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_7019235
_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         'C40 H59 B2 N13 U1,2(C7 H8)'
_chemical_formula_sum            'C54 H75 B2 N13 U'
_chemical_formula_weight         1165.94
_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                97.930(3)
_cell_angle_beta                 101.255(3)
_cell_angle_gamma                106.142(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1993(4)
_cell_length_b                   14.0954(6)
_cell_length_c                   22.3766(7)
_cell_measurement_reflns_used    9427
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      2
_cell_volume                     2676.0(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, 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 0.9240
_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. 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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            50971
_diffrn_reflns_theta_full        65.0
_diffrn_reflns_theta_max         70.13
_diffrn_reflns_theta_min         2.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.911
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_correction_T_min  0.1763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.39
_refine_diff_density_min         -1.46
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         9387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.036
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+4.3016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.096
_refine_ls_wR_factor_ref         0.096
_reflns_number_gt                9373
_reflns_number_total             9387
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            c2dt12439d.txt
_cod_data_source_block           EMM32
_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 

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        2676.03(18)
_cod_original_formula_sum        'C54 H75 B2 N13 U1'
_cod_database_code               7019235