A 4 + 4 strategy for synthesis of zeolitic metal-organic frameworks: an indium-MOF with SOD topology as a light-harvesting antenna
Libo Sun; Hongzhu Xing; Zhiqiang Liang; Jihong Yu; Ruren Xu; Chem.Commun. 49 (2013) 11155–; doi:10.1039/c3cc43383h

data_7110045
_publ_section_title
;
 A 4 + 4 strategy for synthesis of zeolitic metal-organic frameworks: an
 indium-MOF with SOD topology as a light-harvesting antenna
;
_journal_name_full               Chem.Commun.
_journal_page_first              11155
_journal_paper_doi               10.1039/c3cc43383h
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C56 H95 In N6 O16'
_chemical_formula_weight         1223.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :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            18
_cell_length_a                   38.2369(10)
_cell_length_b                   38.2369(10)
_cell_length_c                   22.7356(12)
_cell_measurement_temperature    296(2)
_cell_volume                     28787.4(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0947
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            69588
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Process-auto
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11700
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
The remaining solvent molecules were disordered and assigned as 18 Et2NH2+ ion, 72 DEF molecules,
72 ethanol molecules per unit cell, which were determined by TGA,
elemental analysis and SQUEEZE results. The contributions of these disordered solvents to
the scattering values have been removed by using the PLATON SQUEEZE program. We can see from 
the SQUEEZE that some 6913 electrons were removed from the unit cell, or some 6913/18 = 384 electrons 
per formula unit. This total includes 42 electrons of the Et2NH2+ ion and other electrons (342e) from 
disordered solvent, approximately 4(DEF) + 4(EtOH) in the channel. From the calculation and
related information (The CHN and TGA), the formula unit should include 4 DEF, 4 C2H5OH (56e*4+26e*4=328e).
Anal. Cald. for C56H95N6O16In: C, 54.99; H, 7.83; N, 6.87; found: C, 53.86; H, 6.90; N, 7.89.
;
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         7969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                3195
_reflns_number_total             7969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43383h.txt
_cod_data_source_block           r-3c
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7110045