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_7032844
_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         'C37 H64 O2 Si2 Th'
_chemical_formula_sum            'C37 H64 O2 Si2 Th'
_chemical_formula_weight         829.10
_chemical_name_common            complex_8_formate
_chemical_name_systematic
;
bis(mu-formato)bis{(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
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                95.881(3)
_cell_angle_beta                 113.241(3)
_cell_angle_gamma                113.851(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9293(4)
_cell_length_b                   13.9229(6)
_cell_length_c                   14.3584(5)
_cell_measurement_reflns_used    6926
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.7040
_cell_measurement_theta_min      3.2480
_cell_volume                     1904.24(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    0.00   53.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2445   38.0000 -180.0000 53

  2 omega   -3.00   41.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2445  -99.0000  -90.0000 44

  3 omega  -10.00   82.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2445   77.0000 -180.0000 92

  4 omega   -9.00   82.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2445   77.0000  -30.0000 91

  5 omega   17.00   82.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2445   77.0000   30.0000 65

  6 omega  -28.00   41.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2445  -19.0000    0.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0088997000
_diffrn_orient_matrix_UB_12      -0.0471160000
_diffrn_orient_matrix_UB_13      0.0035522000
_diffrn_orient_matrix_UB_21      -0.0363900000
_diffrn_orient_matrix_UB_22      -0.0218665000
_diffrn_orient_matrix_UB_23      -0.0564586000
_diffrn_orient_matrix_UB_31      0.0639004000
_diffrn_orient_matrix_UB_32      0.0271795000
_diffrn_orient_matrix_UB_33      -0.0012109000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14686
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.680
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.007
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.938
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6696
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0466P)^2^+0.0920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5718
_reflns_number_total             6696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02362e2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7032839--7032844.cif.'
_cod_original_cell_volume        1904.23(14)
_cod_database_code               7032844
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C29, C28, C27, C31, C30, C34, C33, C32, C36, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C29 \\sim C28 \\sim C27 \\sim C31 \\sim C30 \\sim C34 \\sim C33 \\sim C32 \\sim
C36 \\sim C35: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
4.a Ternary CH refined with riding coordinates:
 C24(H24), C18(H18), C15(H15), C21(H21), C12(H12), C9(H9)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C7(H7), C37(H37), C6(H6)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C10(H10A,H10B,H10C), C23(H23A,
 H23B,H23C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C),
 C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C11(H11A,H11B,H11C), C26(H26A,H26B,
 H26C), C33(H33A,H33B,H33C), C25(H25A,H25B,H25C)
;