Mixed-Ligand Uranyl Polyrotaxanes Incorporating a Sulfate/Oxalate Coligand: Achieving Structural Diversity via pH-Dependent Competitive Effect
Xie, Zhen-ni; Mei, Lei; Hu, Kong-qiu; Xia, Liang-shu; Chai, Zhi-fang; Shi, Wei-qun; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.6b02515

data_4345526
_publ_section_title
;
 Mixed-Ligand Uranyl Polyrotaxanes Incorporating a Sulfate/Oxalate
 Coligand: Achieving Structural Diversity via pH-Dependent Competitive
 Effect
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b02515
_journal_year                    2017
_chemical_formula_sum            'C56 H56 N26 O23 U'
_chemical_formula_weight         1699.29
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                87.389(2)
_cell_angle_beta                 87.387(2)
_cell_angle_gamma                72.441(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3634(7)
_cell_length_b                   12.7236(8)
_cell_length_c                   23.2444(14)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      3.08
_cell_volume                     3480.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            151732
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.076
_exptl_absorpt_coefficient_mu    2.427
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       lath-like
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         15928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+5.7245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14737
_reflns_number_total             15928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02515_si_002.cif
_cod_data_source_block           UPO2
_cod_database_code               4345526
_shelxl_version_number           2014-3
_shelx_res_checksum              22977
_shelx_hkl_checksum              82544
_shelx_fab_checksum              11086