Mixed-anion templated cage-like lanthanide clusters: Gd27 and Dy27
Zheng, Xiu-Ying; Peng, Jun-Bo; Kong, Xiang-Jian; Long, La-Sheng; Zheng, Lan-Sun; Inorganic Chemistry Frontiers 3 (2016) 320–; doi:10.1039/C5QI00249D

data_4349073
_publ_section_title
;
 Mixed-anion templated cage-like lanthanide clusters: Gd27 and Dy27
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              320
_journal_paper_doi               10.1039/C5QI00249D
_journal_volume                  3
_journal_year                    2016
_chemical_formula_sum            'C68 H310 Cl13 Gd27 O247'
_chemical_formula_weight         9787.76
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-11-06 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                77.642(2)
_cell_angle_beta                 74.776(2)
_cell_angle_gamma                69.343(2)
_cell_formula_units_Z            2
_cell_length_a                   19.0866(5)
_cell_length_b                   20.1645(4)
_cell_length_c                   32.8057(7)
_cell_measurement_reflns_used    13470
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.9840
_cell_measurement_theta_min      3.2090
_cell_volume                     11296.2(5)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_sigmaI/netI    0.1039
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            135113
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    8.107
_exptl_absorpt_correction_T_max  0.2939
_exptl_absorpt_correction_T_min  0.1947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9286
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         5.228
_refine_diff_density_min         -2.786
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constro
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2425
_refine_ls_number_reflns         39691
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.150
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                26490
_reflns_number_total             39691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qi00249d2.cif
_cod_data_source_block           Gd27
_cod_original_cell_volume        11296.2(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4349073
_platon_gd27_details
;
Because of disorder, 5 ClO4- and 50 water molecules were omited per 
formula unit. This valueis calculated based upon elemental analysis data,
and TGA data.
;