Ultrasensitive fluorescence detection of norfloxacin in aqueous medium employing a 2D Zn(ii)-based coordination polymer
Zeng, Na-Na; Ren, Li; Cui, Guang-Hua; CrystEngComm 24 (2022) 931–935; doi:10.1039/D1CE01537K

data_7244225
_publ_section_title
;
 Ultrasensitive fluorescence detection of norfloxacin in aqueous medium
 employing a 2D Zn(ii)-based coordination polymer
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              931
_journal_page_last               935
_journal_paper_doi               10.1039/D1CE01537K
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C92 H64 N12 O16 S4 Zn4, 7(H2 O)'
_chemical_formula_sum            'C92 H78 N12 O23 S4 Zn4'
_chemical_formula_weight         2109.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-08-23 deposited with the CCDC.	2022-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.798(7)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   8.892(4)
_cell_length_b                   24.276(11)
_cell_length_c                   11.365(5)
_cell_measurement_reflns_used    1009
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.42
_cell_measurement_theta_min      2.53
_cell_volume                     2308.3(18)
_computing_cell_refinement       'SAINT v7.53A (Bruker, 2008)'
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.1367
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13812
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.324
_diffrn_reflns_theta_min         1.678
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.9176
_exptl_absorpt_correction_T_min  0.75778
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5139
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0725P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2228
_reflns_number_total             5139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01537k2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7244225.cif.'
_cod_original_cell_volume        2308.3(19)
_cod_database_code               7244225
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.778
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O4-C9 \\sim O4A-C9A
 with sigma of 0.02
 O3-C9 \\sim O3A-C9A
 with sigma of 0.02
 C4-C9 \\sim C4-C9A
 with sigma of 0.02
 Zn1-O4 \\sim Zn1-O4A
 with sigma of 0.04
 Zn1-O3 \\sim Zn1-O3A
 with sigma of 0.04
 Zn1-C9 \\sim Zn1-C9A
 with sigma of 0.04
 O4-O3 \\sim O4A-O3A
 with sigma of 0.04
 O4-C4 \\sim O4A-C4
 with sigma of 0.04
 O3-C4 \\sim O3A-C4
 with sigma of 0.04
 O1-C1 \\sim O1A-C1A
 with sigma of 0.02
 O2-C1 \\sim O2A-C1A
 with sigma of 0.02
 C2-C1 \\sim C2-C1A
 with sigma of 0.02
 O1-O2 \\sim O1A-O2A
 with sigma of 0.04
 O1-C2 \\sim O1A-C2
 with sigma of 0.04
 O2-C2 \\sim O2A-C2
 with sigma of 0.04
3. Rigid bond restraints
 Zn1, O1
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O3) = Uanis(O3A)
Uanis(C9) = Uanis(C9A)
Uanis(O4) = Uanis(O4A)
Uanis(O2) = Uanis(O2A)
Uanis(O1) = Uanis(O1A)
Uanis(C1) = Uanis(C1A)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O4(0.5) O3(0.5) O1(0.5) O2(0.5) C9(0.5) C1(0.5) O2W(0.75)
 H2WA(0.75) H2WB(0.75) O4A(0.5) C9A(0.5) O3A(0.5) O1A(0.5) C1A(0.5) O2A(0.5)
7.a Free rotating group:
 O1W(H1WA,H1WB,O2W,H2WA,H2WB)
7.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B)
7.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C5(H5), C18(H18), C15(H15), C11(H11), C10(H10), C16(H16),
 C22(H22), C23(H23), C17(H17)
7.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              74804
_shelx_hkl_checksum              98726
_olex2_submission_special_instructions 'No special instructions were received'