Single and Double Alkyl Abstraction from a Bis(anilido)xanthene Thorium(IV) Dibenzyl Complex: Isolation of an Organothorium Cation and a Thorium Dication
Cruz, Carlos A.; Emslie, David J. H.; Harrington, Laura E.; Britten, James F.; Organometallics 27 (2008) 15–; doi:10.1021/om7011503

data_4070956
_publ_section_title
;
 Single and Double Alkyl Abstraction from a Bis(anilido)xanthene
 Thorium(IV) Dibenzyl Complex: Isolation of an Organothorium Cation and a
 Thorium Dication
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              15
_journal_paper_doi               10.1021/om7011503
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety
'C47 H62 N2 O Th, 2(C25 H7 B F15), 1.5(C6 H14), 3(C7 H8)'
_chemical_formula_sum            'C127 H121 B2 F30 N2 O Th'
_chemical_formula_weight         2514.92
_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                76.793(2)
_cell_angle_beta                 87.806(3)
_cell_angle_gamma                89.678(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8360(16)
_cell_length_b                   16.6177(19)
_cell_length_c                   25.570(3)
_cell_measurement_reflns_used    3085
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17.42
_cell_measurement_theta_min      2.16
_cell_volume                     5719.4(11)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1322
_diffrn_reflns_av_sigmaI/netI    0.1960
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            71694
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2550
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1392
_refine_ls_number_reflns         25890
_refine_ls_number_restraints     1039
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1653
_reflns_number_gt                14057
_reflns_number_total             25890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7011503-file003.cif
_cod_data_source_block           cruz30
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5719.5(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070956