Attempting to Reduce the Irreducible: Preparation of a Rare Paramagnetic Thorium Species
Korobkov, Ilia; Vidjayacoumar, Balamurugan; Gorelsky, Serge I.; Billone, Paul; Gambarotta, Sandro; Organometallics 29 (2010) 692–; doi:10.1021/om900996n

data_4067523
_publ_section_title
;
 Attempting to Reduce the Irreducible: Preparation of a Rare Paramagnetic
 Thorium Species
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              692
_journal_paper_doi               10.1021/om900996n
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C55.5 H78 Al3 Cl5 N4 Th2'
_chemical_formula_weight         1523.49
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.726(10)
_cell_length_b                   25.649(14)
_cell_length_c                   28.124(15)
_cell_measurement_reflns_used    1311
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.48
_cell_measurement_theta_min      2.41
_cell_volume                     12787(12)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_sigmaI/netI    0.0687
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_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            58792
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    4.933
_exptl_absorpt_correction_T_max  0.5249
_exptl_absorpt_correction_T_min  0.4387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5944
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.258
_refine_diff_density_min         -0.726
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         10651
_refine_ls_number_restraints     40
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_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+175.1906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1990
_reflns_number_gt                6736
_reflns_number_total             10651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900996n_si_002.cif
_cod_data_source_block           complex2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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_original_cell_volume        12786(12)
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C55.50 H78 Al3 Cl5 N4 Th2'
_cod_database_code               4067523