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_4080373
_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_formula_moiety         'C49 H51 B1 N6 O1 U1,C4 H10 O1'
_chemical_formula_sum            'C53 H61 B N6 O2 U'
_chemical_formula_weight         1062.96
_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                81.376(3)
_cell_angle_beta                 73.371(3)
_cell_angle_gamma                69.5017(19)
_cell_formula_units_Z            2
_cell_length_a                   11.4951(3)
_cell_length_b                   14.2060(4)
_cell_length_c                   16.4196(7)
_cell_measurement_reflns_used    8290
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      2
_cell_volume                     2402.80(15)
_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 0.9070
_diffrn_measured_fraction_theta_max 0.9070
_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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48111
_diffrn_reflns_theta_full        60.0
_diffrn_reflns_theta_max         70.14
_diffrn_reflns_theta_min         2.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.863
_exptl_absorpt_correction_T_max  0.5533
_exptl_absorpt_correction_T_min  0.4978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.03
_refine_diff_density_min         -1.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         8281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.036
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+2.4503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.092
_refine_ls_wR_factor_ref         0.093
_reflns_number_gt                8158
_reflns_number_total             8281
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            om301139h_si_004.cif
_cod_data_source_block           EMM26
_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_cell_volume        2402.80(14)
_cod_original_formula_sum        'C53 H61 B1 N6 O2 U1'
_cod_database_code               4080373