Crystallographic characterization of (C~5~H~4~SiMe~3~)~3~U(BH~4~)
Windorff, Cory J.; Cross, Justin N.; Scott, Brian L.; Kozimor, Stosh A.; Evans, William J.; Acta Crystallographica Section E 77 (2021) 383–389; doi:10.1107/S2056989021002425

data_2243782
_publ_section_title
;
 Crystallographic characterization of (C~5~H~4~SiMe~3~)~3~U(BH~4~)
;
_journal_coeditor_code           ZL5005
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              383
_journal_page_last               389
_journal_paper_doi               10.1107/S2056989021002425
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[U (B H4) (C8 H13 Si)3]'
_chemical_formula_moiety         'C24 H43 B Si3 U'
_chemical_formula_sum            'C24 H43 B Si3 U'
_chemical_formula_weight         664.69
_chemical_name_systematic
(Borohydrido-\k^3^<i>H</i>)tris[\h^5^-(trimethylsilyl)cyclopentadienyl]uranium(IV)
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                94.159(3)
_cell_angle_beta                 96.016(3)
_cell_angle_gamma                103.256(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7530(15)
_cell_length_b                   12.217(2)
_cell_length_c                   13.657(2)
_cell_measurement_reflns_used    30231
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      33.142
_cell_measurement_theta_min      2.409
_cell_volume                     1406.6(4)
_computing_cell_refinement
;
APEX3 (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
<i>SHELXTL2018/3</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELXTL2018/3</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      112(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon II detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'I\mS 3.0 microfocus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30231
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.142
_diffrn_reflns_theta_min         2.409
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.906
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.4131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.881
_exptl_crystal_size_mid          0.622
_exptl_crystal_size_min          0.173
_refine_diff_density_max         3.873
_refine_diff_density_min         -2.719
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         10686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                9355
_reflns_number_total             10686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl5005sup1.cif
_cod_data_source_block           I
_cod_database_code               2243782
_shelx_estimated_absorpt_t_min   0.078
_shelx_estimated_absorpt_t_max   0.428
_shelx_hkl_checksum              2108
_shelx_res_checksum              70956
_cod_database_fobs_code 2243782