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_4067527
_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            'C48 H72 Cl2 Li2 N4 O8 Th'
_chemical_formula_weight         1149.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 112.910(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.323(4)
_cell_length_b                   13.882(3)
_cell_length_c                   22.994(5)
_cell_measurement_reflns_used    2073
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.22
_cell_volume                     5387(2)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39355
_diffrn_reflns_theta_full        24.69
_diffrn_reflns_theta_max         24.69
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    2.918
_exptl_absorpt_correction_T_max  0.7591
_exptl_absorpt_correction_T_min  0.5291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.254
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         9095
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0588P)^2^+15.5627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                6826
_reflns_number_total             9095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900996n_si_002.cif
_cod_data_source_block           complex5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        5387.4(19)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4067527