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_7038033
_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         'C54 H58 O4 Si2 P2 S2 U1,3(C6 H6)'
_chemical_formula_sum            'C72 H76 O4 P2 S2 Si2 U'
_chemical_formula_weight         1425.59
_chemical_properties_physical    'Air-sensitive, Hygroscopic'
_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   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                 95.099(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9048(7)
_cell_length_b                   11.6124(4)
_cell_length_c                   25.6316(8)
_cell_measurement_reflns_used    35035
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      70.181
_cell_measurement_theta_min      5.393
_cell_volume                     6790.5(4)
_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 0.980
_diffrn_measured_fraction_theta_max 0.973
_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  0.057
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35035
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.181
_diffrn_reflns_theta_min         5.393
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    8.446
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_correction_T_min  0.017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.046
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+20.1313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5831
_reflns_number_total             6290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04776e2.cif
_cod_data_source_block           JK717
_cod_depositor_comments
'Adding full bibliography for 7038033--7038036.cif.'
_cod_database_code               7038033
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.283
_shelx_estimated_absorpt_t_max   0.486
_shelx_res_checksum              25450