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_7121461
_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         'C92 H80 N10 O3 Si2 U2, C5 H5 N'
_chemical_formula_sum            'C97 H85 N11 O3 Si2 U2'
_chemical_formula_weight         1985.00
_chemical_name_systematic        '[{HPh2SiO(py)UOU(py)OSiPh2H}(LA)]'
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 114.099(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8381(5)
_cell_length_b                   17.7807(2)
_cell_length_c                   21.4711(4)
_cell_measurement_reflns_used    19902
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.7760
_cell_measurement_theta_min      3.3510
_cell_volume                     8307.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            125163
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.958
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.982
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       block
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.766
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         8502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.766
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7300
_reflns_number_total             8502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00341f2.cif
_cod_data_source_block           5py_py
_cod_depositor_comments
'Adding full bibliography for 7121458--7121462.cif.'
_cod_database_code               7121461
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.506
_shelx_estimated_absorpt_t_max   0.790
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              6944