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_7116772
_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_moiety         'C12 H14 O20 U2, C4 H12 N2, 4(H2 O)'
_chemical_formula_sum            'C16 H34 N2 O24 U2'
_chemical_formula_weight         1114.51
_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_date             2014-03-28T08:11:53-00:00
_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                94.6846(18)
_cell_angle_beta                 98.8324(18)
_cell_angle_gamma                104.5031(17)
_cell_formula_units_Z            1
_cell_length_a                   6.3074(4)
_cell_length_b                   10.0063(6)
_cell_length_c                   11.9920(7)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.56
_cell_volume                     718.32(8)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.998
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14292
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.9
_exptl_absorpt_coefficient_mu    11.363
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocky
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.373
_refine_diff_density_min         -1.87
_refine_diff_density_rms         0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+5.5226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                3166
_reflns_number_total             3280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc08657k2.cif
_cod_data_source_block           U2pip
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7116772