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_4085417
_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         'C28 H67 N5 Si3 Th'
_chemical_formula_sum            'C28 H67 N5 Si3 Th'
_chemical_formula_weight         790.17
_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, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.754(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0050(4)
_cell_length_b                   23.2032(8)
_cell_length_c                   16.5776(6)
_cell_measurement_reflns_used    17447
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.149
_cell_volume                     3813.3(2)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.34 (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_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                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36814
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.438
_diffrn_reflns_theta_min         2.149
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.027
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.2815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/2 (Bruker,2007) was used for absorption correction. wR2(int) was 
0.1134 before and 0.0505 after correction. The Ratio of minimum to maximum 
transmission is 0.6539. The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.746
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         8678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+3.4221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7814
_reflns_number_total             8678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501177s_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4085415--4085420.cif.'
_cod_database_code               4085417
_nottingham_internal_coll_name   THBGLr
_nottingham_internal_coll_number 12061
_nottingham_internal_coll_client pczbg
_nottingham_internal_coll_type   hemisphere
_nottingham_internal_coll_frame_time 15
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   pczbg
_nottingham_internal_coll_date   26/11/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user pczbg
_nottingham_internal_process_date 28/11/2012
_nottingham_internal_solution_user pczbg
_nottingham_internal_solution_date 27/11/2012
_nottingham_internal_refinement_user pczbg
_nottingham_internal_refinement_date 28/11/2012
_nottingham_internal_self_validation_user pczbg
_nottingham_internal_self_validation_date 02/10/2014
_nottingham_internal_self_archive_date 02/10/2014
_nottingham_internal_validation_user pczwl
_nottingham_internal_validation_date 10/11/2014
_nottingham_internal_archive_date 10/11/2014
_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.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), C25(H25A,H25B), C27(H27A,H27B)
2.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), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id THBGLR
_olex2_submission_special_instructions 'No special instructions were received'