Aqueous media ultra-sensitive detection of antibiotics via highly stable luminescent 3D Cadmium-based MOF
Asad, Muhammad; Wang, Shan; Wang, Qian-You; Li, Lin-Ke; Anwar, Muhammad Imran; Younas, Ayesha; Zang, Shuang-Quan; New Journal of Chemistry 45 (2021) 20887–20894; doi:10.1039/D1NJ04413C

data_7061022
_publ_section_title
;
 Aqueous media ultra-sensitive detection of antibiotics via highly stable
 luminescent 3D Cadmium-based MOF
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20887
_journal_page_last               20894
_journal_paper_doi               10.1039/D1NJ04413C
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C84 H56 Cd2 N4 O8, 3(C3 H7 N O)'
_chemical_formula_sum            'C93 H77 Cd2 N7 O11'
_chemical_formula_weight         1693.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-05 deposited with the CCDC.	2021-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.140(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4126(2)
_cell_length_b                   20.6834(4)
_cell_length_c                   16.4770(3)
_cell_measurement_reflns_used    8965
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.2990
_cell_measurement_theta_min      3.4640
_cell_volume                     4763.00(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_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    -36.00  72.00   0.50    1.10    --   53.30 -57.00-150.00  216
  2  \w     78.00 142.00   0.50    1.10    --   53.30  38.00 120.00  128
  3  \w     92.00 121.00   0.50    1.10    --   53.30  77.00  60.00   58
  4  \w     32.00  77.00   0.50    1.10    --   53.30  77.00  60.00   90
  5  \w      6.00 103.00   0.50    3.00    --   93.00 -30.00  90.00  194
  6  \w     70.00 164.00   0.50    3.00    --   93.00  15.00  60.00  188
  7  \w     66.00 112.00   0.50    3.00    --   93.00 -30.00 -60.00   92
  8  \w     95.00 121.00   0.50    3.00    --   93.00 -82.00 -30.00   52
  9  \w     37.00 125.00   0.50    3.00    --   93.00 -82.00 -90.00  176
 10  \w     66.00  92.00   0.50    3.00    --   93.00  82.00  30.00   52
 11  \w    132.00 158.00   0.50    3.00    --   93.00  82.00  30.00   52
 12  \w      7.00  33.00   0.50    3.00    --   93.00 -82.00 -30.00   52
 13  \w    122.00 177.00   0.50    3.00    --   93.00  61.00  60.00  110
 14  \w      7.00 117.00   0.50    3.00    --   93.00 -61.00 -90.00  220
 15  \w     14.00  39.00   0.50    3.00    --   93.00 -30.00 -60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0978918000
_diffrn_orient_matrix_UB_12      -0.0140279000
_diffrn_orient_matrix_UB_13      0.0600894000
_diffrn_orient_matrix_UB_21      -0.0470791000
_diffrn_orient_matrix_UB_22      -0.0003826000
_diffrn_orient_matrix_UB_23      0.0744566000
_diffrn_orient_matrix_UB_31      -0.0184844000
_diffrn_orient_matrix_UB_32      -0.0731929000
_diffrn_orient_matrix_UB_33      -0.0117726000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31299
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.775
_diffrn_reflns_theta_min         3.162
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         9196
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+18.3872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6995
_reflns_number_total             9196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04413c2.cif
_cod_data_source_block           hy
_cod_depositor_comments          'Adding full bibliography for 7061022.cif.'
_cod_database_code               7061022
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.889
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6-C46
 1.15 with sigma of 0.02
 N4-C47 = N4-C46
 1.4 with sigma of 0.02
 N4-C48
 1.4 with sigma of 0.02
 C47-C48
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C46 \\sim C47 \\sim C48 \\sim N4 \\sim O6: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C45) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C48) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C46(0.5) H46(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C48(0.5)
 H48A(0.5) H48B(0.5) H48C(0.5) N4(0.5) O6(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C21(H21), C23(H23), C24(H24), C26(H26), C29(H29),
  C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C46(H46)
5.b Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C)
;
_shelx_res_checksum              86869
_shelx_fab_checksum              31802
_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 1.507
_oxdiff_exptl_absorpt_empirical_full_min 0.493