Synthesis, Structure, and Reactivity of the Sterically Crowded Th(3+) Complex (C5Me5)3Th Including Formation of the Thorium Carbonyl, [(C5Me5)3Th(CO)][BPh4].
Langeslay, Ryan R.; Chen, Guo P.; Windorff, Cory J.; Chan, Alan K.; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Journal of the American Chemical Society 139 (2017) 3387–3398; doi:10.1021/jacs.6b10826

data_4125468
_publ_section_title
;
 Synthesis, Structure, and Reactivity of the Sterically Crowded Th(3+)
 Complex (C5Me5)3Th Including Formation of the Thorium Carbonyl,
 [(C5Me5)3Th(CO)][BPh4].
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3387
_journal_page_last               3398
_journal_paper_doi               10.1021/jacs.6b10826
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C62 H81 B O2 Th'
_chemical_formula_weight         1101.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.0068(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0198(9)
_cell_length_b                   12.6245(8)
_cell_length_c                   29.5965(19)
_cell_measurement_reflns_used    9494
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.84
_cell_measurement_theta_min      2.26
_cell_volume                     5235.2(6)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.936
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            61761
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.836
_diffrn_reflns_theta_min         1.377
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.891
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_correction_T_min  0.3153
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.557
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         12822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0278P)^2^+3.1119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10832
_reflns_number_total             12822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10826_si_004.cif
_cod_data_source_block           rrl57
_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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4125468--4125470.cif.
;
_cod_database_code               4125468
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.466
_shelx_estimated_absorpt_t_max   0.721
_shelx_res_checksum              84514
_shelx_hkl_checksum              78474
_shelx_fab_checksum              57612