Monomeric Thorium Dihydrido Complex: A Versatile Precursor to Actinide Metallacycles
Qin, Guorui; Wang, Yang; Shi, Xianghui; del Rosal, Iker; Laurent, Maron; Cheng, Jianhua; Chemical Communications  (2019) –; doi:10.1039/C9CC04013G

data_7123737
_publ_section_title
;
 Monomeric Thorium Dihydrido Complex: A Versatile Precursor to Actinide
 Metallacycles
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04013G
_journal_year                    2019
_chemical_formula_moiety         'C99  H132  Th1'
_chemical_formula_sum            'C99 H132 Th'
_chemical_formula_weight         1554.08
_chemical_name_common            '[(CpAr)Th(CH2-C6H4-CH3)3]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-06-22 deposited with the CCDC.    2019-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.1160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9020(5)
_cell_length_b                   16.9604(3)
_cell_length_c                   47.2064(9)
_cell_measurement_reflns_used    70443
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.409
_cell_measurement_theta_min      0.890
_cell_volume                     20112.0(7)
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            62628
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.456
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Sheldrick, G. M. SADABS, Version 2.10; Bruker AXS, Inc.: Madison, WI 2003.'
_exptl_crystal_colour            Pale-Yellow
_exptl_crystal_density_diffrn    1.026
_exptl_crystal_description       Block
_exptl_crystal_F_000             6528
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.685
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         17013
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0764P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11768
_reflns_number_total             17013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04013g2.cif
_cod_data_source_block           D033
_cod_original_cell_volume        20111.9(7)
_cod_database_code               7123737
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.676
_shelx_estimated_absorpt_t_max   0.751
_shelx_res_checksum              24855
_shelx_fab_checksum              40088