N2S2 pyridinophane-based fluorescent chemosensors for selective optical detection of Cd2+ in soils
Garau, Alessandra; Lvova, Larisa; Macedi, Eleonora; Ambrosi, Gianluca; Aragoni, M. Carla; Arca, Massimiliano; Caltagirone, Claudia; Coles, Simon J.; Formica, Mauro; Fusi, Vieri; Giorgi, Luca; Isaia, Francesco; Lippolis, Vito; Orton, James B.; Paolesse, Roberto; New Journal of Chemistry 44 (2020) 20834–20852; doi:10.1039/D0NJ03858J

data_7060127
_publ_section_title
;
 N2S2 pyridinophane-based fluorescent chemosensors for selective optical
 detection of Cd2+ in soils
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20834
_journal_page_last               20852
_journal_paper_doi               10.1039/D0NJ03858J
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C23 H27 Cd N5 O8 S2'
_chemical_formula_sum            'C23 H27 Cd N5 O8 S2'
_chemical_formula_weight         678.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-05-12 deposited with the CCDC.	2020-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                96.042(2)
_cell_angle_beta                 93.5240(19)
_cell_angle_gamma                109.789(2)
_cell_formula_units_Z            2
_cell_length_a                   8.16330(18)
_cell_length_b                   8.7604(3)
_cell_length_c                   19.2048(5)
_cell_measurement_reflns_used    16259
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8930
_cell_measurement_theta_min      2.1990
_cell_volume                     1278.19(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -31.00  77.00   0.50    2.00    --  -13.00  72.00   0.00  216
  2  \w    -70.00  23.00   0.50    2.00    --  -13.00 -72.00-120.00  186
  3  \w    -67.00  23.00   0.50    2.00    --  -13.00 -72.00  60.00  180
  4  \w    -83.00  -8.00   0.50    2.00    --  -13.00   0.00-120.00  150
  5  \w    -63.00 -38.00   0.50    2.00    --  -13.00 -54.00-180.00   50
  6  \w    -81.00  23.00   0.50    2.00    --  -13.00 -72.00 150.00  208
  7  \w    -22.00  77.00   0.50    2.00    --  -13.00  72.00-120.00  198
  8  \w    -76.00 -25.00   0.50    2.00    --  -13.00 -72.00 -30.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and a Rigaku AFC12 goniometer and an enhanced sensitivity (HG) Saturn724+ CCD detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0260112000
_diffrn_orient_matrix_UB_12      -0.0607770000
_diffrn_orient_matrix_UB_13      0.0144052000
_diffrn_orient_matrix_UB_21      0.0228495000
_diffrn_orient_matrix_UB_22      -0.0242523000
_diffrn_orient_matrix_UB_23      -0.0333819000
_diffrn_orient_matrix_UB_31      0.0862785000
_diffrn_orient_matrix_UB_32      0.0572963000
_diffrn_orient_matrix_UB_33      0.0086932000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18879
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.458
_diffrn_reflns_theta_min         2.493
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    'pale yellow'
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       lath
_exptl_crystal_F_000             688
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.9974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5657
_reflns_number_total             5819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03858j2.cif
_cod_data_source_block           2015cag0001_1a
_cod_depositor_comments          'Adding full bibliography for 7060127.cif.'
_cod_original_cell_volume        1278.18(6)
_cod_database_code               7060127
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C23H27CdN5O8S2
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.855
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C15(H15), C16(H16), C19(H19), C22(H22)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              59626
_olex2_date_sample_data_collection 2015-01-17
_olex2_date_sample_submission    2015-01-17
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 2015CAG0001
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.589
_oxdiff_exptl_absorpt_empirical_full_min 0.641