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_4345527
_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            'C31 H30 N13 O21 U2'
_chemical_formula_weight         1396.74
_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   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                97.075(8)
_cell_angle_beta                 109.271(7)
_cell_angle_gamma                104.827(7)
_cell_formula_units_Z            2
_cell_length_a                   11.5890(19)
_cell_length_b                   12.452(2)
_cell_length_c                   16.987(3)
_cell_measurement_reflns_used    9402
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      3.01
_cell_volume                     2178.3(7)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60375
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.736
_exptl_absorpt_coefficient_mu    7.521
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_description       block
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.722
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+21.4540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8121
_reflns_number_total             9948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02515_si_002.cif
_cod_data_source_block           UPO3
_cod_original_cell_volume        2178.4(7)
_cod_database_code               4345527
_shelxl_version_number           2014-3
_shelx_res_checksum              80952
_shelx_hkl_checksum              42383
_shelx_fab_checksum              21652