A series of porous interpenetrating metal‒organic frameworks based on fluorescent ligands for nitroaromatic explosive detection
Zeng, Xiao-Shan; Xu, Hui-Ling; Xu, Yu-Ci; Li, Xiao-Qing; Nie, Zhao-Yang; Gao, Shu-Zhen; Xiao, Dong-Rong; Inorganic Chemistry Frontiers 5 (2018) 1622–; doi:10.1039/C8QI00123E

data_4349834
_publ_section_title
;
 A series of porous interpenetrating metal--organic frameworks based on
 fluorescent ligands for nitroaromatic explosive detection
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1622
_journal_paper_doi               10.1039/C8QI00123E
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C156 H126 Cd5 Cl4 N26 O19, 4(C3 H7 N O)'
_chemical_formula_sum            'C168 H154 Cd5 Cl4 N30 O23'
_chemical_formula_weight         3665.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-05-03 deposited with the CCDC.
2018-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.3592(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.0432(4)
_cell_length_b                   17.4458(3)
_cell_length_c                   26.3825(4)
_cell_measurement_reflns_used    34666
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.8340
_cell_measurement_theta_min      4.1960
_cell_volume                     9020.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 1.000
_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    -56.00  32.00   1.00    2.95    --  -37.16  38.00 -30.00   88
  2  \w   -104.00 -20.00   1.00    2.95    --  -37.16 -57.00-180.00   84
  3  \w    -54.00  30.00   1.00    2.95    --  -37.16  57.00  30.00   84
  4  \w   -106.00 -18.00   1.00    2.95    --  -37.16 -38.00  30.00   88
  5  \w    -91.00  -3.00   1.00    2.95    --  -37.16 126.00 120.00   88
  6  \w     24.00  91.00   1.00    2.95    --   37.16-126.00 -30.00   67
  7  \w     24.00  91.00   1.00    2.95    --   37.16-126.00   0.00   67
  8  \w     24.00  91.00   1.00    2.95    --   37.16-126.00-180.00   67
  9  \w     20.00 104.00   1.00    2.95    --   37.16  57.00-120.00   84
 10  \w     18.00 106.00   1.00    2.95    --   37.16  38.00   0.00   88
 11  \w     18.00 106.00   1.00    2.95    --   37.16  38.00 -60.00   88
 12  \w     41.00 116.00   1.00    2.00    --  110.47-112.00 -60.00   75
 13  \w     43.00 137.00   1.00    2.00    --  110.47 -77.00   0.00   94
 14  \w     40.00 149.00   1.00    2.00    --  110.47 -15.00 150.00  109
 15  \w     41.00 109.00   1.00    2.00    --  110.47 -95.00-180.00   68
 16  \w     92.00 177.00   1.00    2.00    --  110.47  61.00 -60.00   85
 17  \w     84.00 178.00   1.00    2.00    --  110.47  77.00   0.00   94
 18  \w     89.00 178.00   1.00    2.00    --  110.47  30.00 150.00   89
 19  \w     41.00 132.00   1.00    2.00    --  110.47 -30.00 -30.00   91
 20  \w     43.00 137.00   1.00    2.00    --  110.47 -77.00-120.00   94
 21  \w    -54.00 -19.00   1.00    2.95    --  -37.16  57.00  90.00   35
 22  \w    -54.00  30.00   1.00    2.95    --  -37.16  57.00 120.00   84
 23  \w     10.00 105.00   1.00    2.95    --   37.16  77.00   0.00   95
 24  \w     10.00 105.00   1.00    2.95    --   37.16  77.00 -90.00   95
 25  \w     10.00 105.00   1.00    2.95    --   37.16  77.00  60.00   95
 26  \w     10.00 105.00   1.00    2.95    --   37.16  77.00 150.00   95
 27  \w    -30.00  54.00   1.00    2.95    --   37.16 -57.00-180.00   84
 28  \w     20.00 104.00   1.00    2.95    --   37.16  57.00 150.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            81643
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.598
_exptl_absorpt_coefficient_mu    5.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
;
_refine_diff_density_max         2.276
_refine_diff_density_min         -2.527
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         16113
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0764
_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^)+(0.1318P)^2^+39.4084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2152
_refine_ls_wR_factor_ref         0.2235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13535
_reflns_number_total             16113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00123e2.cif
_cod_data_source_block           Compound4
_cod_database_code               4349834
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.330
_shelx_estimated_absorpt_t_min   0.281
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C56) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C80) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C54) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: Cd3(0.5) O9(0.5) C79(0.5) H79(0.5) C80(0.5) H80A(0.5) H80B(0.5)
 H80C(0.5) C81(0.5) H81A(0.5) H81B(0.5) H81C(0.5) N14(0.5) O11(0.5) C85(0.5)
 H85(0.5) C86(0.5) H86A(0.5) H86B(0.5) H86C(0.5) C87(0.5) H87A(0.5) H87B(0.5)
 H87C(0.5) N16(0.5) O13(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C13(H13),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44),
  C46(H46), C48(H48), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55),
 C56(H56), C57(H57), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
  C66(H66), C69(H69), C71(H71), C73(H73), C76(H76), C79(H79), C82(H82), C85(H85)
4.b Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C87(H87A,
 H87B,H87C)
;
_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
;