A Crystallizable Dinuclear Tuck-In-Tuck-Over Tuck-Over Dialkyl Tren Uranium Complex and Double Dearylation of BPh4- To Give the BPh2-Functionalized Metallocycle [U{N(CH2CH2NSiMe3)2(CH2CH2NSiMe2CHBPh2)}(THF)]
Benedict M. Gardner; Jonathan McMaster; William Lewis; Alexander J. Blake; Stephen T. Liddle; Journal of the American Chemical Society 131 (2009) 10388–10389; doi:10.1021/ja904459q

data_4104788
_publ_section_title
;
 A Crystallizable Dinuclear Tuck-In-Tuck-Over Tuck-Over Dialkyl Tren
 Uranium Complex and Double Dearylation of BPh4- To Give the
 BPh2-Functionalized Metallocycle
 [U{N(CH2CH2NSiMe3)2(CH2CH2NSiMe2CHBPh2)}(THF)]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10388
_journal_page_last               10389
_journal_paper_doi               10.1021/ja904459q
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C30 H76 N8 Si6 U2'
_chemical_formula_sum            'C30 H76 N8 Si6 U2'
_chemical_formula_weight         1193.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.067(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9142(15)
_cell_length_b                   16.979(2)
_cell_length_c                   25.765(4)
_cell_measurement_reflns_used    5210
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.24
_cell_volume                     4701.1(11)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction
'Bruker SAINT; Bruker SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'enCIFer(Allen et al., 2004); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            27844
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.063
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       plate
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.771
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         10665
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                8341
_reflns_number_total             10665
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja904459q_si_004.cif
_cod_data_source_block           5
_cod_original_cell_volume        4701.2(11)
_cod_database_code               4104788