A hydrostable CuII coordination network prepared hydrothermally as “turn–on” fluorescent sensor for S2– and selective adsorbent for methylene blue
Yu, XinXin; Cheng, Hao; Li, Xuan; Li, YaJun; Song, Xue-Qin; Dalton Transactions  (2022) –; doi:10.1039/D1DT04283A

data_7709342
_publ_section_title
;
 A hydrostable CuII coordination network prepared hydrothermally as
 &#x201C;turn--on&#x201D; fluorescent sensor for S2-- and selective
 adsorbent for methylene blue
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04283A
_journal_year                    2022
_chemical_formula_moiety         'C10 H6 Cu N O5'
_chemical_formula_sum            'C10 H6 Cu N O5'
_chemical_formula_weight         283.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-10 deposited with the CCDC.	2022-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.268(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.0500(9)
_cell_length_b                   5.0906(3)
_cell_length_c                   26.2723(16)
_cell_measurement_reflns_used    1934
_cell_measurement_temperature    173.20(10)
_cell_measurement_theta_max      69.7710
_cell_measurement_theta_min      7.2090
_cell_volume                     1821.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.20(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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    -85.00 -55.00   1.00    2.00    --   -8.50 178.00  60.00   30
  2  \w    -27.00   0.00   1.00    2.00    --   -8.50 111.00  60.00   27
  3  \w    -56.00  -2.00   1.00    2.00    --   -8.50 -50.00 -90.00   54
  4  \w    -54.00 -28.00   1.00    2.00    --   -8.50 111.00  60.00   26
  5  \w     22.00 112.00   1.00    2.00    --   54.00  77.00-120.00   90
  6  \w     20.00  45.00   1.00    2.00    --   54.00  81.00 139.27   25
  7  \w     90.00 116.00   1.00    2.00    --   54.00 152.00 -45.00   26
  8  \w    101.00 157.00   1.00    3.00    --  108.00 111.00-120.00   56
  9  \w     41.00  92.00   1.00    3.00    --  108.00 -38.00-120.00   51
 10  \w     41.00 115.00   1.00    3.00    --  108.00-111.00 -30.00   74
 11  \w     36.00  92.00   1.00    3.00    --  108.00 -25.00 -30.00   56
 12  \w     98.00 123.00   1.00    3.00    --  108.00 121.00 154.00   25
 13  \w     52.00  94.00   1.00    3.00    --  108.00 -25.00 -90.00   42
 14  \w     81.00 128.00   1.00    3.00    --  108.00 -91.00  30.00   47
 15  \w     48.00  73.00   1.00    3.00    --  108.00 -38.00  30.00   25
 16  \w    121.00 178.00   1.00    3.00    --  108.00  38.00  60.00   57
 17  \w     44.00 130.00   1.00    3.00    --  108.00 -63.00 120.00   86
 18  \w    -10.00  21.00   1.00    2.00    --   -8.50 -77.00 -60.00   31
 19  \w     41.00  68.00   1.00    2.00    --   54.00 -99.00  60.00   27
 20  \w     11.00  37.00   1.00    2.00    --   54.00 -99.00  60.00   26
 21  \w    105.00 140.00   1.00    3.00    --  108.00 -77.00 150.00   35
 22  \w     57.00 101.00   1.00    3.00    --  108.00 -50.00  30.00   44
 23  \w     58.00  84.00   1.00    3.00    --  108.00 -25.00 -60.00   26
 24  \w     73.00  99.00   1.00    3.00    --  108.00 -77.00 150.00   26
;
_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      0.0159122000
_diffrn_orient_matrix_UB_12      0.2779810000
_diffrn_orient_matrix_UB_13      0.0237145000
_diffrn_orient_matrix_UB_21      -0.0352590000
_diffrn_orient_matrix_UB_22      0.1193745000
_diffrn_orient_matrix_UB_23      -0.0553679000
_diffrn_orient_matrix_UB_31      -0.1063204000
_diffrn_orient_matrix_UB_32      0.0023700000
_diffrn_orient_matrix_UB_33      0.0060747000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            1773
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        66.548
_diffrn_reflns_theta_max         66.548
_diffrn_reflns_theta_min         3.472
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.070
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         1773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+13.3174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1715
_reflns_number_total             1773
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9122\% 
 around [-0.00 -0.00 1.00] (reciprocal) or [0.42 -0.00 0.91] (direct)
;
_cod_data_source_file            d1dt04283a2.cif
_cod_data_source_block           linzg_1104_twin1_hklf4
_cod_database_code               7709342
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C10 H6 Cu N O5'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.812(2)
 0.188(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3.a Rotating group:
 O5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C3(H3), C5(H5)
;
_shelx_res_checksum              22573
_shelx_hkl_checksum              74185
_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 1.635
_oxdiff_exptl_absorpt_empirical_full_min 0.553
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2