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_1547198
_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_sum            'C21 H21 N2 O1.5'
_chemical_formula_weight         325.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2b'
_space_group_name_H-M_alt        'P b c 21'
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   11.0775(3)
_cell_length_b                   16.5200(10)
_cell_length_c                   37.7334(13)
_cell_measurement_reflns_used    5091
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      25.1970
_cell_measurement_theta_min      2.2650
_cell_volume                     6905.2(5)
_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
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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      99.98(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -50.00   69.00   1.0000  195.0000
omega____ theta____ kappa____ phi______ frames
    -       27.3512   19.0000  120.0000 119

  2 omega   50.00  105.00   1.0000  195.0000
omega____ theta____ kappa____ phi______ frames
    -       27.3512  178.0000    0.0000 55
;
_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      0.0565604000
_diffrn_orient_matrix_UB_12      0.0199124000
_diffrn_orient_matrix_UB_13      0.0013251000
_diffrn_orient_matrix_UB_21      -0.0128586000
_diffrn_orient_matrix_UB_22      0.0101841000
_diffrn_orient_matrix_UB_23      0.0178705000
_diffrn_orient_matrix_UB_31      0.0271309000
_diffrn_orient_matrix_UB_32      -0.0366429000
_diffrn_orient_matrix_UB_33      0.0056832000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            14831
_diffrn_reflns_point_group_measured_fraction_full 0.642
_diffrn_reflns_point_group_measured_fraction_max 0.642
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.838
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41882
_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    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.2568
_exptl_crystal_size_mid          0.2479
_exptl_crystal_size_min          0.1612
_refine_diff_density_max         -0.784
_refine_diff_density_min         -0.80
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 1059 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7552
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0849
_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^)+(0.0530P)^2^+25.7980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.265
_reflns_Friedel_fraction_full    0.274
_reflns_Friedel_fraction_max     0.274
_reflns_number_gt                6807
_reflns_number_total             7552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac7b03503_si_004.cif
_cod_data_source_block           br_45d
_cod_depositor_comments
;
Adding full bibliography for 1547198--1547200.cif.

2019-02-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C84 H84 N8 O6'
_cod_original_formula_sum        'C84 H84 N8 O6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1301.6376
_cod_database_code               1547198
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C84 H84 N8 O6'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6B
 0.85 with sigma of 0.02
 O6-H6A
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C73) = Uanis(C74) = Uanis(C75) = Uanis(C76) = Uanis(C77) = Uanis(C64) =
Uanis(C65) = Uanis(C66) = Uanis(C67) = Uanis(C68) = Uanis(C69) = Uanis(C70) =
Uanis(C71) = Uanis(C72) = Uanis(C78) = Uanis(C79) = Uanis(C80) = Uanis(C83) =
Uanis(C84) = Uanis(C81) = Uanis(C82)
Uanis(C25) = Uanis(C24) = Uanis(C23) = Uanis(C22) = Uanis(C35) = Uanis(C34) =
Uanis(C33) = Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29) = Uanis(C28) =
Uanis(C27) = Uanis(C26) = Uanis(C36) = Uanis(C37) = Uanis(C38) = Uanis(C41) =
Uanis(C42) = Uanis(C39) = Uanis(C40)
Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56) = Uanis(C43) =
Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48) = Uanis(C49) =
Uanis(C50) = Uanis(C51) = Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60) =
Uanis(C61) = Uanis(C62) = Uanis(C63)
Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) =
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) =
Uanis(C7) = Uanis(C8) = Uanis(C15) = Uanis(C17) = Uanis(C20) = Uanis(C21) =
Uanis(C18) = Uanis(C19) = Uanis(C16)
Uanis(N8) = Uanis(N7) = Uanis(N6) = Uanis(N5) = Uanis(N3) = Uanis(N4) =
Uanis(N2) = Uanis(N1)
Uanis(O3) = Uanis(O4) = Uanis(O1) = Uanis(O2) = Uanis(O6) = Uanis(O5)
4.a Free rotating group:
 O5(H5A,H5B)
4.b Ternary CH refined with riding coordinates:
 C78(H78), C57(H57), C36(H36), C15(H15)
4.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N1(H1), N5(H5), C76(H76), C32(H32), C71(H71), C3(H3A), C22(H22),
 C67(H67), C45(H45), C11(H11), C46(H46), C31(H31), C55(H55), C72(H72), C51(H51),
  C4(H4), C25(H25), C29(H29), C64(H64), C34(H34), C23(H23), C52(H52), C74(H74),
 C24(H24), C8(H8), C66(H66), C50(H50), C1(H1A), C43(H43), C65(H65), C44(H44),
 C10(H10), C9(H9), C13(H13), C2(H2), C73(H73), C53(H53), C30(H30)
4.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C84(H84A,H84B,H84C), C63(H63A,H63B,
 H63C), C61(H61A,H61B,H61C), C79(H79A,H79B,H79C), C82(H82A,H82B,H82C), C19(H19A,
 H19B,H19C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C37(H37A,H37B,H37C),
 C58(H58A,H58B,H58C)
;
_shelx_res_checksum              58147
_shelx_hkl_checksum              56292
_olex2_date_sample_data_collection 1421134125.0
_olex2_submission_special_instructions 'No special instructions were received'