Synthesis and Reactivity of Trivalent Tp*U(CH2Ph)2(THF): Insertion vs Oxidation at Low-Valent Uranium–Carbon Bonds
Matson, Ellen M.; Forrest, William P.; Fanwick, Phillip E.; Bart, Suzanne C.; Organometallics 32 (2013) 1484–; doi:10.1021/om301139h

data_4080372
_publ_section_title
;
 Synthesis and Reactivity of Trivalent Tp*U(CH2Ph)2(THF): Insertion vs
 Oxidation at Low-Valent Uranium--Carbon Bonds
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1484
_journal_paper_doi               10.1021/om301139h
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H44 B1 N6 O1 U1'
_chemical_formula_sum            'C33 H44 B N6 O U'
_chemical_formula_weight         789.60
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   28.1568(11)
_cell_length_b                   40.7185(18)
_cell_length_c                   11.4426(4)
_cell_measurement_reflns_used    54850
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     13119.0(9)
_computing_cell_refinement
'DENZO/SCALEPACK (Otwinowski &amp; Minor, 1996)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction
'DENZO/SCALEPACK (Otwinowski &amp; 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      150.00(2)
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1030
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_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            54850
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.984
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.9618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski &amp; Minor, 1997)'
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6224
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.88
_refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.423(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7382
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0112P)^2^+334.7383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.074
_refine_ls_wR_factor_ref         0.079
_reflns_Friedel_coverage         0.9325
_reflns_number_gt                6416
_reflns_number_total             7382
_reflns_threshold_expression     &gt;2.0\s(I)
_cod_data_source_file            om301139h_si_004.cif
_cod_data_source_block           EMM23
_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 2.4.2 from 2011-04-26.

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_formula_sum        'C33 H44 B1 N6 O1 U1'
_cod_database_code               4080372