Synthesis of U(iv) imidos from Tp*(2)U(CH(2)Ph) (Tp* = hydrotris(3,5-dimethylpyrazolyl)borate) by extrusion of bibenzyl.
Matson, Ellen M.; Crestani, Marco G.; Fanwick, Phillip E.; Bart, Suzanne C.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 7952–7958; doi:10.1039/c2dt12439d

data_7019236
_publ_section_title
;
 Synthesis of U(iv) imidos from Tp*(2)U(CH(2)Ph) (Tp* =
 hydrotris(3,5-dimethylpyrazolyl)borate) by extrusion of bibenzyl.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7952
_journal_page_last               7958
_journal_paper_doi               10.1039/c2dt12439d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C39 H55 B2 N13 U1'
_chemical_formula_sum            'C39 H55 B2 N13 U'
_chemical_formula_weight         965.61
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 106.487(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3252(5)
_cell_length_b                   14.1075(4)
_cell_length_c                   19.9873(4)
_cell_measurement_reflns_used    8260
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72
_cell_measurement_theta_min      2
_cell_volume                     4143.6(2)
_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 0.9640
_diffrn_measured_fraction_theta_max 0.9640
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49215
_diffrn_reflns_theta_full        72.2
_diffrn_reflns_theta_max         72.18
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.207
_exptl_absorpt_correction_T_max  0.5432
_exptl_absorpt_correction_T_min  0.1867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.49
_refine_diff_density_min         -1.53
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7883
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.030
_refine_ls_R_factor_gt           0.030
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+6.9090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.081
_refine_ls_wR_factor_ref         0.082
_reflns_number_gt                7558
_reflns_number_total             7883
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            c2dt12439d.txt
_cod_data_source_block           SBMG01
_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 
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_cod_original_formula_sum        'C39 H55 B2 N13 U1'
_cod_database_code               7019236