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_7235809
_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         'C15 H13 N3 O5 Zn, C3 H7 N O'
_chemical_formula_sum            'C18 H20 N4 O6 Zn'
_chemical_formula_weight         453.75
_chemical_name_systematic        '[Zn(dcbpy)(DMF)]'
_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     iterative
_audit_creation_date             2015-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-01-24 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.058(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3725(2)
_cell_length_b                   14.7643(3)
_cell_length_c                   14.7153(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1998.47(7)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14313
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        51.439
_diffrn_reflns_theta_max         51.439
_diffrn_reflns_theta_min         4.282
_exptl_absorpt_coefficient_mu    2.089
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_preparation
'Solvothermal synthesis, zinc nitrate hexahydrate, 2,2'-bipyridine-4,4'-dicarboxylic acid, DMF'
_exptl_crystal_recrystallization_method 'from reaction mixture'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00010(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         2158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0488P)^2^+3.1283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1824
_reflns_number_total             2158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ta05638h2.cif
_cod_data_source_block           xstr0165
_cod_database_code               7235809
_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. Others
 Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C16(H16)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18A(H18A,H18B,
 H18C), C18B(H18D,H18E,H18F)
;
_shelx_res_checksum              58938
_shelx_hkl_checksum              16227
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id MJ.3B
_olex2_submission_special_instructions 'No special instructions were received'