Neighbouring group participation of thiol through aldehyde group assisted thiolysis of active ether: ratiometric and vapor phase fast detection of hydrogen sulfide in mixed aqueous media
Das, Avijit Kumar; Goswami, Shyamaprosad; Quah, Ching Kheng; Fun, Hoong-Kun; New J. Chem. 39 (2015) 5669–; doi:10.1039/C5NJ00689A

data_7054847
_publ_section_title
;
 Neighbouring group participation of thiol through aldehyde group assisted
 thiolysis of active ether: ratiometric and vapor phase fast detection of
 hydrogen sulfide in mixed aqueous media
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              5669
_journal_paper_doi               10.1039/C5NJ00689A
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C16 H10 N2 O5'
_chemical_formula_sum            'C16 H10 N2 O5'
_chemical_formula_weight         310.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-01-23 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.655(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9055(19)
_cell_length_b                   4.6272(4)
_cell_length_c                   13.7499(12)
_cell_measurement_reflns_used    3742
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.52
_cell_measurement_theta_min      2.79
_cell_volume                     1392.2(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and PLATON (Spek, 2009)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Bruker SMART APEX II DUO CCD area-detector diffractometer 
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18679
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.557
_diffrn_reflns_theta_min         1.861
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.624
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.5549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1973
_reflns_number_total             2898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00689a2.cif
_cod_data_source_block           mo_fs394_0m
_cod_depositor_comments
'Adding full bibliography for 7054846--7054847.cif.'
_cod_database_code               7054847
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.992
_shelxl_version_number           2014-3
_shelx_res_checksum              62637