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_7123738
_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         'C89  H130  O1  Th1'
_chemical_formula_sum            'C89 H130 O Th'
_chemical_formula_weight         1447.96
_chemical_name_common            '[(CpAr*)(Cp*)ThH2(THF)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_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                97.141(3)
_cell_angle_beta                 95.688(2)
_cell_angle_gamma                118.572(3)
_cell_formula_units_Z            2
_cell_length_a                   14.7237(17)
_cell_length_b                   14.9064(17)
_cell_length_c                   24.091(3)
_cell_measurement_reflns_used    26331
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.462
_cell_measurement_theta_min      1.599
_cell_volume                     4530.6(9)
_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    'SUPERFLIP(Palatinus & Chapuis 2007)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.1487
_diffrn_reflns_av_unetI/netI     0.4174
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23279
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.135
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.733
_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            Colorless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             1524
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.126
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         15513
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.2170
_refine_ls_R_factor_gt           0.0941
_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^)+(0.0485P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6057
_reflns_number_total             15513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04013g2.cif
_cod_data_source_block           D082
_cod_original_cell_volume        4530.7(9)
_cod_database_code               7123738
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.740
_shelx_estimated_absorpt_t_max   0.824
_shelx_res_checksum              2305
_shelx_fab_checksum              53417