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_4349835
_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
'C75 H51 Cd2 Cl N12 O6, 2(C3 H7 N O), Cl, 2(H O)'
_chemical_formula_sum            'C81 H69 Cd2 Cl2 N14 O10'
_chemical_formula_weight         1694.23
_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   mixed
_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                 111.047(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0221(5)
_cell_length_b                   17.4201(5)
_cell_length_c                   26.3666(7)
_cell_measurement_reflns_used    16692
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.5880
_cell_measurement_theta_min      4.2000
_cell_volume                     9011.5(5)
_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 0.983
_diffrn_measured_fraction_theta_max 0.996
_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 -13.00   1.00    1.44    --  -37.03 -77.00-120.00   43
  2  \w     48.00  75.00   1.00    1.44    --   37.03-126.00  30.00   27
  3  \w     24.00  75.00   1.00    1.44    --   37.03 -99.00 120.00   51
  4  \w     44.00 114.00   1.00    3.00    --  110.47 -61.00 120.00   70
  5  \w     41.00 116.00   1.00    3.00    --  110.47-112.00  30.00   75
  6  \w     86.00 117.00   1.00    3.00    --  110.47 -61.00 -60.00   31
  7  \w     67.00 113.00   1.00    3.00    --  110.47-112.00 -90.00   46
  8  \w     47.00  74.00   1.00    3.00    --  110.47 -61.00 -60.00   27
  9  \w     43.00 129.00   1.00    3.00    --  110.47 -30.00-180.00   86
 10  \w     96.00 178.00   1.00    3.00    --  110.47  30.00-120.00   82
 11  \w    124.00 177.00   1.00    3.00    --  110.47  61.00 -90.00   53
 12  \w    140.00 178.00   1.00    3.00    --  110.47 112.00 -90.00   38
 13  \w    116.00 171.00   1.00    3.00    --  110.47 112.00-180.00   55
 14  \w    101.00 132.00   1.00    3.00    --  110.47 112.00 -90.00   31
 15  \w     74.00 105.00   1.00    1.44    --   37.03  77.00 -30.00   31
 16  \w     29.00  56.00   1.00    1.44    --   37.03  77.00 -30.00   27
 17  \w     11.00 105.00   1.00    1.44    --   37.03  77.00-120.00   94
 18  \w    -12.00  16.00   1.00    1.44    --  -37.03  57.00 -60.00   28
 19  \w    -46.00 -14.00   1.00    1.44    --  -37.03  57.00 -60.00   32
 20  \w    -84.00  -7.00   1.00    1.44    --  -37.03 126.00  30.00   77
 21  \w     27.00  97.00   1.00    1.44    --   37.03  57.00 150.00   70
 22  \w   -105.00 -78.00   1.00    1.44    --  -37.03 -77.00-120.00   27
 23  \w   -105.00 -80.00   1.00    1.44    --  -37.03-150.00 -61.00   25
;
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            40496
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.440
_exptl_absorpt_coefficient_mu    4.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44525
_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    1.247
_exptl_crystal_description       prism
_exptl_crystal_F_000             3444
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_platon_squeeze_details
;
;
_refine_diff_density_max         2.503
_refine_diff_density_min         -1.925
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         16038
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0768
_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^)+(0.1255P)^2^+35.6512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2166
_refine_ls_wR_factor_ref         0.2256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13687
_reflns_number_total             16038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00123e2.cif
_cod_data_source_block           Compound1
_cod_original_cell_volume        9011.5(4)
_cod_database_code               4349835
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.336
_shelx_estimated_absorpt_t_min   0.308
_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, All O(H) groups
2. Restrained distances
 H14-O14
 0.84 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(N18)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C93) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(O8) \\sim Ueq,
Uanis(C87) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C82) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N14) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(O9)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: 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) O8(0.5) C82(0.5) H82(0.5) C83(0.5)
 H83A(0.5) H83B(0.5) H83C(0.5) C84(0.5) H84A(0.5) H84B(0.5) H84C(0.5) N15(0.5)
 O9(0.5) C85(0.5) H85A(0.5) H85B(0.5) H85C(0.5) C86(0.5) H86A(0.5) H86B(0.5)
 H86C(0.5) C87(0.5) H87(0.5) N16(0.5) O10(0.5) C91(0.5) H91A(0.5) H91B(0.5)
 H91C(0.5) C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C93(0.5) H93(0.5) N18(0.5)
 O12(0.5)
5.a Free rotating group:
 O13(H13A), O14(H14)
5.b 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), C79(H79), C82(H82), C87(H87), C93(H93)
5.c Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,
 H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C91(H91A,H91B,H91C), C92(H92A,
 H92B,H92C)
;
_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
;