Amino-functionalized MOFs with high physicochemical stability for efficient gas storage/separation, dye adsorption and catalytic performance
Fan, Weidong; Wang, Xia; Xu, Ben; Wang, Yutong; Liu, Dandan; Zhang, Ming; Shang, Yizhu; Dai, Fangna; Zhang, Liangliang; Sun, Daofeng; Journal of Materials Chemistry A 6 (2018) 24486–; doi:10.1039/C8TA07839D

data_7237199
_publ_section_title
;
 Amino-functionalized MOFs with high physicochemical stability for
 efficient gas storage/separation, dye adsorption and catalytic
 performance
;
_journal_issue                   47
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              24486
_journal_paper_doi               10.1039/C8TA07839D
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         '0.5(C80 H52 In2 N4 O16)'
_chemical_formula_sum            'C40 H26 In N2 O8'
_chemical_formula_weight         777.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-09 deposited with the CCDC.
2018-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.407(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7988(18)
_cell_length_b                   30.8674(10)
_cell_length_c                   15.6757(9)
_cell_measurement_reflns_used    2671
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      63.7960
_cell_measurement_theta_min      4.0850
_cell_volume                     5725.4(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00  22.00   1.00    5.00    --    0.00 -57.00  60.00   91
  2  \w    -46.00  -4.00   1.00    5.00    --    0.00  19.00 150.00   42
  3  \w     34.00  72.00   1.00    5.00    --    0.00  19.00 150.00   38
  4  \w     54.00  83.00   1.00   35.00    --   54.00-125.00  30.00   29
  5  \w     43.00  78.00   1.00   35.00    --   54.00 -38.00 -90.00   35
  6  \w     -9.00  71.00   1.00   35.00    --   54.00 -57.00 120.00   80
  7  \w     28.00 127.00   1.00   35.00    --   54.00  38.00  90.00   99
  8  \w    -11.00  42.00   1.00   35.00    --   54.00 -38.00 -90.00   53
  9  \w     37.00 147.00   1.00   40.00    --  108.00 -25.00-120.00  110
 10  \w    140.00 177.00   1.00   40.00    --  108.00 111.00 -90.00   37
 11  \w     95.00 147.00   1.00   40.00    --  108.00 178.00 -30.00   52
 12  \w     59.00  86.00   1.00   40.00    --  108.00 178.00 -30.00   27
 13  \w     87.00 164.00   1.00   40.00    --  108.00  63.00  60.00   77
 14  \w    102.00 178.00   1.00   40.00    --  108.00 111.00 -60.00   76
 15  \w     43.00 109.00   1.00   40.00    --  108.00-111.00 -60.00   66
 16  \w     70.00 127.00   1.00   40.00    --  108.00 -63.00 -30.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0504736000
_diffrn_orient_matrix_UB_12      0.0206426000
_diffrn_orient_matrix_UB_13      0.0653099000
_diffrn_orient_matrix_UB_21      -0.1193043000
_diffrn_orient_matrix_UB_22      -0.0140117000
_diffrn_orient_matrix_UB_23      -0.0653530000
_diffrn_orient_matrix_UB_31      0.0148102000
_diffrn_orient_matrix_UB_32      -0.0431699000
_diffrn_orient_matrix_UB_33      0.0524501000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10661
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.781
_diffrn_reflns_theta_min         4.001
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.902
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.341
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5344
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.366
_refine_ls_R_factor_all          0.1572
_refine_ls_R_factor_gt           0.1310
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3566
_refine_ls_wR_factor_ref         0.3822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3158
_reflns_number_total             5344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta07839d2.cif
_cod_data_source_block           in_sq
_cod_database_code               7237199
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N In'
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2. Restrained distances
 C7-C9 = C1A-C4
 1.4 with sigma of 0.01
 C16-C9 = C13-C10 = C11-C19
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
Uanis(C7) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C11(H11), C13(H13), C1(H1), C14(H14), C18(H18),
 C17(H17), C15(H15)
5.b Fitted hexagon refined as free rotating group:
 C14(C18,C1A,C17,C15,C7)
5.c Idealised Me refined as rotating group:
 N9(H9A,H9B,H9C)
;
_shelx_res_checksum              454
_shelx_hkl_checksum              49399
_shelx_fab_checksum              24281
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.215
_oxdiff_exptl_absorpt_empirical_full_min 0.592