Influence of Linker Geometry on Uranyl Complexation by Rigidly Linked Bis(3-hydroxy-N-methyl-pyridin-2-one)
Géza Szigethy; Kenneth N. Raymond; Inorganic Chemistry 49 (2010) 6755–6765; doi:10.1021/ic1007878

data_4316084
_publ_section_title
;
 Influence of Linker Geometry on Uranyl Complexation by Rigidly Linked
 Bis(3-hydroxy-N-methyl-pyridin-2-one)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6755
_journal_page_last               6765
_journal_paper_doi               10.1021/ic1007878
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C22 H22 N4 O9 U, C2 H6 O S'
_chemical_formula_sum            'C24 H28 N4 O10 S U'
_chemical_formula_weight         802.59
_chemical_melting_point          ?
_chemical_name_common            uranyl-3-aminomethylaniline(Me-3,2-HOPO)2
_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                64.277(3)
_cell_angle_beta                 75.544(3)
_cell_angle_gamma                71.472(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8897(18)
_cell_length_b                   13.317(3)
_cell_length_c                   13.577(3)
_cell_measurement_reflns_used    1583
_cell_measurement_temperature    165(2)
_cell_measurement_theta_max      19.546
_cell_measurement_theta_min      2.438
_cell_volume                     1361.2(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      165(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7628
_diffrn_reflns_theta_full        24.44
_diffrn_reflns_theta_max         24.44
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.102
_exptl_absorpt_correction_T_max  0.7110
_exptl_absorpt_correction_T_min  0.4613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       wedge
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         4443
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0508P)^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         0.0956
_reflns_number_gt                3704
_reflns_number_total             4443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1007878_si_002_4.cif
_cod_data_source_block           mtolhp
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/adriana/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_enum 1555 2011-01-17 13:19:09Z saulius 

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 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_database_code               4316084