Use of Alkylsodium Reagents for the Synthesis of Trivalent Uranium Alkyl Complexes
Matson, Ellen M.; Forrest, William P.; Fanwick, Phillip E.; Bart, Suzanne C.; Organometallics 31 (2012) 4467–; doi:10.1021/om3002763

data_4078491
_publ_section_title
;
 Use of Alkylsodium Reagents for the Synthesis of Trivalent Uranium Alkyl
 Complexes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              4467
_journal_paper_doi               10.1021/om3002763
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C15 H22 B1 I3 N6 U1,C16 H36 Li1 O4'
_chemical_formula_sum            'C31 H58 B I3 Li N6 O4 U'
_chemical_formula_weight         1215.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 112.352(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3062(7)
_cell_length_b                   11.9134(6)
_cell_length_c                   20.5103(7)
_cell_measurement_reflns_used    7626
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      3
_cell_volume                     4363.0(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 1997)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
 PATTY (DIRDIF99, Beurskins, 1999)
;
_diffrn_measured_fraction_theta_full 0.8843
_diffrn_measured_fraction_theta_max 0.7841
_diffrn_measurement_device_type  Rigaku_Rapid_II
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20023
_diffrn_reflns_theta_full        51.9
_diffrn_reflns_theta_max         70.18
_diffrn_reflns_theta_min         3.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    28.436
_exptl_absorpt_correction_T_max  0.4261
_exptl_absorpt_correction_T_min  0.1960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.13
_refine_diff_density_min         -2.40
_refine_ls_d_res_high            0.85
_refine_ls_extinction_coef       0.12E-03
_refine_ls_extinction_method     'SHELXL97 (Sheldrick 2008)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6625
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.078
_refine_ls_R_factor_gt           0.067
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.1369P)^2^+19.1046P] where P=(Fo^2^+2Fc^2^)/3 '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.188
_refine_ls_wR_factor_ref         0.202
_reflns_number_gt                5388
_reflns_number_total             6625
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            om3002763_si_004.cif
_cod_data_source_block           SCB106
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_formula_sum        'C31 H58 B1 I3 Li1 N6 O4 U1'
_cod_database_code               4078491