4588(11)
_cell_length_c                   23.2285(8)
_cell_measurement_reflns_used    5822
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.298
_cell_measurement_theta_min      3.105
_cell_volume                     10145.5(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE DUO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            341079
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.318
_diffrn_reflns_theta_min         1.951
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  0.7231
_exptl_absorpt_correction_T_min  0.6921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0681 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.9299.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             3772
_exptl_crystal_preparation       'Salt metathesis'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.682
_refine_diff_density_min         -2.379
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1115
_refine_ls_number_reflns         25217
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+13.3462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21983
_reflns_number_total             25217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01076d2.cif
_cod_data_source_block           dal24_54
_cod_depositor_comments
'Adding full bibliography for 7718809--7718812.cif.'
_cod_database_code               7718812
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.715
_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 B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C66-C72 \\sim C66-C71
 with sigma of 0.02
 C66-C68 \\sim C66-C67
 with sigma of 0.02
 C66-C70 \\sim C66-C69
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C71, C72, C70, C69, C66, C67, C68
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=1-FVAR(1)
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C109(H10A,H10B), C112(H11A,H11B), C111(H11C,H11D), C114(H11E,H11F), C116(H11G,
 H11H), C113(H11I,H11J), C115(H11K,H11L), C110(H11M,H11N)
5.b Aromatic/amide H refined with riding coordinates:
 C98(H98), C26(H26), C57(H57), C45(H45), C81(H81), C58(H58), C12(H12),
 C37(H37), C76(H76), C8(H8), C85(H85), C94(H94), C77(H77), C78(H78), C83(H83),
 C24(H24), C5(H5), C22(H22), C60(H60), C38(H38), C97(H97), C10(H10), C39(H39),
 C47(H47), C43(H43), C3(H3), C4(H4)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), B3(H3A,H3B,H3C), C20(H20A,H20B,H20C), C16(H16A,H16B,
 H16C), B1(H1A,H1B,H1C), C34(H34A,H34B,H34C), B2(H2A,H2B,H2C), C65(H65A,H65B,
 H65C), C54(H54A,H54B,H54C), C19(H19A,H19B,H19C), C55(H55A,H55B,H55C), C53(H53A,
 H53B,H53C), C15(H15A,H15B,H15C), C49(H49A,H49B,H49C), C91(H91A,H91B,H91C),
 C63(H63A,H63B,H63C), C88(H88A,H88B,H88C), C106(H10C,H10D,H10E), C14(H14A,H14B,
 H14C), C33(H33A,H33B,H33C), C93(H93A,H93B,H93C), C32(H32A,H32B,H32C), C28(H28A,
 H28B,H28C), C102(H10F,H10G,H10H), C92(H92A,H92B,H92C), C108(H10I,H10J,H10K),
 C64(H64A,H64B,H64C), C103(H10L,H10M,H10N), C107(H10O,H10P,H10Q), C87(H87A,H87B,
 H87C), C101(H10R,H10S,H10T), C50(H50A,H50B,H50C), C30(H30A,H30B,H30C),
 C51(H51A,H51B,H51C), C29(H29A,H29B,H29C), C89(H89A,H89B,H89C), C72(H72A,H72B,
 H72C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C67(H67A,H67B,H67C), C69(H69A,
 H69B,H69C), C71(H71A,H71B,H71C)
;
_shelx_res_checksum              33250
_shelx_hkl_checksum              92303
_olex2_submission_special_instructions 'No special instructions were received'