Synthesis, structure, and reactivity of crystalline molecular complexes of the {[C5H3(SiMe3)2]3Th}1−anion containing thorium in the formal +2 oxidation state
Langeslay, Ryan R.; Fieser, Megan E.; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Chem. Sci. 6 (2015) 517–; doi:10.1039/C4SC03033H

data_1518167
_publ_section_title
;
 Synthesis, structure, and reactivity of crystalline molecular complexes
 of the {[C5H3(SiMe3)2]3Th}1&#x2212;anion containing thorium in the formal
 +2 oxidation state
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              517
_journal_paper_doi               10.1039/C4SC03033H
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C51 H99 K N2 O6 Si6 Th'
_chemical_formula_weight         1276.00
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                100.9296(8)
_cell_angle_beta                 104.4481(8)
_cell_angle_gamma                95.5814(8)
_cell_formula_units_Z            2
_cell_length_a                   12.1595(8)
_cell_length_b                   12.7622(8)
_cell_length_c                   22.2587(14)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.23
_cell_volume                     3246.1(4)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2013.10-0, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      138(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker SMART 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  0.0445
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38800
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.750
_diffrn_reflns_theta_min         1.644
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.513
_exptl_absorpt_correction_T_max  0.9194
_exptl_absorpt_correction_T_min  0.6059
_exptl_absorpt_correction_type   numerical
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_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.307
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_refine_diff_density_max         0.835
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_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         15230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13490
_reflns_number_total             15230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03033h3.cif
_cod_data_source_block           rrl19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 1518167--1518170.cif.
;
_cod_original_cell_volume        3246.0(4)
_cod_database_code               1518167
_shelx_estimated_absorpt_t_min   0.513
_shelx_estimated_absorpt_t_max   0.872
_shelxl_version_number           2014-2
_shelx_res_checksum              72489