Uranium(IV) Alkyl Complexes of a Rigid Dianionic NON-Donor Ligand: Synthesis and Quantitative Alkyl Exchange Reactions with Alkyllithium Reagents
Andreychuk, Nicholas R.; Ilango, Sougandi; Vidjayacoumar, Balamurugan; Emslie, David J. H.; Jenkins, Hilary A.; Organometallics 32 (2013) 1466–; doi:10.1021/om301136f

data_4080366
_publ_section_title
;
 Uranium(IV) Alkyl Complexes of a Rigid Dianionic NON-Donor Ligand:
 Synthesis and Quantitative Alkyl Exchange Reactions with Alkyllithium
 Reagents
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1466
_journal_paper_doi               10.1021/om301136f
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C50 H71 N2 O U, C12 H30 Li O6, C4 H10 O2'
_chemical_formula_sum            'C66 H111 Li N2 O9 U'
_chemical_formula_weight         1321.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.978(5)
_cell_angle_beta                 81.499(5)
_cell_angle_gamma                83.966(6)
_cell_formula_units_Z            2
_cell_length_a                   14.259(4)
_cell_length_b                   14.344(4)
_cell_length_c                   17.959(5)
_cell_measurement_reflns_used    2668
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      35.072
_cell_measurement_theta_min      4.695
_cell_volume                     3529.6(17)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1075
_diffrn_reflns_av_sigmaI/netI    0.1577
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41002
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    2.350
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         14468
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                8061
_reflns_number_total             14468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301136f_si_002.cif
_cod_data_source_block           si4_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3529.4(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080366