A colorimetric and “turn-on” fluorimetric chemosensor for selective detection of cyanide and its application in food sample
Hu, JingHan; Sun, You; Qi, Jing; Pei, Peng-Xiang; Lin, Qi; Zhang, You-Ming; RSC Adv.  (2016) –; doi:10.1039/C6RA16378E

data_7226821
_publ_section_title
;
 A colorimetric and &#x201C;turn-on&#x201D; fluorimetric chemosensor for
 selective detection of cyanide and its application in food sample
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA16378E
_journal_year                    2016
_chemical_formula_moiety         'C17 H20 N4 O2, H2 O'
_chemical_formula_sum            'C17 H22 N4 O3'
_chemical_formula_weight         330.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-22 deposited with the CCDC.
2016-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                94.51(2)
_cell_angle_beta                 105.05(3)
_cell_angle_gamma                104.130(18)
_cell_formula_units_Z            2
_cell_length_a                   7.1776(19)
_cell_length_b                   9.8366(15)
_cell_length_c                   13.673(6)
_cell_measurement_reflns_used    687
_cell_measurement_temperature    293.16(13)
_cell_measurement_theta_max      22.2330
_cell_measurement_theta_min      3.6830
_cell_volume                     893.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      air
_diffrn_ambient_temperature      293.16(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -33.00  99.00   1.20   12.00    --   22.71  19.00  60.00  110
  2  \w     23.00  61.40   1.20   12.00    --   22.71 -99.00   0.00   32
  3  \w    -13.00  24.20   1.20   12.00    --  -19.35 -99.00-180.00   31
  4  \w     38.00  84.80   1.20   12.00    --   22.71 178.00 -60.00   39
  5  \w    -52.00   2.00   1.20   12.00    --  -19.51 -57.00 120.00   45
  6  \w      4.00  76.00   1.20   12.00    --   22.79  57.00 120.00   60
  7  \w    -35.00  35.80   1.20   12.00    --   22.79 -57.00-120.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0459301000
_diffrn_orient_matrix_UB_12      0.0165316000
_diffrn_orient_matrix_UB_13      0.0377620000
_diffrn_orient_matrix_UB_21      0.0883703000
_diffrn_orient_matrix_UB_22      0.0022010000
_diffrn_orient_matrix_UB_23      0.0391026000
_diffrn_orient_matrix_UB_31      0.0376789000
_diffrn_orient_matrix_UB_32      0.0732799000
_diffrn_orient_matrix_UB_33      -0.0012795000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.2205
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6373
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.707
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6373
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.708
_refine_ls_R_factor_all          0.1944
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                1886
_reflns_number_total             6373
_reflns_threshold_expression     >2sigma(I)
_twin_special_details
;
Component 2 rotated by 179.9721\% 
 around [-0.00 0.98 -0.20] (reciprocal) or [0.32 0.95 0.00] (direct)
;
_cod_data_source_file            c6ra16378e2.cif
_cod_data_source_block           sunyou_0612_twin1_hklf4
_cod_database_code               7226821
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5537(9) 0.4463(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C14') \\sim Ueq, Uanis(C15') \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C16(0.5) H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5)
 H17C(0.5) C14'(0.5) H14C(0.5) H14D(0.5) C15'(0.5) H15D(0.5) H15E(0.5) H15F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C14'(H14C,H14D)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2A), C1(H1), C2(H2B), C3(H3), C4(H4), C7(H7), C10(H10), C12(H12), C13(H13)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C15'(H15D,H15E,H15F)
5.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.527
_oxdiff_exptl_absorpt_empirical_full_min 0.531
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2