Diamido-Ether Actinide Complexes as Catalysts for the Intramolecular Hydroamination of Aminoalkenes
Hayes, Cassandra E.; Platel, Rachel H.; Schafer, Laurel L.; Leznoff, Daniel B.; Organometallics 31 (2012) 6732–; doi:10.1021/om300410h

data_4079053
_publ_section_title
;
 Diamido-Ether Actinide Complexes as Catalysts for the Intramolecular
 Hydroamination of Aminoalkenes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6732
_journal_paper_doi               10.1021/om300410h
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H52 Cl2 N2 O3 Th1'
_chemical_formula_sum            'C32 H52 Cl2 N2 O3 Th'
_chemical_formula_weight         815.72
_chemical_name_systematic        ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0499(10)
_cell_length_b                   16.871(2)
_cell_length_c                   26.702(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3626.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
ORTEP 3 
;
_computing_publication_material
;
CRYSTALS (Betteridge et al., 2003) 
;
_computing_structure_refinement
;
CRYSTALS (Betteridge et al., 2003) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40999
_diffrn_reflns_theta_full        26.782
_diffrn_reflns_theta_max         26.782
_diffrn_reflns_theta_min         1.945
_exptl_absorpt_coefficient_mu    4.290
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5119
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_details 'Flack (1983), 3370 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.008(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6760
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.001493
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0245
_refine_ls_wR_factor_gt          0.0235
_refine_ls_wR_factor_ref         0.0233
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                6909
_reflns_number_total             7729
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.89
_oxford_diffrn_Wilson_scale      252.35
_oxford_refine_ls_r_factor_ref   0.0237
_oxford_refine_ls_scale          0.06753(8)
_oxford_reflns_number_all        7729
_oxford_reflns_threshold_expression_ref I>2.5\s(I)
_cod_data_source_file            om300410h_si_001.cif
_cod_data_source_block           '[iPr2PhNCOCN]ThCl2DME'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
;
_cod_original_cell_volume        3626.4(8)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C32 H52 Cl2 N2 O3 Th1'
_cod_database_code               4079053