Temperature-induced Reversible Single-Crystal-to-Single-Crystal Isomerisation of Uranyl Polyrotaxane: An Exquisite Case of Coordination Variability of Uranyl Center
Xie, Zhen-ni; Mei, Lei; Wu, Qunyan; Hu, Kong-qiu; Xia, Liang-Shu; Chai, Zhifang; Shi, Weiqun; Dalton Trans.  (2017) –; doi:10.1039/C7DT01034F

data_7042838
_publ_section_title
;
 Temperature-induced Reversible Single-Crystal-to-Single-Crystal
 Isomerisation of Uranyl Polyrotaxane: An Exquisite Case of Coordination
 Variability of Uranyl Center
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01034F
_journal_year                    2017
_chemical_formula_sum            'C108 H112 Br2 N52 O34 U'
_chemical_formula_weight         3080.34
_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
_audit_update_record
;
2017-02-22 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.387(3)
_cell_angle_beta                 98.122(4)
_cell_angle_gamma                94.716(4)
_cell_formula_units_Z            1
_cell_length_a                   12.6946(10)
_cell_length_b                   14.7727(11)
_cell_length_c                   17.0721(12)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      3.00
_cell_volume                     3158.2(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      170(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56722
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.998
_exptl_absorpt_coefficient_mu    2.018
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       block
_exptl_crystal_F_000             1558
_refine_diff_density_max         3.034
_refine_diff_density_min         -2.991
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       0.0075(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         14362
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+42.3265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2330
_refine_ls_wR_factor_ref         0.2472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12235
_reflns_number_total             14362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01034f2.cif
_cod_data_source_block           6-IMS-170K
_cod_database_code               7042838
_shelxl_version_number           2014-3
_shelx_res_checksum              76517
_shelx_fab_checksum              67524