Cation exchange in a fluorescent zinc-based metal–organic framework for cadmium ion detection
Chen, Mao-Long; Qi, Zhen-Li; Jin, Wan-Ting; Xu, Zhou; Cheng, Yun-Hui; Zhou, Zhao-Hui; CrystEngComm 23 (2021) 7442–7449; doi:10.1039/D1CE00931A

data_7243615
_publ_section_title
;
 Cation exchange in a fluorescent zinc-based metal--organic framework for
 cadmium ion detection
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              7442
_journal_page_last               7449
_journal_paper_doi               10.1039/D1CE00931A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C14 H13 N O6 Zn, C2 H8 N'
_chemical_formula_sum            'C16 H21 N2 O6 Zn'
_chemical_formula_weight         402.72
_chemical_name_systematic        Zn-MOF
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-07-16
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3597(8)
_cell_length_b                   30.8839(13)
_cell_length_c                   11.3262(4)
_cell_measurement_reflns_used    2975
_cell_measurement_temperature    193
_cell_measurement_theta_max      60.4570
_cell_measurement_theta_min      4.1500
_cell_volume                     6422.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      193.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    -20.00  32.00   1.00    2.50    --    0.78   0.00 -30.00   52
  2  \w     52.00  86.00   1.00    2.50    --    0.78   0.00 -30.00   34
  3  \w   -113.00 -32.00   1.00   15.00    --  -46.29 126.00-120.00   81
  4  \w     51.00 122.00   1.00   15.00    --   47.85  57.00-180.00   71
  5  \w     80.00 110.00   1.00   15.00    --   47.85 126.00-120.00   30
  6  \w   -166.00 -64.00   1.00   35.00    --  -93.36 -50.00  90.00  102
  7  \w   -154.00-126.00   1.00   35.00    --  -93.36-112.00 -90.00   28
  8  \w   -107.00 -22.00   1.00   35.00    --  -93.36  64.00 -30.00   85
  9  \w   -132.00-107.00   1.00   35.00    --  -93.36-112.00-180.00   25
 10  \w     64.00  90.00   1.00   35.00    --   94.92-112.00-180.00   26
 11  \w     22.00  48.00   1.00   35.00    --   94.92-112.00-180.00   26
 12  \w     58.00  85.00   1.00   35.00    --   94.92-112.00 -30.00   27
 13  \w     16.00  41.00   1.00   35.00    --   94.92-112.00 -30.00   25
 14  \w     52.00  89.00   1.00   35.00    --   94.92-112.00 120.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0617905000
_diffrn_orient_matrix_UB_12      0.0251834000
_diffrn_orient_matrix_UB_13      -0.0614432000
_diffrn_orient_matrix_UB_21      -0.0546868000
_diffrn_orient_matrix_UB_22      -0.0174468000
_diffrn_orient_matrix_UB_23      0.0915827000
_diffrn_orient_matrix_UB_31      0.0151527000
_diffrn_orient_matrix_UB_32      0.0393870000
_diffrn_orient_matrix_UB_33      0.0795679000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11235
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        60.698
_diffrn_reflns_theta_max         60.698
_diffrn_reflns_theta_min         2.862
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.833
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0749P)^2^+14.9771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.1901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4169
_reflns_number_total             4910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00931a2.cif
_cod_data_source_block           exp_21699_sq
_cod_depositor_comments          'Adding full bibliography for 7243615.cif.'
_cod_original_cell_volume        6422.2(4)
_cod_database_code               7243615
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C7(H7), C4(H4), C11(H11), C12(H12)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C16(H16A,H16B,
 H16C)
;
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.739
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.790
_shelx_fab_checksum              97416
_shelx_hkl_checksum              23711
_shelx_res_checksum              93960
_shelx_shelxl_version_number     2018/3