(C4N2H12)3[Ln3(OH)(SO4)7] (Ln = Sm, Eu, and Tb): A Series of Honeycomb-like Open-Framework Lanthanide Sulfates with Extra-Large Channels Containing 24-Membered Rings
Deng Zhang; Yun Lu; Dunru Zhu; Yan Xu; Inorganic Chemistry 52 (2013) 3253–3258; doi:10.1021/ic3027682

data_4334221
_publ_section_title
;
 (C4N2H12)3[Ln3(OH)(SO4)7] (Ln = Sm, Eu, and Tb): A Series of
 Honeycomb-like Open-Framework Lanthanide Sulfates with Extra-Large
 Channels Containing 24-Membered Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3253
_journal_page_last               3258
_journal_paper_doi               10.1021/ic3027682
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         (C4N2H12)3[Sm3(OH)(SO4)7]
_chemical_formula_sum            'C12 H37 N6 O29 S7 Sm3'
_chemical_formula_weight         1404.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   14.3551(8)
_cell_length_b                   14.3551(8)
_cell_length_c                   10.1132(11)
_cell_measurement_reflns_used    1835
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.711
_cell_measurement_theta_min      2.595
_cell_volume                     1804.8(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13024
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    5.335
_exptl_absorpt_correction_T_max  0.6175
_exptl_absorpt_correction_T_min  0.5669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.585
_exptl_crystal_description       Block
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2365
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0085P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0462
_reflns_number_gt                2202
_reflns_number_total             2365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3027682_si_001_1.cif
_cod_data_source_block           sm
_cod_database_code               4334221