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_4345524
_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            'C27 H34 N13 O17 S U'
_chemical_formula_weight         1082.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 110.6498(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1824(2)
_cell_length_b                   21.4688(2)
_cell_length_c                   12.25055(17)
_cell_measurement_reflns_used    7096
_cell_measurement_temperature    296.44(10)
_cell_measurement_theta_max      28.8860
_cell_measurement_theta_min      3.5080
_cell_volume                     3490.39(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,

;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,

;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies
;
_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      296.44(10)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14851
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.070
_exptl_absorpt_coefficient_mu    4.810
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.83392
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_description       prism-like
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         6137
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+3.9993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4792
_reflns_number_total             6137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02515_si_002.cif
_cod_data_source_block           UPS1
_cod_original_cell_volume        3490.40(9)
_cod_database_code               4345524
_shelxl_version_number           2014-3
_shelx_res_checksum              39556
_shelx_hkl_checksum              5159