Thorium(IV) Complexes of Bidentate Hydroxypyridinonates1
Jide Xu; Donald W. Whisenhunt; Alan C. Veeck; Linda C. Uhlir; Kenneth N. Raymond; Inorganic Chemistry 42 (2003) 2665–2674; doi:10.1021/ic0259888

data_4313478
_publ_contact_author
;
Kenneth N. Raymond
Department of Chemistry
University of California
Berkeley, CA  94720-1460
;
_publ_contact_author_email       raymond@socrates.berkeley.edu
_publ_contact_author_fax         510-486-5283
_publ_contact_author_phone       510-642-7219
_publ_section_title
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 Thorium(IV) Complexes of Bidentate Hydroxypyridinonates1
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2665
_journal_page_last               2674
_journal_paper_doi               10.1021/ic0259888
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[Th(C10H13N2O3)4] H2O'
_chemical_formula_sum            'C40 H54 N8 O13 Th'
_chemical_formula_weight         1086.95
_chemical_name_common            ThPR-Me-3,2-HOPO
_chemical_name_systematic
; 
 Thorium tetrakis(1-Methyl-2-oxo-4-propylcarbamoyl-1,2-dihydro-pyridin-3-olate)

;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   17.1250(5)
_cell_length_b                   12.3036(7)
_cell_length_c                   23.8803(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    132(2)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      2.66
_cell_volume                     5031.6(4)
_computing_cell_refinement
; 
SMART (Siemens, 1995) SAINT (Siemens, 1995) 
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
; 
SAINT (Siemens, 1995) XPREP (Siemens, 1995) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      132(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  '3 circle diffractomter'
_diffrn_measurement_method       'omega scan with profile analysis'
_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  0.0838
_diffrn_reflns_av_sigmaI/netI    0.1005
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17640
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.027
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         6581
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+1.1599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                4606
_reflns_number_total             6581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0259888si20030220_022322.cif
_cod_data_source_block           ThPR32HOPO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4313478