Radical Reductive Elimination from Tetrabenzyluranium Mediated by an Iminoquinone Ligand
Matson, Ellen M.; Franke, Sebastian M.; Anderson, Nickolas H.; Cook, Timothy D.; Fanwick, Phillip E.; Bart, Suzanne C.; Organometallics 33 (2014) 1964–; doi:10.1021/om4012104

data_4082952
_publ_section_title
;
 Radical Reductive Elimination from Tetrabenzyluranium Mediated by an
 Iminoquinone Ligand
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1964
_journal_paper_doi               10.1021/om4012104
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C41 H60 I1 N1 O3 U1,0.5(C7 H8)'
_chemical_formula_sum            'C44.5 H64 I N O3 U'
_chemical_formula_weight         1025.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 108.301(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.2048(9)
_cell_length_b                   15.3209(5)
_cell_length_c                   22.6313(7)
_cell_measurement_reflns_used    19686
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      68
_cell_measurement_theta_min      1
_cell_volume                     9284.9(5)
_computing_cell_refinement
'DENZO/SCALEPACK (Otwinowski &amp; Minor, 1996)'
_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_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
;
 Direct methods (Shelxs97, Sheldrick, 2008)
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_measured_fraction_theta_max 0.9960
_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  0.1090
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            121346
_diffrn_reflns_theta_full        60.0
_diffrn_reflns_theta_max         68.36
_diffrn_reflns_theta_min         1.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.322
_exptl_absorpt_correction_T_max  0.6315
_exptl_absorpt_correction_T_min  0.1612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski &amp; Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_platon_squeeze_details
'                                                                       '
_refine_diff_density_max         1.86
_refine_diff_density_min         -2.08
_refine_ls_d_res_high            0.89
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         13745
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.082
_refine_ls_R_factor_gt           0.070
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1441P)^2^+25.1546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.201
_refine_ls_wR_factor_ref         0.211
_reflns_number_gt                11340
_reflns_number_total             13745
_reflns_threshold_expression     &gt;2.0\s(I)
_cod_data_source_file            om4012104_si_003.cif
_cod_data_source_block           EMM53
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4082952--4082954.cif.

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        9284.8(5)
_cod_original_formula_sum        'C44.50 H64 I1 N1 O3 U1'
_cod_database_code               4082952