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_4078490
_publ_section_title
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 Use of Alkylsodium Reagents for the Synthesis of Trivalent Uranium Alkyl
 Complexes
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_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         'C34 H55 B2 N12 Si1 U1,0.5(C6 H14)'
_chemical_formula_sum            'C37 H62 B2 N12 Si U'
_chemical_formula_weight         962.73
_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_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                78.889(5)
_cell_angle_beta                 66.013(5)
_cell_angle_gamma                84.836(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6822(8)
_cell_length_b                   13.1029(10)
_cell_length_c                   14.4609(10)
_cell_measurement_reflns_used    7836
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     2154.2(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, 2003)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
 PATTY (DIRDIF, Beurskins, 2008)
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.9210
_diffrn_measured_fraction_theta_max 0.9210
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not cusp 
data but mostly high angle data.
Also the use of HKL2000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total
;
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37563
_diffrn_reflns_theta_full        72.3
_diffrn_reflns_theta_max         72.26
_diffrn_reflns_theta_min         3.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.187
_exptl_absorpt_correction_T_max  0.7995
_exptl_absorpt_correction_T_min  0.7182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.38
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7832
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.066
_refine_ls_R_factor_gt           0.055
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+17.3186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.129
_refine_ls_wR_factor_ref         0.138
_reflns_number_gt                6732
_reflns_number_total             7832
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            om3002763_si_003.cif
_cod_data_source_block           EMM20
_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 

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 
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_cod_original_formula_sum        'C37 H62 B2 N12 Si1 U1'
_cod_database_code               4078490