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_4065191
_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         'C39 H49 B2 N12 O2 U1,C4 H8 O1'
_chemical_formula_sum            'C43 H57 B2 N12 O3 U'
_chemical_formula_weight         1049.66
_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                106.638(10)
_cell_angle_beta                 93.975(11)
_cell_angle_gamma                99.747(7)
_cell_formula_units_Z            2
_cell_length_a                   11.8162(13)
_cell_length_b                   13.8657(16)
_cell_length_c                   14.487(2)
_cell_measurement_reflns_used    6601
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      63
_cell_measurement_theta_min      3
_cell_volume                     2223.8(5)
_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 (DIRDIF, Beurskins, 2008)
;
_diffrn_ambient_temperature      150(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. 
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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31224
_diffrn_reflns_theta_full        60.0
_diffrn_reflns_theta_max         63.43
_diffrn_reflns_theta_min         3.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.467
_exptl_absorpt_correction_T_max  0.7951
_exptl_absorpt_correction_T_min  0.5768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1050
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.69
_refine_diff_density_min         -1.28
_refine_ls_d_res_high            0.89
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.073
_refine_ls_R_factor_gt           0.065
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1079P)^2^+14.3377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.176
_refine_ls_wR_factor_ref         0.183
_reflns_number_gt                5358
_reflns_number_total             6103
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            om200612h_si_002.cif
_cod_data_source_block           EMM11
_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 
;
_cod_original_cell_volume        2223.9(5)
_cod_original_formula_sum        'C43 H57 B2 N12 O3 U1'
_cod_database_code               4065191