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_7718810
_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 H162.58 B3 O4 U, 2(C5 H12)'
_chemical_formula_sum            'C120 H186.58 B3 O4 U'
_chemical_formula_weight         1963.72
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 92.2340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7381(6)
_cell_length_b                   16.4819(5)
_cell_length_c                   30.7694(10)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.375
_cell_measurement_theta_min      2.471
_cell_volume                     11522.6(6)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE DUO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            126317
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.411
_diffrn_reflns_theta_min         1.998
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0788 before and 0.0534 after correction.
The Ratio of minimum to maximum transmission is 0.9441.
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    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             4182
_exptl_crystal_preparation       'Salt Metathesis'
_exptl_crystal_recrystallization_method 'Concentrate and cool'
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.865
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         11804
_refine_ls_number_restraints     522
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0307P)^2^+23.3190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11341
_reflns_number_total             11804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01076d2.cif
_cod_data_source_block           mo_dal24_73
_cod_depositor_comments
'Adding full bibliography for 7718809--7718812.cif.'
_cod_database_code               7718810
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.775
_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
 C59-C60 \\sim C59-C65
 with sigma of 0.02
 C59-C66 \\sim C59-C63
 with sigma of 0.02
 C59-C62 \\sim C59-C61
 with sigma of 0.02
 C18-C21 \\sim C18-C20
 with sigma of 0.02
 C18-C19 \\sim C18-C24
 with sigma of 0.02
 C18-C23 \\sim C18-C22
 with sigma of 0.02
 C31-C35 \\sim C31-C34
 with sigma of 0.02
 C31-C33 \\sim C31-C32
 with sigma of 0.02
 C31-C37 \\sim C31-C36
 with sigma of 0.02
 C38-C44 \\sim C38-C43
 with sigma of 0.02
 C38-C40 \\sim C38-C39
 with sigma of 0.02
 C38-C42 \\sim C38-C41
 with sigma of 0.02
 O1-C69 \\sim O1-C68
 with sigma of 0.02
 O2-C70 \\sim O2-C71
 with sigma of 0.02
 C69-C70 \\sim C68-C71
 with sigma of 0.02
 O1-C70 \\sim O1-C71
 with sigma of 0.04
 O2-C69 \\sim O2-C68
 with sigma of 0.04
 C73-C74 \\sim C82-C80
 with sigma of 0.02
 C74-C75 \\sim C80-C79
 with sigma of 0.02
 C75-C81 \\sim C79-C78
 with sigma of 0.02
 C81-C76 \\sim C78-C77
 with sigma of 0.02
 C73-C75 \\sim C82-C79
 with sigma of 0.04
 C74-C81 \\sim C80-C78
 with sigma of 0.04
 C75-C76 \\sim C79-C77
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C31 \\sim C35 \\sim C33 \\sim C37 \\sim C34 \\sim C36 \\sim C32: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C18 \\sim C21 \\sim C19 \\sim C23 \\sim C20 \\sim C24 \\sim C22: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C38 \\sim C44 \\sim C40 \\sim C42 \\sim C43 \\sim C39 \\sim C41: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C75 \\sim C81 \\sim C76 \\sim C82 \\sim C80 \\sim C79 \\sim C78 \\sim C77 \\sim
C73 \\sim C74: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C71) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C31, C35, C33, C37, C34, C36, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C18, C21, C19, C23, C20, C24, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C38, C44, C40, C42, C43, C39, C41
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C73, C74, C75, C81, C82, C80, C79, C78, C76, C77
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=1-FVAR(1)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=1-FVAR(2)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(3)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(3)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=1-FVAR(4)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(4)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C71)=Sof(H71A)=Sof(H71B)=1-FVAR(5)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70)=FVAR(5)
 Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(C79)=
 Sof(H79A)=Sof(H79B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C77)=Sof(H77A)=Sof(H77B)=
 Sof(H77C)=1-FVAR(6)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=
 Sof(H75A)=Sof(H75B)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C76)=Sof(H76A)=Sof(H76B)=
 Sof(H76C)=FVAR(6)
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C74(H74A,H74B), C75(H75A,H75B), C81(H81A,H81B), C68(H68A,
 H68B), C71(H71A,H71B), C80(H80A,H80B), C79(H79A,H79B), C78(H78A,H78B)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C54(H54), C5(H5), C47(H47), C10(H10), C30(H30), C50(H50), C8(H8),
 C52(H52), C28(H28), C4(H4), C26(H26), C3(H3), C48(H48), C70(H70)
6.c Idealised Me refined as rotating group:
 B2(H2A,H2B,H2C), C58(H58A,H58B,H58C), C67(H67A,H67B,H67C), C56(H56A,H56B,
 H56C), B1(H1A,H1B,H1C), C57(H57A,H57B,H57C), C72(H72A,H72B,H72C), C17(H17A,
 H17B,H17C), C15(H15A,H15B,H15C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C),
 C14(H14A,H14B,H14C), C37(H37A,H37B,H37C), C60(H60A,H60B,H60C), C21(H21A,H21B,
 H21C), C44(H44A,H44B,H44C), C66(H66A,H66B,H66C), C62(H62A,H62B,H62C), C73(H73A,
 H73B,H73C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C19(H19A,H19B,H19C),
 C23(H23A,H23B,H23C), C76(H76A,H76B,H76C), C61(H61A,H61B,H61C), C63(H63A,H63B,
 H63C), C65(H65A,H65B,H65C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C22(H22A,
 H22B,H22C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C32(H32A,H32B,H32C),
 C43(H43A,H43B,H43C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C82(H82A,H82B,
 H82C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              73502
_shelx_hkl_checksum              66818
_olex2_submission_special_instructions 'No special instructions were received'