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_7121460
_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         'C94 H94 N8 O5 Si2 U2, C4 H8 O'
_chemical_formula_sum            'C98 H102 N8 O7 Si2 U2'
_chemical_formula_weight         2036.12
_chemical_name_systematic
;
 [{HPh2SiO(THF)UOU(THF)OSiPh2H}(LA)]
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-12-20 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.2830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.5124(2)
_cell_length_b                   19.8405(2)
_cell_length_c                   20.1410(2)
_cell_measurement_reflns_used    22958
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.693
_cell_measurement_theta_min      3.0660
_cell_volume                     8438.29(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  22.00   1.00   30.00    --  -18.53 -99.00 120.00   47
  2  \w    -25.00  22.00   1.00   30.00    --  -18.53 -99.00 -60.00   47
  3  \w    -25.00  22.00   1.00   30.00    --  -18.53 -99.00-180.00   47
  4  \w    -93.00 -34.00   1.00   30.00    --  -18.53-179.00 -30.00   59
  5  \w    -93.00 -34.00   1.00   30.00    --  -18.53-179.00-180.00   59
  6  \w    -25.00  22.00   1.00   30.00    --  -18.53 -99.00  30.00   47
  7  \w     -2.00  91.00   1.00   30.00    --   20.25  38.00 -90.00   93
  8  \w    -48.00  39.00   1.00   30.00    --   20.25 -57.00   0.00   87
  9  \w      2.00  89.00   1.00   30.00    --   20.25  57.00 -90.00   87
 10  \w    -48.00  39.00   1.00   30.00    --   20.25 -57.00 120.00   87
 11  \w    -67.00  12.00   1.00   30.00    --  -18.53 114.00-133.62   79
 12  \w      2.00  89.00   1.00   30.00    --   20.25  57.00 150.00   87
 13  \w    -48.00  39.00   1.00   30.00    --   20.25 -57.00 150.00   87
 14  \w     -2.00  42.00   1.00   30.00    --   20.25-126.00 160.91   44
 15  \w    -18.00  93.00   1.00   30.00    --   20.25  19.00 120.00  111
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            88911
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    3.925
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.3404
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (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            orange
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4056
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8628
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+30.4918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                7290
_reflns_number_total             8628
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c8cc00341f2.cif
_cod_data_source_block           5THF_THF
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7121458--7121462.cif.
;
_cod_original_cell_volume        8438.29(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7121460