Thorium Triamidoamine Complexes: Synthesis of an Unusual Dinuclear Tuck-in‒Tuck-over Thorium Metallacycle Featuring the Longest Known Thorium−σ-Alkyl Bond
Gardner, Benedict M.; Lewis, William; Blake, Alexander J.; Liddle, Stephen T.; Organometallics 34 (2015) 2386–; doi:10.1021/om501177s

data_4085416
_publ_section_title
;
 Thorium Triamidoamine Complexes: Synthesis of an Unusual Dinuclear
 Tuck-in--Tuck-over Thorium Metallacycle Featuring the Longest Known
 Thorium&#x2212;\s-Alkyl Bond
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2386
_journal_paper_doi               10.1021/om501177s
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C24 H57 I N4 Si3 Th'
_chemical_formula_sum            'C24 H57 I N4 Si3 Th'
_chemical_formula_weight         844.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.20 svn.r3092 for OlexSys, GUI svn.r4949)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.547(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7217(9)
_cell_length_b                   22.435(2)
_cell_length_c                   16.0507(15)
_cell_measurement_reflns_used    12828
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.49
_cell_volume                     3470.4(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34380
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.569
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.308
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.2309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/2 (Bruker,2007) was used for absorption correction.
wR2(int) was 0.1478 before and 0.0806 after correction.
The Ratio of minimum to maximum transmission is 0.5364.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.04
_refine_diff_density_max         6.879
_refine_diff_density_min         -5.152
_refine_diff_density_rms         0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6117
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0785
_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^)+(0.0722P)^2^+229.7088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2000
_refine_ls_wR_factor_ref         0.2214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4298
_reflns_number_total             6117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501177s_si_001.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4085415--4085420.cif.'
_cod_database_code               4085416
_nottingham_internal_coll_name   THBGLI
_nottingham_internal_coll_number 12008
_nottingham_internal_coll_client BMG/STL
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_method '\w and \f scans'
_nottingham_internal_coll_frame_time '10 s'
_nottingham_internal_coll_frame_width '0.3 and 0.5 degrees'
_nottingham_internal_coll_user   pczbg
_nottingham_internal_coll_date   19/11/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 20/11/2012
_nottingham_internal_process_user pczbg
_nottingham_internal_solution_date 20/11/2012
_nottingham_internal_solution_user BMG
_nottingham_internal_refinement_date 13/10/2014
_nottingham_internal_refinement_user BMG
_nottingham_internal_self_archive_date 13/10/2014
_nottingham_internal_self_validation_date 13/10/2014
_nottingham_internal_self_validation_user BMG
_nottingham_internal_validation_date 21/11/2014
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 21/11/2014
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B),
 C24(H24A,H24B)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_hkl_checksum              9021
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'