Formation of Trivalent U–C, U–N, and U–S Bonds and Their Reactivity toward Carbon Dioxide and Acetone
Matson, Ellen M.; Fanwick, Phillip E.; Bart, Suzanne C.; Organometallics 30 (2011) 5753–; doi:10.1021/om200612h

data_4065192
_publ_section_title
;
 Formation of Trivalent U--C, U--N, and U--S Bonds and Their Reactivity
 toward Carbon Dioxide and Acetone
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5753
_journal_paper_doi               10.1021/om200612h
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C36 H49 B2 N12 S1 U1,0.5(C7 H8)'
_chemical_formula_sum            'C39.5 H53 B2 N12 S U'
_chemical_formula_weight         987.66
_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                101.936(4)
_cell_angle_beta                 103.289(3)
_cell_angle_gamma                90.589(3)
_cell_formula_units_Z            4
_cell_length_a                   10.7260(4)
_cell_length_b                   19.6760(6)
_cell_length_c                   22.8275(9)
_cell_measurement_reflns_used    15330
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      72
_cell_measurement_theta_min      2
_cell_volume                     4578.8(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 0.8490
_diffrn_measured_fraction_theta_max 0.8490
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39912
_diffrn_reflns_theta_full        72.2
_diffrn_reflns_theta_max         72.16
_diffrn_reflns_theta_min         2.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.466
_exptl_absorpt_correction_T_max  0.3996
_exptl_absorpt_correction_T_min  0.3859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_platon_squeeze_details
'                                                                       '
_refine_diff_density_max         2.33
_refine_diff_density_min         -1.74
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1026
_refine_ls_number_reflns         15320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.045
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+9.6783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.118
_refine_ls_wR_factor_ref         0.121
_reflns_number_gt                13834
_reflns_number_total             15320
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            om200612h_si_003.cif
_cod_data_source_block           EMM13
_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 1715 2011-07-08 13:25:40Z adriana 

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_formula_sum        'C39.50 H53 B2 N12 S1 U1'
_cod_database_code               4065192