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_7718811
_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 Nd O2'
_chemical_formula_sum            'C110 H160 B3 Nd O2'
_chemical_formula_weight         1691.04
_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                 96.375(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4185(6)
_cell_length_b                   30.3781(12)
_cell_length_c                   23.2224(11)
_cell_measurement_reflns_used    9214
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.413
_cell_measurement_theta_min      2.216
_cell_volume                     10108.7(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE DUO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            271583
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.429
_diffrn_reflns_theta_min         1.888
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0945 before and 0.0488 after correction.
The Ratio of minimum to maximum transmission is 0.9575.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_description       plate
_exptl_crystal_F_000             3644
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.500
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1115
_refine_ls_number_reflns         20738
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0236P)^2^+12.3549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19592
_reflns_number_total             20738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01076d2.cif
_cod_data_source_block           mo_dal24_82
_cod_depositor_comments
'Adding full bibliography for 7718809--7718812.cif.'
_cod_database_code               7718811
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.856
_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
 C51-C56 \\sim C51-C57
 with sigma of 0.02
 C51-C54 \\sim C51-C55
 with sigma of 0.02
 C51-C52 \\sim C51-C53
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C53, C54, C51, C55, C56, C57, C52
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=1-FVAR(1)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C107(H10A,H10B), C106(H10C,H10D), C113(H11A,H11B), C112(H11C,H11D), C109(H10E,
 H10F), C108(H10G,H10H), C110(H11E,H11F), C111(H11G,H11H)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C43(H43), C42(H42), C23(H23), C94(H94), C5(H5), C80(H80), C59(H59),
 C8(H8), C93(H93), C39(H39), C3(H3), C79(H79), C22(H22), C4(H4), C63(H63),
 C12(H12), C97(H97), C37(H37), C46(H46), C60(H60), C38(H38), C74(H74), C83(H83),
  C76(H76), C26(H26), C75(H75)
5.c Idealised Me refined as rotating group:
 C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C91(H91A,H91B,H91C), C66(H66A,H66B,
 H66C), B1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C65(H65A,H65B,H65C), C48(H48A,
 H48B,H48C), C89(H89A,H89B,H89C), C30(H30A,H30B,H30C), C67(H67A,H67B,H67C),
 C85(H85A,H85B,H85C), B3(H3A,H3B,H3C), C49(H49A,H49B,H49C), C33(H33A,H33B,H33C),
  C19(H19A,H19B,H19C), B2(H2A,H2B,H2C), C34(H34A,H34B,H34C), C105(H10I,H10J,
 H10K), C50(H50A,H50B,H50C), C103(H10L,H10M,H10N), C90(H90A,H90B,H90C),
 C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C100(H10O,H10P,H10Q), C28(H28A,H28B,
 H28C), C14(H14A,H14B,H14C), C69(H69A,H69B,H69C), C104(H10R,H10S,H10T),
 C70(H70A,H70B,H70C), C32(H32A,H32B,H32C), C101(H10U,H10V,H10W), C18(H18A,H18B,
 H18C), C99(H99A,H99B,H99C), C29(H29A,H29B,H29C), C71(H71A,H71B,H71C), C56(H56A,
 H56B,H56C), C54(H54A,H54B,H54C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C57(H57A,H57B,H57C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              63616
_shelx_hkl_checksum              15947
_olex2_submission_special_instructions 'No special instructions were received'