Reductive silylation of Cp*UO2((Mes)PDI(Me)) promoted by Lewis bases.
Kiernicki, J. J.; Harwood, J. S.; Fanwick, P. E.; Bart, S. C.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 3111–3119; doi:10.1039/c5dt04776e

data_7038035
_publ_section_title
;
 Reductive silylation of Cp*UO2((Mes)PDI(Me)) promoted by Lewis bases.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3111
_journal_page_last               3119
_journal_paper_doi               10.1039/c5dt04776e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C6 H5 P1 S2 Si1 U1,C3 H9 O1 Si1,2(C1 F3),8(H2 O1),2(C4 H8 O1),3(C1 H3),2(C6 H5)'
_chemical_formula_sum            'C34 H49 F6 O11 P S2 Si2 U'
_chemical_formula_weight         1137.03
_chemical_properties_physical    'Air-sensitive, Hygroscopic, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-10 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.3790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0951(3)
_cell_length_b                   18.5493(4)
_cell_length_c                   17.7595(5)
_cell_measurement_reflns_used    53002
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.875
_cell_measurement_theta_min      3.941
_cell_volume                     4639.29(19)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53002
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.875
_diffrn_reflns_theta_min         3.941
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    12.173
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, Pentane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         4.064
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         8289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+18.9372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7883
_reflns_number_total             8289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04776e2.cif
_cod_data_source_block           JK755
_cod_depositor_comments
'Adding full bibliography for 7038033--7038036.cif.'
_cod_database_code               7038035
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.195
_shelx_estimated_absorpt_t_max   0.376
_shelx_res_checksum              84308