Crystal structure, morphology and sorption behaviour of porous indium-tetracarboxylate framework materials
Qian, Jinjie; Yu, Panpan; Su, Kongzhao; Dong, Youqing; Huang, Shaoming; Hong, Maochun; CrystEngComm 17 (2015) 8512–; doi:10.1039/C5CE01376C

data_7222451
_publ_section_title
;
 Crystal structure, morphology and sorption behaviour of porous
 indium-tetracarboxylate framework materials
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              8512
_journal_paper_doi               10.1039/C5CE01376C
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C21.6 H26 In O13'
_chemical_formula_sum            'C16 H6 In O8'
_chemical_formula_weight         441.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           131
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c 2'
_symmetry_space_group_name_H-M   'P 42/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2015-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9843(6)
_cell_length_b                   9.9843(6)
_cell_length_c                   18.2816(18)
_cell_measurement_temperature    173(2)
_cell_volume                     1822.4(2)
_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  'SuperNova, Dual, Cu at zero, Atlas'
_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  0.1238
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13298
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.9738
_exptl_absorpt_correction_T_min  0.9674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             430
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
SQUEEZE removed disordered DMA, isolated water molecules and EtOH per formula unit.  This value is calculated based upon volume/count_electrons analysis and TG analyses. 

Specifically, the above reported formulation is fully in accord with the SQUEEZE data where we see that some 190 electrons were removed from the unit-cell contents; equivalent to some 195.7/2 ?\"O 98 electrons per formula unit in this P42/mmc  system with Z = 2. The electron count from the reported disordered 2/3DMA, 3H2O, 4/3EtOH material is 32 + 30 + 36 = 98 electrons.  

See ref: a) CrystEngComm, 2015, 17, 1750-1753
;
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       0.037(9)
_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   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         1200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.1967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2219
_reflns_number_gt                912
_reflns_number_total             1200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01376c2.cif
_cod_data_source_block           InOF-12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7222451--7222452.cif.
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_cod_original_sg_symbol_H-M      P42/mmc
_cod_database_code               7222451