Reactivity of Organothorium Complexes with TEMPO.
Langeslay, Ryan R.; Walensky, Justin R.; Ziller, Joseph W.; Evans, William J.; Inorganic chemistry 53 (2014) 8455–8463; doi:10.1021/ic501034b

data_4340563
_publ_section_title
;
 Reactivity of Organothorium Complexes with TEMPO.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8455
_journal_page_last               8463
_journal_paper_doi               10.1021/ic501034b
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C32 H53 N O Th'
_chemical_formula_weight         699.79
_chemical_name_systematic
; 
 ? 
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 112.4316(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8295(10)
_cell_length_b                   10.0546(6)
_cell_length_c                   19.3499(11)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.32
_cell_volume                     3026.5(3)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2011.4-1, 2011'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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  0.0203
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33857
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         1.368
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.950
_exptl_absorpt_correction_T_max  0.4824
_exptl_absorpt_correction_T_min  0.2752
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.224
_refine_diff_density_max         1.460
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         6837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+2.7403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6353
_reflns_number_total             6837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501034b_si_002.cif
_cod_data_source_block           rrl6
_cod_depositor_comments
;Adding full bibliography for 4340558--4340566.cif.

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 
;
_cod_database_code               4340563
_shelx_estimated_absorpt_t_min   0.267
_shelx_estimated_absorpt_t_max   0.404
_shelxl_version_number           2013-3
_shelx_res_checksum              99376
_shelx_hkl_checksum              46057