Chemical controls on uranyl citrate speciation and the self-assembly of nanoscale macrocycles and sandwich complexes in aqueous solutions
M. Basile; D. K. Unruh; K. Gojdas; E. Flores; L. Streicher; T. Z. Forbes; Chem.Commun. 51 (2015) 5306–; doi:10.1039/C4cc08657K

data_7116774
_publ_section_title
;
 Chemical controls on uranyl citrate speciation and the self-assembly of
 nanoscale macrocycles and sandwich complexes in aqueous solutions
;
_journal_name_full               Chem.Commun.
_journal_page_first              5306
_journal_paper_doi               10.1039/C4cc08657K
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C60 H96 N12 Na4 O94 U6'
_chemical_formula_weight         4009.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   const
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-22T16:30:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-10-28 deposited with the CCDC.
2014-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                68.4670(13)
_cell_angle_beta                 64.4190(13)
_cell_angle_gamma                67.9600(13)
_cell_formula_units_Z            2
_cell_length_a                   19.9870(8)
_cell_length_b                   20.5879(8)
_cell_length_c                   21.1208(8)
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.12
_cell_measurement_theta_min      2.21
_cell_volume                     7044.4(5)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CrystalMaker v2.7.7'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            169407
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
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_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         1.286
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_exptl_absorpt_correction_T_max  0.0506
_exptl_absorpt_correction_T_min  0.0173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
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_exptl_crystal_description       prism
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_exptl_crystal_size_max          0.23
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_refine_diff_density_max         5.883
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_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         39483
_refine_ls_number_restraints     1867
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_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+40.5825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                34170
_reflns_number_total             39483
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           U3
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_shelxl_version_number           2014/6
_shelx_res_checksum              83849