The vapour phase detection of explosive markers and derivatives using two fluorescent metal‒organic frameworks
Jurcic, Monika; Peveler, William J.; Savory, Christopher N.; Scanlon, David O.; Kenyon, Anthony J.; Parkin, Ivan P.; Journal of Materials Chemistry A 3 (2015) 6351–; doi:10.1039/C4TA05638H

data_7235810
_publ_section_title
;
 The vapour phase detection of explosive markers and derivatives using two
 fluorescent metal--organic frameworks
;
_journal_issue                   12
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              6351
_journal_paper_doi               10.1039/C4TA05638H
_journal_volume                  3
_journal_year                    2015
_chemical_formula_moiety         'C18 H20 Dy N5 O9'
_chemical_formula_sum            'C18 H20 Dy N5 O9'
_chemical_formula_weight         612.89
_chemical_name_systematic        Dy(DCBPY)(DMF)2(NO2)(H2O)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-10-20
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2014-10-21 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                76.388(4)
_cell_angle_beta                 69.431(4)
_cell_angle_gamma                86.377(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2414(5)
_cell_length_b                   10.3040(5)
_cell_length_c                   12.8291(6)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    149.90(15)
_cell_measurement_theta_max      74.2680
_cell_measurement_theta_min      4.3960
_cell_volume                     1111.37(10)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      149.90(15)
_diffrn_detector_area_resol_mean 5.2031
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.8812
_diffrn_measurement_details
;
  1 omega  -50.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000    0.0000 37

  2 omega  -59.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000   60.0000 86

  3 omega  -64.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   61.0000 -180.0000 91

  4 omega  -84.00   -4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000 -120.0000 80

  5 omega   15.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000   30.0000 100

  6 omega   23.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   38.0000 -180.0000 90

  7 omega   14.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000  -90.0000 100

  8 omega   14.00   52.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000  150.0000 38

  9 omega   74.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000   90.0000 26

 10 omega   18.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000   90.0000 51

 11 omega   55.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000  150.0000 27

 12 omega   16.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000 -150.0000 61

 13 omega   15.00   58.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000  -30.0000 43

 14 omega   83.00  109.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940  -94.0000  -90.0000 26

 15 omega   78.00  178.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000 -180.0000 100

 16 omega   81.00  175.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000   60.0000 94

 17 omega   77.00  104.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000   60.0000 27

 18 omega  138.00  176.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000    0.0000 38

 19 omega   77.00  104.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000    0.0000 27

 20 omega   82.00  173.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000  150.0000 91

 21 omega   77.00  103.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  -90.0000 26

 22 omega   44.00  121.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940 -125.0000 -180.0000 77

 23 omega   77.00  104.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  120.0000 27

 24 omega   77.00  165.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  -30.0000 88

 25 omega  123.00  168.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000   90.0000 45

 26 omega   81.00  140.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000 -120.0000 59

 27 omega   82.00  134.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000   30.0000 52

 28 omega   33.00   60.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940  -94.0000  -90.0000 27

 29 omega   82.00  156.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000  120.0000 74

 30 omega   81.00  137.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000  -60.0000 56

 31 omega   79.00  105.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000   90.0000 26

 32 omega   81.00  107.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000   90.0000 26

 33 omega   81.00  107.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000  -90.0000 26

 34 omega  125.00  152.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000 -150.0000 27

 35 omega   77.00  104.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  150.0000 27

 36 omega   78.00  105.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000   30.0000 27

 37 omega   77.00  103.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000 -150.0000 26

 38 omega   81.00  107.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000 -180.0000 26

 39 omega   84.00  111.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000 -150.0000 27

 40 omega   79.00  176.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000 -120.0000 97

 41 omega   36.00  136.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940  -77.0000  -30.0000 100

 42 omega   78.00  163.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  -60.0000 85

 43 omega   37.00  135.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940  -77.0000 -180.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1389665000
_diffrn_orient_matrix_UB_12      0.0987776000
_diffrn_orient_matrix_UB_13      -0.0548622000
_diffrn_orient_matrix_UB_21      -0.0623812000
_diffrn_orient_matrix_UB_22      0.0643304000
_diffrn_orient_matrix_UB_23      -0.0965586000
_diffrn_orient_matrix_UB_31      -0.0922766000
_diffrn_orient_matrix_UB_32      0.0988915000
_diffrn_orient_matrix_UB_33      0.0708545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16503
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.895
_diffrn_reflns_theta_min         4.416
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.524
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'pinkish colourless'
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       plate
_exptl_crystal_F_000             602
_exptl_crystal_preparation
'solvoethermal synthesis. Dysprosium nitrate pentahydrate , 2,2'-bipyridine-4,4'-dicarboxylic acid, DMF'
_exptl_crystal_recrystallization_method 'From reaction mixture'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.707
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0938P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4086
_reflns_number_total             4464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ta05638h2.cif
_cod_data_source_block           xstr0263
_cod_database_code               7235810
_chemical_oxdiff_formula         'C54 H20 N20 O16 Dy2'
_chemical_oxdiff_usercomment     3dy_3
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C7(H7), C15(H15), C17(H17), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,
 H1EC)
;
_olex2_exptl_crystal_mounting_method 'Nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'
_shelxl_version_number           2013-2