Three Giant Lanthanide Clusters Ln37 (Ln = Gd, Tb, and Eu) Featuring A Double-Cage Structure.
Zhou, Yang; Zheng, Xiu-Ying; Cai, Jing; Hong, Zi-Feng; Yan, Zhi-Hao; Kong, Xiang-Jian; Ren, Yan-Ping; Long, La-Sheng; Zheng, Lan-Sun; Inorganic chemistry 56 (2017) 2037–2041; doi:10.1021/acs.inorgchem.6b02714

data_4345172
_publ_section_title
;
 Three Giant Lanthanide Clusters Ln37 (Ln = Gd, Tb, and Eu) Featuring A
 Double-Cage Structure.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2037
_journal_page_last               2041
_journal_paper_doi               10.1021/acs.inorgchem.6b02714
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C104 H500 Cl21 O378 Tb37'
_chemical_formula_weight         14425.42
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   48.1145(14)
_cell_length_b                   26.6472(18)
_cell_length_c                   28.6307(10)
_cell_measurement_reflns_used    2263
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.8870
_cell_measurement_theta_min      3.2070
_cell_volume                     36708(3)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.1676
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49313
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.912
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.608
_exptl_crystal_description       block
_exptl_crystal_F_000             27600
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_platon_squeeze_details
;
;
_refine_diff_density_max         4.015
_refine_diff_density_min         -2.030
_refine_diff_density_rms         0.313
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1840
_refine_ls_number_reflns         22707
_refine_ls_number_restraints     1174
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0338P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                16205
_reflns_number_total             22707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02714_si_003.cif
_cod_data_source_block           Tb37
_cod_depositor_comments
'Adding full bibliography for 4345172--4345173.cif.'
_cod_database_code               4345172
_shelx_estimated_absorpt_t_min   0.352
_shelx_estimated_absorpt_t_max   0.427
_platon_tb37_details
;
SQUEEZE removed 7 disordered ClO4- anions and 100 disordered 
water molecules per formula unit. This valueis calculated 
based upon elemental analysis data.
;
_shelxl_version_number           2013-2
_shelx_res_checksum              54329
_shelx_hkl_checksum              43323