Mixed sandwich thorium complexes incorporating bis(tri-isopropylsilyl)cyclooctatetraenyl and pentamethylcyclopentadienyl ligands: synthesis, structure and reactivity.
Button, Zoë E; Higgins, Jessica A.; Suvova, Markéta; Cloke, F Geoffrey N; Roe, S. Mark; Dalton transactions (Cambridge, England : 2003) 44 (2015) 2588–2596; doi:10.1039/c4dt02362e

data_7032842
_publ_section_title
;
 Mixed sandwich thorium complexes incorporating
 bis(tri-isopropylsilyl)cyclooctatetraenyl and pentamethylcyclopentadienyl
 ligands: synthesis, structure and reactivity.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2588
_journal_page_last               2596
_journal_paper_doi               10.1039/c4dt02362e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C88 H142 O4 Si4 Th2'
_chemical_formula_sum            'C88 H142 O4 Si4 Th2'
_chemical_formula_weight         1840.46
_chemical_name_common            complex_4_oxalate
_chemical_name_systematic
;
(mu-oxalato)bis{(eta-5-pentamethylcyclopentadienyl)
(eta-8-(bis{triisopropylsilyl}cyclooctatetraene))thorium(IV)}
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-08-30T12:42:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                65.525(2)
_cell_angle_beta                 67.618(2)
_cell_angle_gamma                72.722(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3722(5)
_cell_length_b                   13.3983(4)
_cell_length_c                   15.7276(7)
_cell_measurement_reflns_used    42280
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2163.84(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.401144E-1
_diffrn_orient_matrix_UB_12      -0.341333E-1
_diffrn_orient_matrix_UB_13      0.524375E-1
_diffrn_orient_matrix_UB_21      0.786876E-1
_diffrn_orient_matrix_UB_22      0.89971E-2
_diffrn_orient_matrix_UB_23      -0.509516E-1
_diffrn_orient_matrix_UB_31      -0.74135E-2
_diffrn_orient_matrix_UB_32      0.752868E-1
_diffrn_orient_matrix_UB_33      0.23018E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.053
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28262
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.61
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.534
_exptl_absorpt_correction_T_max  0.9384
_exptl_absorpt_correction_T_min  0.8547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         9819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+3.2251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                8532
_reflns_number_total             9819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02362e2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7032839--7032844.cif.'
_cod_database_code               7032842