Designing the Ideal Uranyl Ligand: a Sterically Induced Speciation Change in Complexes with Thiophene-Bridged Bis(3-hydroxy-N-methylpyridin-2-one)(1)
Géza Szigethy; Kenneth N. Raymond; Inorganic Chemistry 48 (2009) 11489–11491; doi:10.1021/ic901815b

data_4303872
_publ_section_title
;
Designing the Ideal Uranyl Ligand: a Sterically Induced Speciation Change
in Complexes with Thiophene-Bridged Bis(3-hydroxy-N-methylpyridin-2-one)(1)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11489
_journal_page_last               11491
_journal_paper_doi               10.1021/ic901815b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C21 H21 N5 O9 S U'
_chemical_formula_sum            'C21 H21 N5 O9 S U'
_chemical_formula_weight         757.52
_chemical_melting_point          ?
_chemical_name_common
;
3,4-thiophene-bis-Me-3,2-HOPO uranyl complex
;
_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                   7.1702(9)
_cell_length_b                   16.166(2)
_cell_length_c                   20.461(3)
_cell_measurement_reflns_used    2085
_cell_measurement_temperature    156(2)
_cell_measurement_theta_max      22.208
_cell_measurement_theta_min      2.520
_cell_volume                     2371.7(5)
_computing_cell_refinement       'SAINT v.7.07'
_computing_data_collection       'Bruker SMART v.6.531'
_computing_data_reduction        'SAINT v.7.07'
_computing_molecular_graphics    'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32'
_computing_publication_material  'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      156(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-I'
_diffrn_measurement_method       \w-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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12701
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.995
_exptl_absorpt_correction_T_max  0.8176
_exptl_absorpt_correction_T_min  0.4874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.738
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(13)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4534
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                3064
_reflns_number_total             4534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901815b_si_001_1.cif
_cod_data_source_block           gs4126
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4303872