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_7116773
_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, 2(C5 H6 N), 2(H2 O)'
_chemical_formula_sum            'C22 H30 N2 O22 U2'
_chemical_formula_weight         1150.54
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-28T08:12:49-00:00
_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                100.6621(23)
_cell_angle_beta                 99.5051(23)
_cell_angle_gamma                91.0417(22)
_cell_formula_units_Z            1
_cell_length_a                   6.7978(5)
_cell_length_b                   9.8815(8)
_cell_length_c                   11.7825(9)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.48
_cell_volume                     766.15(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_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            19074
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.436
_diffrn_reflns_theta_min         3.042
_exptl_absorpt_coefficient_mu    10.654
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3482
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.015
_refine_ls_R_factor_gt           0.0134
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+0.3105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0327
_reflns_number_gt                3305
_reflns_number_total             3482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08657k2.cif
_cod_data_source_block           U2pyr
_cod_database_code               7116773
_shelx_estimated_absorpt_t_min   0.25
_shelx_estimated_absorpt_t_max   0.483
_shelxl_version_number           2013-4
_shelx_res_checksum              39960