Adducts of aqua complexes of Ln3+ with a di-hydroxylated symmetrical octamethyl-substituted cucurbituril: potential applications for isolation of heavier lanthanides
Shen, Fang-Fang; Chen, Kai; Hua, Zi-Yi; Wang, Yuan; Xu, Jing; Chen, Mindong; Zhang, Yun-Qian; Tao, Zhu; CrystEngComm  (2017) –; doi:10.1039/C7CE01365E

data_7228943
_publ_section_title
;
 Adducts of aqua complexes of Ln3+ with a di-hydroxylated symmetrical
 octamethyl-substituted cucurbituril: potential applications for isolation
 of heavier lanthanides
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01365E
_journal_year                    2017
_chemical_formula_moiety
'C44 H52 N24 O14, Gd H16 O8, 2(N O3), Cl, 8(H2 O)'
_chemical_formula_sum            'C44 H84 Cl Gd N26 O36'
_chemical_formula_weight         1746.07
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.573(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.316(5)
_cell_length_b                   12.427(3)
_cell_length_c                   26.976(6)
_cell_measurement_temperature    223(2)
_cell_volume                     6908(3)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10314
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_T_max  0.8334
_exptl_absorpt_correction_T_min  0.7839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3596
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
;
_refine_diff_density_max         2.069
_refine_diff_density_min         -3.464
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         5781
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      3.729
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+249.5343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2462
_refine_ls_wR_factor_ref         0.2541
_reflns_number_gt                4781
_reflns_number_total             5781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce01365e2.cif
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7228943