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_4078489
_publ_section_title
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 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         'C30.92 H46.76 B2 I0.079 N12 U1'
_chemical_formula_sum            'C30.92 H46.76 B2 I0.08 N12 U'
_chemical_formula_weight         856.29
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                96.786(7)
_cell_angle_beta                 100.517(6)
_cell_angle_gamma                115.091(6)
_cell_formula_units_Z            2
_cell_length_a                   10.2751(7)
_cell_length_b                   10.7169(9)
_cell_length_c                   18.3052(13)
_cell_measurement_reflns_used    6162
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      2
_cell_volume                     1751.0(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, 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 0.9240
_diffrn_measured_fraction_theta_max 0.9240
_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  0.0870
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31805
_diffrn_reflns_theta_full        67.5
_diffrn_reflns_theta_max         70.18
_diffrn_reflns_theta_min         2.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.908
_exptl_absorpt_correction_T_max  0.7572
_exptl_absorpt_correction_T_min  0.4765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.58
_refine_diff_density_min         -1.75
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         6161
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.064
_refine_ls_R_factor_gt           0.060
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1005P)^2^+9.0762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.163
_refine_ls_wR_factor_ref         0.167
_reflns_number_gt                5695
_reflns_number_total             6161
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            om3002763_si_002.cif
_cod_data_source_block           EMM33
_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 
;
_cod_original_cell_volume        1751.0(2)
_cod_original_formula_sum        'C30.92 H46.76 B2 I0.08 N12 U1'
_cod_database_code               4078489