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_7032843
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C43 H70 Si2 Th'
_chemical_formula_sum            'C43 H70 Si2 Th'
_chemical_formula_weight         875.21
_chemical_name_common            complex_5_benzyl
_chemical_name_systematic
;
benzyl(eta-5-pentamethylcyclopentadienyl)
(eta-8-(bis{triisopropylsilyl}cyclooctatetraene))thorium(IV)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2014-10-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                82.3334(9)
_cell_angle_beta                 75.2024(9)
_cell_angle_gamma                69.8092(7)
_cell_formula_units_Z            4
_cell_length_a                   13.0170(2)
_cell_length_b                   17.3983(3)
_cell_length_c                   20.0305(3)
_cell_measurement_reflns_used    36078
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     4111.28(12)
_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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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      -0.396874E-1
_diffrn_orient_matrix_UB_12      -0.154445E-1
_diffrn_orient_matrix_UB_13      -0.300755E-1
_diffrn_orient_matrix_UB_21      0.672889E-1
_diffrn_orient_matrix_UB_22      -0.69015E-2
_diffrn_orient_matrix_UB_23      -0.392261E-1
_diffrn_orient_matrix_UB_31      0.308948E-1
_diffrn_orient_matrix_UB_32      -0.589368E-1
_diffrn_orient_matrix_UB_33      0.151573E-1
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70493
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         1.053
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.713
_exptl_absorpt_correction_T_max  0.7268
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.828
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         18670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+2.7590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14329
_reflns_number_total             18670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02362e2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7032839--7032844.cif.'
_cod_original_cell_volume        4111.27(12)
_cod_database_code               7032843
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: H32A(0.5) H32B(0.5) H32C(0.5) H32D(0.5) H32E(0.5) H32F(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) H33D(0.5) H33E(0.5) H33F(0.5) H34A(0.5)
 H34B(0.5) H34C(0.5) H34D(0.5) H34E(0.5) H34F(0.5) H35A(0.5) H35B(0.5)
 H35C(0.5) H35D(0.5) H35E(0.5) H35F(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
 H36D(0.5) H36E(0.5) H36F(0.5) H75A(0.5) H75B(0.5) H75C(0.5) H75D(0.5)
 H75E(0.5) H75F(0.5) H76A(0.5) H76B(0.5) H76C(0.5) H76D(0.5) H76E(0.5)
 H76F(0.5) H77A(0.5) H77B(0.5) H77C(0.5) H77D(0.5) H77E(0.5) H77F(0.5)
 H78A(0.5) H78B(0.5) H78C(0.5) H78D(0.5) H78E(0.5) H78F(0.5) H79A(0.5)
 H79B(0.5) H79C(0.5) H79D(0.5) H79E(0.5) H79F(0.5)
3.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C15(H15), C18(H18), C21(H21), C24(H24), C52(H52), C55(H55),
 C58(H58), C61(H61), C64(H64), C67(H67)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C80(H80A,H80B)
3.c Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C),
 C68(H68A,H68B,H68C), C69(H69A,H69B,H69C)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C39(H39), C40(H40), C41(H41),
 C42(H42), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51),
  C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
3.e Disordered Me refined as rotating group:
 C32(H32A,H32B,H32C,H32D,H32E,H32F), C33(H33A,H33B,H33C,H33D,H33E,H33F),
 C34(H34A,H34B,H34C,H34D,H34E,H34F), C35(H35A,H35B,H35C,H35D,H35E,H35F),
 C36(H36A,H36B,H36C,H36D,H36E,H36F), C75(H75A,H75B,H75C,H75D,H75E,H75F),
 C76(H76A,H76B,H76C,H76D,H76E,H76F), C77(H77A,H77B,H77C,H77D,H77E,H77F),
 C78(H78A,H78B,H78C,H78D,H78E,H78F), C79(H79A,H79B,H79C,H79D,H79E,H79F)
;