In Search of Tris(Trimethylsilylcyclopentadienyl) Thorium
Wedal, Justin C.; Bekoe, Samuel; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Dalton Transactions  (2019) –; doi:10.1039/C9DT03674A

data_7701390
_publ_section_title
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 In Search of Tris(Trimethylsilylcyclopentadienyl) Thorium
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03674A
_journal_year                    2019
_chemical_formula_sum            'C48 H78 O Si6 Th2'
_chemical_formula_weight         1303.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-09-10 deposited with the CCDC.    2019-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.9575(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5444(6)
_cell_length_b                   18.4598(11)
_cell_length_c                   15.7099(10)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      29.15
_cell_measurement_theta_min      2.53
_cell_volume                     2686.2(3)
_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      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.944
_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  0.0256
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.155
_diffrn_reflns_theta_min         1.732
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.695
_exptl_absorpt_correction_T_max  0.4319
_exptl_absorpt_correction_T_min  0.3096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0162
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+1.0857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0320
_refine_ls_wR_factor_ref         0.0331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6208
_reflns_number_total             6849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03674a2.cif
_cod_data_source_block           jcw5
_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 
;
_cod_database_code               7701390
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.256
_shelx_estimated_absorpt_t_max   0.568
_exptl_absorpt_special_details
; 
Reflections not merged 
33446 Corrected reflections written to file jcw5s.hkl 
Estimated minimum and maximum transmission:  0.3096  0.4319 
The ratio (0.7168) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.6000 
Lambda/2 correction factor = 0.00150 
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_shelx_res_checksum              53883