Highly Selective Sub-ppm Naked-Eye Detection of Hydrazine with Conjugated-1,3-Diketo Probes: Imaging Hydrazine in Drosophila Larvae.
Roy, Biswajit; Halder, Sudipta; Guha, Abhishek; Bandyopadhyay, Subhajit; Analytical chemistry 89 (2017) 10625–10636; doi:10.1021/acs.analchem.7b03503

data_1547199
_publ_section_title
;
 Highly Selective Sub-ppm Naked-Eye Detection of Hydrazine with
 Conjugated-1,3-Diketo Probes: Imaging Hydrazine in Drosophila Larvae.
;
_journal_issue                   19
_journal_name_full               'Analytical chemistry'
_journal_page_first              10625
_journal_page_last               10636
_journal_paper_doi               10.1021/acs.analchem.7b03503
_journal_volume                  89
_journal_year                    2017
_chemical_formula_moiety         'C22 H16 O2'
_chemical_formula_sum            'C22 H16 O2'
_chemical_formula_weight         312.35
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.715(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1242(11)
_cell_length_b                   7.7930(5)
_cell_length_c                   14.2055(10)
_cell_measurement_reflns_used    2464
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      27.8690
_cell_measurement_theta_min      2.9210
_cell_volume                     1536.34(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   85.00  118.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       27.8622    0.0000   90.0000 33

  2 omega   55.00  104.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       27.8622  178.0000   60.0000 49

  3 omega  -14.00   68.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       27.8622  -77.0000 -150.0000 82

  4 omega  -63.00   28.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       27.8622    0.0000   90.0000 91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0457437000
_diffrn_orient_matrix_UB_12      0.0092091000
_diffrn_orient_matrix_UB_13      -0.0301911000
_diffrn_orient_matrix_UB_21      0.0018966000
_diffrn_orient_matrix_UB_22      0.0899252000
_diffrn_orient_matrix_UB_23      0.0080525000
_diffrn_orient_matrix_UB_31      0.0226559000
_diffrn_orient_matrix_UB_32      0.0110118000
_diffrn_orient_matrix_UB_33      -0.0401020000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4717
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.212
_diffrn_reflns_theta_max         24.911
_diffrn_reflns_theta_min         1.867
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.2589
_exptl_crystal_size_mid          0.2148
_exptl_crystal_size_min          0.1859
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0587P)^2^+0.2534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2145
_reflns_number_total             2603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac7b03503_si_002.cif
_cod_data_source_block           br-83
_cod_depositor_comments
'Adding full bibliography for 1547198--1547200.cif.'
_cod_original_cell_volume        1536.3(2)
_cod_database_code               1547199
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C22 H16 O2'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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), C15(H15), C16(H16), C17(H17), C11(H11), C3(H3), C7(H7), C10(H10),
 C6(H6), C9(H9)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              6298
_shelx_hkl_checksum              21444
_olex2_date_sample_data_collection 2015-04-20
_olex2_submission_special_instructions 'No special instructions were received'