Two Three-Dimensional 2p-3d-4f Heterometallic Frameworks Featuring a Ln6Cu24Na12 Cluster as a Node
Gui-Lin Zhuang; Wen-Xian Chen; Hai-Xia Zhao; Xiang-Jian Kong; La-Sheng Long; Rong-Bin Huang; Lan-Sun Zheng; Inorganic Chemistry 50 (2011) 3843–3845; doi:10.1021/ic200077r

data_4324987
_publ_section_title
;
 Two Three-Dimensional 2p-3d-4f Heterometallic Frameworks Featuring a
 Ln6Cu24Na12 Cluster as a Node
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3843
_journal_page_last               3845
_journal_paper_doi               10.1021/ic200077r
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C60 H288 Cl5 Cu24 Gd6 N25 Na12 O207'
_chemical_formula_weight         7594.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            3
_cell_length_a                   29.5532(4)
_cell_length_b                   29.5532(4)
_cell_length_c                   36.1951(7)
_cell_measurement_temperature    173(2)
_cell_volume                     27377.2(7)
_computing_cell_refinement       'CrysAlis RED'
_computing_data_collection       'CrysAlis CCD'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CrysAlis CCD, Oxford Diffraction Ltd.'
_diffrn_measurement_method       'phi and omega 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  0.1016
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            85552
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    2.575
_exptl_absorpt_correction_T_max  0.4660
_exptl_absorpt_correction_T_min  0.4257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       block
_exptl_crystal_F_000             11328
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.703
_refine_diff_density_min         -2.596
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       0.000269(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         11918
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1263P)^2^+791.1600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2284
_refine_ls_wR_factor_ref         0.2386
_reflns_number_gt                8541
_reflns_number_total             11918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200077r_si_002.cif
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4324987
_platon_complex1_details
;
SQUEEZE removed 5 disordered NO3-, 4 disordered Cl- and
48 disordered water molecules per formula unit. This valueis 
calculated based upon elemental analysis data.
;