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_4080365
_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         '(C57 H84 N2 O U), (C6 H14)'
_chemical_formula_sum            'C63 H98 N2 O U'
_chemical_formula_weight         1137.51
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.716(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.383(16)
_cell_length_b                   9.827(5)
_cell_length_c                   38.880(20)
_cell_measurement_reflns_used    6113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.13
_cell_measurement_theta_min      2.26
_cell_volume                     11697(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1296
_diffrn_reflns_av_sigmaI/netI    0.1047
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            117765
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    2.815
_exptl_absorpt_correction_T_max  0.7661
_exptl_absorpt_correction_T_min  0.4143
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4632
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
two molecules of disordered hexane solvent were squeezed from the lattice.
These two molecules are included in the moiety formula, which is a source of 
checkcif error.
;
_refine_diff_density_max         1.851
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1130
_refine_ls_number_reflns         20610
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                12817
_reflns_number_total             20610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301136f_si_002.cif
_cod_data_source_block           nra19_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4080365