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_7222452
_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         'C23.7 H28.7 In N2.3 O11.3'
_chemical_formula_sum            'C22 H19 In N2 O8'
_chemical_formula_weight         554.22
_chemical_name_common            InOF-13
_chemical_name_systematic        InOF-13
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-18 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            4
_cell_length_a                   19.72440(10)
_cell_length_b                   17.08140(10)
_cell_length_c                   9.95540(10)
_cell_measurement_reflns_used    6539
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.5460
_cell_measurement_theta_min      4.4550
_cell_volume                     3354.18(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            69475
_diffrn_reflns_theta_full        73.54
_diffrn_reflns_theta_max         73.54
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    5.935
_exptl_absorpt_correction_T_max  0.8420
_exptl_absorpt_correction_T_min  0.6482
_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_colour            colorless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
SQUEEZE removed disordered DEF and isolated water molecules 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 200.4 electrons were removed from the unit-cell contents; equivalent to some 200.4/4 ?\"O 50 electrons per formula unit in this P21212 system with Z = 4. The electron count from the reported disordered 1/3DEF and 3H2O material is 19 + 30 = 49 electrons.   

See Ref: a) CrystEngComm, 2015, 17, 1750-1753
;
_refine_diff_density_max         1.758
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         6764
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0800P)^2^+1.3813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                6576
_reflns_number_total             6764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01376c2.cif
_cod_data_source_block           InOF-13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      P21212
_cod_database_code               7222452