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_4123036
_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 U, 3(C7)'
_chemical_formula_sum            'C66 H90 N6 Si6 U'
_chemical_formula_weight         1374.01
_chemical_name_common            moris372
_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                95.5880(18)
_cell_angle_beta                 92.6530(15)
_cell_angle_gamma                102.1780(8)
_cell_formula_units_Z            2
_cell_length_a                   12.0440(2)
_cell_length_b                   14.0560(3)
_cell_length_c                   23.1880(4)
_cell_measurement_reflns_used    11075
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.56
_cell_measurement_theta_min      0.88
_cell_volume                     3809.92(12)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11339
_diffrn_reflns_theta_full        24.56
_diffrn_reflns_theta_max         24.56
_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    2.262
_exptl_absorpt_correction_T_max  0.6128
_exptl_absorpt_correction_T_min  0.4501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         11339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                8815
_reflns_number_total             11339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5091436_si_002.cif
_cod_data_source_block           moris372
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-23
;
_cod_original_cell_volume        3809.91(12)
_cod_database_code               4123036