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_4303874
_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         'C48 H56 N8 O18 S8 U2, 5.33(C H4 O)'
_chemical_formula_sum            'C53.33 H77.2 N8 O23.33 S8 U2'
_chemical_formula_weight         1936.35
_chemical_melting_point          ?
_chemical_name_common
'Et-3,4-Thiophene-bis-Me-3,2-HOPO, uranyl dimer, methanol solvate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.808(6)
_cell_angle_beta                 90.613(6)
_cell_angle_gamma                109.875(6)
_cell_formula_units_Z            2
_cell_length_a                   12.472(5)
_cell_length_b                   16.603(7)
_cell_length_c                   18.674(7)
_cell_measurement_reflns_used    5870
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      25.296
_cell_measurement_theta_min      2.633
_cell_volume                     3546(2)
_computing_cell_refinement       'SAINT V7.60A'
_computing_data_collection       'Bruker APEX2 v2009.3-0'
_computing_data_reduction        'SAINT V7.60A'
_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      143(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans and phi 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  0.0593
_diffrn_reflns_av_sigmaI/netI    0.1286
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24740
_diffrn_reflns_theta_full        25.54
_diffrn_reflns_theta_max         25.54
_diffrn_reflns_theta_min         2.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.875
_exptl_absorpt_correction_T_max  0.6964
_exptl_absorpt_correction_T_min  0.3638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         8.789
_refine_diff_density_min         -3.062
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         12742
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0794
_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^)+(0.1239P)^2^+11.9873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1997
_refine_ls_wR_factor_ref         0.2271
_reflns_number_gt                7789
_reflns_number_total             12742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901815b_si_001_3.cif
_cod_data_source_block           gs7077b
_cod_depositor_comments
;
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 
;
_cod_original_formula_sum        'C53.33 H77.20 N8 O23.33 S8 U2'
_cod_database_code               4303874