Fabrication of amine and imine-functionalized isoreticular pillared-layer metal‒organic frameworks for the highly selective detection of nitro-aromatics
Tarasi, Somayeh; Azhdari Tehrani, Alireza; Morsali, Ali; Retailleau, Pascal; New Journal of Chemistry 42 (2018) 14772–; doi:10.1039/C8NJ02407C

data_7057585
_publ_section_title
;
 Fabrication of amine and imine-functionalized isoreticular pillared-layer
 metal--organic frameworks for the highly selective detection of
 nitro-aromatics
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14772
_journal_paper_doi               10.1039/C8NJ02407C
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C25 H18 N2 O5 Zn, C3 H7 N O'
_chemical_formula_sum            'C28 H25 N3 O6 Zn'
_chemical_formula_weight         564.88
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-07-14 deposited with the CCDC.
2018-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.865(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6564(9)
_cell_length_b                   25.3323(10)
_cell_length_c                   15.9430(8)
_cell_measurement_reflns_used    10812
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5490
_cell_measurement_theta_min      4.2190
_cell_volume                     5567.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (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_temperature      293(2)
_diffrn_detector                 'HPAD dectris PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.921
_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     42.00  68.00   0.50   45.00    --   -0.30  38.00 150.00   52
  2  \w    -18.00  44.00   0.50   45.00    --   -0.30  38.00 -60.00  124
  3  \w     56.00  82.00   0.50   45.00    --   -0.30  38.00 -60.00   52
  4  \w     -9.00  21.00   0.50   45.00    --   -0.30  38.00  90.00   60
  5  \w     44.00  79.00   0.50   45.00    --   -0.30  38.00-150.00   70
  6  \w    -21.00  16.00   0.50   45.00    --   -0.30  38.00 -90.00   74
  7  \w    -24.00  89.00   0.50   45.00    --   -0.30  38.00  30.00  226
  8  \w     51.00  86.00   0.50   45.00    --   -0.30  19.00  90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0231646000
_diffrn_orient_matrix_UB_12      -0.0134472000
_diffrn_orient_matrix_UB_13      -0.0407013000
_diffrn_orient_matrix_UB_21      0.0353460000
_diffrn_orient_matrix_UB_22      0.0098442000
_diffrn_orient_matrix_UB_23      -0.0172538000
_diffrn_orient_matrix_UB_31      0.0293631000
_diffrn_orient_matrix_UB_32      -0.0225063000
_diffrn_orient_matrix_UB_33      0.0167998000
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44109
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.560
_diffrn_reflns_theta_min         4.212
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Rigaku mm003 microsource'
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         7863
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+2.5694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6003
_reflns_number_total             7876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02407c2.cif
_cod_data_source_block           TMU-21(RL2)_sq
_cod_depositor_comments
'Adding full bibliography for 7057584--7057585.cif.'
_cod_database_code               7057585
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 N2-H2
 0.87 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C19(H19), C18(H18), C9(H9), C3(H3), C13(H13), C7(H7),
 C4(H4), C15(H15), C6(H6), C24(H24), C22(H22), C16(H16), C23(H23)
;
_shelx_res_checksum              33922
_shelx_fab_checksum              93050