Double uranium oxo cations derived from uranyl by borane or silane reduction.
Cowie, Bradley E.; Nichol, Gary S.; Love, Jason B.; Arnold, Polly L.; Chemical communications (Cambridge, England) 54 (2018) 3839–3842; doi:10.1039/c8cc00341f

data_7121459
_publ_section_title
;
 Double uranium oxo cations derived from uranyl by borane or silane
 reduction.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3839
_journal_page_last               3842
_journal_paper_doi               10.1039/c8cc00341f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C85 H71 B2 N11 O7 U2, C4 H8 O'
_chemical_formula_sum            'C89 H79 B2 N11 O8 U2'
_chemical_formula_weight         1928.36
_chemical_name_systematic        '[{(py){cat(py)BO)UOUOBcat(py)}(LA)]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-12-20 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                68.5930(10)
_cell_angle_beta                 79.0720(10)
_cell_angle_gamma                86.2280(10)
_cell_formula_units_Z            2
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_cell_length_b                   15.0681(3)
_cell_length_c                   18.9308(4)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      3.01
_cell_volume                     3863.52(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            88345
_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.345
_diffrn_reflns_theta_min         2.993
_exptl_absorpt_coefficient_mu    4.253
_exptl_absorpt_correction_T_max  0.4311
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_exptl_transmission_factor_max   0.4311
_exptl_transmission_factor_min   0.3817
_refine_diff_density_max         1.102
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_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         18474
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0259P)^2^+4.7880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14137
_reflns_number_total             18474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00341f2.cif
_cod_data_source_block           3_THF
_cod_depositor_comments
'Adding full bibliography for 7121458--7121462.cif.'
_cod_database_code               7121459
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.469
_shelx_estimated_absorpt_t_max   0.549
_shelx_res_checksum              8134