Mono(imidazolin-2-iminato) Actinide Complexes: Synthesis and Application in the Catalytic Dimerization of Aldehydes
Karmel, Isabell S. R.; Fridman, Natalia; Tamm, Matthias; Eisen, Moris S.; Journal of the American Chemical Society 136 (2014) 17180–17192; doi:10.1021/ja5091436

data_4123035
_publ_section_title
;
 Mono(imidazolin-2-iminato) Actinide Complexes: Synthesis and Application
 in the Catalytic Dimerization of Aldehydes
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17180
_journal_page_last               17192
_journal_paper_doi               10.1021/ja5091436
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C45 H90 N6 Si6 Th, 3(C7)'
_chemical_formula_sum            'C66 H90 N6 Si6 Th'
_chemical_formula_weight         1368.02
_chemical_name_common            moris371
_chemical_name_systematic        ?
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.8390(11)
_cell_angle_beta                 92.6290(11)
_cell_angle_gamma                102.239(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0820(4)
_cell_length_b                   14.0920(4)
_cell_length_c                   23.2090(10)
_cell_measurement_reflns_used    12313
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      0.88
_cell_volume                     3832.5(2)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2006)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_sigmaI/netI    0.1426
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12969
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         0.88
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    2.077
_exptl_absorpt_correction_T_max  0.7062
_exptl_absorpt_correction_T_min  0.5747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         12969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1691
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+12.6790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.2008
_reflns_number_gt                7524
_reflns_number_total             12969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5091436_si_002.cif
_cod_data_source_block           moris371
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-23
;
_cod_database_code               4123035