Si‒H addition followed by C‒H bond activation induced by a terminal thorium imido metallocene: a combined experimental and computational study
Ren, Wenshan; Zhou, Enwei; Fang, Bo; Zi, Guofu; Fang, De-Cai; Walter, Marc D.; Chemical Science 5 (2014) 3165–; doi:10.1039/c4sc00576g

data_1516590
_publ_section_title
;
 Si--H addition followed by C--H bond activation induced by a terminal
 thorium imido metallocene: a combined experimental and computational
 study
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              3165
_journal_paper_doi               10.1039/c4sc00576g
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C54 H87 N3 Th'
_chemical_formula_sum            'C54 H87 N3 Th'
_chemical_formula_weight         1010.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.787(3)
_cell_angle_beta                 92.250(3)
_cell_angle_gamma                109.072(3)
_cell_formula_units_Z            2
_cell_length_a                   10.436(2)
_cell_length_b                   15.509(3)
_cell_length_c                   20.314(4)
_cell_measurement_reflns_used    8388
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.32
_cell_volume                     3098.4(10)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10908
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    2.436
_exptl_absorpt_correction_T_max  0.7755
_exptl_absorpt_correction_T_min  0.4070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         5.744
_refine_diff_density_min         -7.006
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         10908
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1431P)^2^+26.0755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2304
_reflns_number_gt                9578
_reflns_number_total             10908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00576g2.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 1516588--1516590.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1516590