Preparation of (η5-C5Me5)2Th(bipy) and Its Reactivity toward Small Molecules
Yang, Pikun; Zhou, Enwei; Fang, Bo; Hou, Guohua; Zi, Guofu; Walter, Marc D.; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00357

data_4086518
_publ_section_title
;
 Preparation of (\h5-C5Me5)2Th(bipy) and Its Reactivity toward Small
 Molecules
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00357
_journal_year                    2016
_chemical_formula_moiety         'C50 H56 N2 S Th'
_chemical_formula_sum            'C50 H56 N2 S Th'
_chemical_formula_weight         949.06
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                93.160(2)
_cell_angle_beta                 103.261(2)
_cell_angle_gamma                98.499(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4662(10)
_cell_length_b                   11.7308(11)
_cell_length_c                   17.3984(16)
_cell_measurement_reflns_used    3382
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.25
_cell_measurement_theta_min      2.27
_cell_volume                     2047.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14073
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.623
_diffrn_reflns_theta_min         2.043
_exptl_absorpt_coefficient_mu    3.730
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_refine_diff_density_max         1.568
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         9402
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7955
_reflns_number_total             9402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00357_si_002.cif
_cod_data_source_block           compound11
_cod_database_code               4086518
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.433
_shelx_estimated_absorpt_t_max   0.508
_shelx_res_checksum              73244
_shelx_hkl_checksum              99164