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_7032839
_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         'C36 H63 Cl Si2 Th, C6 H12'
_chemical_formula_sum            'C42 H75 Cl Si2 Th'
_chemical_formula_weight         903.69
_chemical_name_common            complex_1_chloride
_chemical_name_systematic
;
chloro(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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                92.8860(10)
_cell_angle_beta                 99.1770(10)
_cell_angle_gamma                109.519(2)
_cell_formula_units_Z            2
_cell_length_a                   8.67790(10)
_cell_length_b                   12.8594(2)
_cell_length_c                   20.8423(4)
_cell_measurement_reflns_used    5394
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2150.66(7)
_computing_cell_refinement       'SHELXL-97 (Sheldrick, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'HKL 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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26588
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.062
_diffrn_reflns_theta_min         3.418
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.611
_exptl_absorpt_correction_T_max  0.9218
_exptl_absorpt_correction_T_min  0.8347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9259
_refine_ls_number_restraints     543
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+9.5726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7789
_reflns_number_total             9259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02362e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7032839--7032844.cif.'
_cod_original_cell_volume        2150.66(6)
_cod_database_code               7032839
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 Th1, C1, C2, C8, Si1, H2, C3, C7, H8, C9, C12, C15, C5, Cl1, C6, C4, C30, C29,
  C31, H3, H7, H9, C10, C11, H12, C13, C14, H15, C16, C17, H14A, H5, H6, Si2,
 C35, C28, C34, C27, C36, H10A, H10B, H10C, H11A, H11B, H11C, H13A, H13B, H13C,
 H14B, H14C, H16A, H16B, H16C, H17A, H17B, H17C, C18, C21, C24, H35A, H35B,
 H35C, C33, H34A, H34B, H34C, C32, H36A, H36B, H36C, H18, C19, C20, H21, C22,
 C23, H24, C25, C26, H33A, H33B, H33C, H32A, H32B, H32C, H19A, H19B, H19C, H20A,
  H20B, H20C, H22A, H22B, H22C, H23A, H23B, H23C, H25A, H25B, H25C, H26A, H26B,
 H26C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C50, C54, C55, C57, C53, C55, C56, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H54C)=Sof(H54D)=Sof(H56C)=Sof(H56D)=Sof(C57)=Sof(H57A)=Sof(H57B)=1-FVAR(1)
 Sof(H54A)=Sof(H54B)=Sof(H56A)=Sof(H56B)=Sof(C55)=Sof(H55A)=Sof(H55B)=FVAR(1)
 Sof(H50C)=Sof(H50D)=Sof(H52C)=Sof(H52D)=Sof(C51)=Sof(H51A)=Sof(H51B)=1-FVAR(2)
 Sof(H50A)=Sof(H50B)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H52A)=Sof(H52B)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C15(H15), C18(H18), C21(H21), C24(H24)
4.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C54(H54C,H54D), C56(H56A,H56B), C56(H56C,H56D), C50(H50A,
 H50B), C50(H50C,H50D), C53(H53A,H53B), C55(H55A,H55B), C52(H52A,H52B),
 C52(H52C,H52D), C57(H57A,H57B), C51(H51A,H51B)
4.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), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8)
;