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_4345173
_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 H490 Cl21 Eu37 O378'
_chemical_formula_weight         14157.90
_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                   49.948(10)
_cell_length_b                   27.552(6)
_cell_length_c                   29.639(6)
_cell_measurement_reflns_used    174031
_cell_measurement_temperature    173(2)
_cell_volume                     40788(15)
_computing_data_collection       bluice
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'MarCCD mx300'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'synchrotron Monochr'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.0939
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            67156
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.088
_diffrn_source                   'Sychrotron X-Ray'
_exptl_absorpt_coefficient_mu    5.863
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             27304
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         2.255
_refine_diff_density_min         -2.673
_refine_diff_density_rms         0.301
_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   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1840
_refine_ls_number_reflns         36309
_refine_ls_number_restraints     1150
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+216.5794P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                35133
_reflns_number_total             36309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02714_si_004.cif
_cod_data_source_block           Eu37
_cod_depositor_comments
'Adding full bibliography for 4345172--4345173.cif.'
_cod_original_cell_volume        40788(14)
_cod_database_code               4345173
_shelx_estimated_absorpt_t_min   0.540
_shelx_estimated_absorpt_t_max   0.592
_platon_eu37_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              73323
_shelx_hkl_checksum              70484