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_1547200
_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         'C20 H16 O2'
_chemical_formula_sum            'C20 H16 O2'
_chemical_formula_weight         288.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_symmetry_space_group_name_Hall  'P -2ac -2n'
_symmetry_space_group_name_H-M   'P n 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.5147(11)
_cell_length_b                   33.238(2)
_cell_length_c                   5.0184(5)
_cell_measurement_reflns_used    2790
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.7700
_cell_measurement_theta_min      2.4440
_cell_volume                     2921.5(4)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details
;
  1 omega   36.00   85.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -       27.5074  178.0000 -150.0000 49

  2 omega  -48.00   72.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -       27.5074   19.0000  -60.0000 120
;
_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      -0.0401823000
_diffrn_orient_matrix_UB_12      -0.0004315000
_diffrn_orient_matrix_UB_13      0.0172631000
_diffrn_orient_matrix_UB_21      0.0033706000
_diffrn_orient_matrix_UB_22      0.0134153000
_diffrn_orient_matrix_UB_23      0.1094491000
_diffrn_orient_matrix_UB_31      -0.0037448000
_diffrn_orient_matrix_UB_32      0.0165791000
_diffrn_orient_matrix_UB_33      -0.0878505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            6907
_diffrn_reflns_point_group_measured_fraction_full 0.802
_diffrn_reflns_point_group_measured_fraction_max 0.687
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         2.326
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79474
_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    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.2489
_exptl_crystal_size_mid          0.2358
_exptl_crystal_size_min          0.1589
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 1287 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0556P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1217
_reflns_Friedel_coverage         0.518
_reflns_Friedel_fraction_full    0.596
_reflns_Friedel_fraction_max     0.477
_reflns_number_gt                4395
_reflns_number_total             4997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac7b03503_si_003.cif
_cod_data_source_block           br-40a
_cod_depositor_comments
;
Adding full bibliography for 1547198--1547200.cif.

2019-01-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C20 H16 O2)'
_cod_original_formula_sum        'C40 H32 O4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     576.65
_cod_database_code               1547200
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H16 O2'
_reflns_odcompleteness_completeness 99.86
_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:
 C15(H15), C7(H8), C4(H5), C2(H3), C12(H13), C27(H30), C23(H34), C35(H37),
 C29(H28), C25(H32), C10(H11), C3(H4), C11(H12), C22(H35), C5(H6), C30(H27),
 C24(H33), C9(H10), C32(H25), C31(H26)
2.b Idealised Me refined as rotating group:
 C20(H22A,H22B,H22C), C18(H21A,H21B,H21C), C40(H43A,H43B,H43C), C38(H44A,H44B,
 H44C)
;
_olex2_date_sample_data_collection 2014-11-26
_olex2_submission_special_instructions 'No special instructions were received'