Insertion, protonolysis and photolysis reactivity of a thorium monoalkyl amidinate complex.
Settineri, Nicholas S.; Arnold, John; Chemical science 9 (2018) 2831–2841; doi:10.1039/c7sc05328b

data_1548920
_publ_section_title
;
 Insertion, protonolysis and photolysis reactivity of a thorium monoalkyl
 amidinate complex.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2831
_journal_page_last               2841
_journal_paper_doi               10.1039/c7sc05328b
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C29 H62 N6 O Si Th'
_chemical_formula_weight         770.97
_chemical_name_systematic        Th(OC(CH2)SiMe3)(BIMA)3
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-14 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                103.843(10)
_cell_angle_beta                 97.592(10)
_cell_angle_gamma                93.871(12)
_cell_formula_units_Z            4
_cell_length_a                   12.986(4)
_cell_length_b                   16.992(5)
_cell_length_c                   17.337(4)
_cell_measurement_reflns_used    9584
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.24
_cell_volume                     3662.3(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Mercury
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            118651
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.469
_diffrn_reflns_theta_max         26.469
_diffrn_reflns_theta_min         1.224
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    4.132
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       Block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_refine_diff_density_max         3.302
_refine_diff_density_min         -2.439
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         15074
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0157P)^2^+8.2466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12934
_reflns_number_total             15074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05328b2.cif
_cod_data_source_block           Th(OC(CH2)SiMe3)(BIMA)3
_cod_depositor_comments
;

2019-07-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1548917--1548927.cif.
;
_cod_original_cell_volume        3662.2(17)
_cod_original_formula_sum        'C58 H124 N12 O2 Si2 Th2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1541.94
_cod_database_code               1548920
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.380
_shelx_estimated_absorpt_t_max   0.576
_shelx_res_checksum              73271