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_4080364
_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         '2(C55 H84 N2 O Si2 U), 4(C6H14)'
_chemical_formula_sum            'C134 H224 N2 O2 Si2 U2'
_chemical_formula_weight         2427.39
_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                82.016(4)
_cell_angle_beta                 79.396(4)
_cell_angle_gamma                88.571(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3983(16)
_cell_length_b                   19.246(3)
_cell_length_c                   26.498(4)
_cell_measurement_reflns_used    1257
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17.48
_cell_measurement_theta_min      2.65
_cell_volume                     6154.7(16)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0801
_diffrn_reflns_av_sigmaI/netI    0.1024
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64632
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    2.697
_exptl_absorpt_correction_T_max  0.8998
_exptl_absorpt_correction_T_min  0.4983
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
squeeze used to remove contribution from 3 disordered hexane molecules. 
These three molecules are included in the moiety formula, which is a source of 
checkcif error.
;
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         21560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                13751
_reflns_number_total             21560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301136f_si_002.cif
_cod_data_source_block           si5-sr
_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 

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 

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        6154.8(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080364