Selective detection of sulfasalazine antibiotic and its controllable photodegradation into 5-aminosalicylic acid by visible-light-responsive metal–organic framework
Li, Han-Shu; Gong, Yuxuan; Ji, Chen; Wu, Pengyan; Gao, Bingzhuo; Du, Yufan; Wang, Jian; Dalton Transactions  (2022) –; doi:10.1039/D2DT01270G

data_7710716
_publ_section_title
;
 Selective detection of sulfasalazine antibiotic and its controllable
 photodegradation into 5-aminosalicylic acid by visible-light-responsive
 metal--organic framework
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01270G
_journal_year                    2022
_chemical_formula_moiety
'C25 H10 Br3.534 Cl0.466 Co N1.25 O5, 1.5[CH4O]'
_chemical_formula_sum            'C26.5 H16 Br3.534 Cl0.466 Co N1.25 O6.5'
_chemical_formula_weight         813.760
_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'
_symmetry_Int_Tables_number      15
_audit_creation_date             2022-07-07
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.05.31 svn.r152b0213 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-07-08 deposited with the CCDC.	2022-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.847(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.753(3)
_cell_length_b                   16.409(3)
_cell_length_c                   16.565(3)
_cell_measurement_reflns_used    2259
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.288
_cell_measurement_theta_min      2.482
_cell_volume                     5338.5(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9939
_diffrn_measured_fraction_theta_max 0.9939
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.9939
_diffrn_reflns_Laue_measured_fraction_max 0.9939
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13615
_diffrn_reflns_point_group_measured_fraction_full 0.9939
_diffrn_reflns_point_group_measured_fraction_max 0.9939
_diffrn_reflns_theta_full        25.1572
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    6.026
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_description       block
_exptl_crystal_F_000             3154.492
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.5111
_refine_diff_density_min         -2.0741
_refine_diff_density_rms         0.2209
_refine_ls_d_res_high            0.8359
_refine_ls_d_res_low             7.3750
_refine_ls_goodness_of_fit_ref   1.0275
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    35
_refine_ls_number_parameters     391
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.0026
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+51.2878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              23
_reflns_limit_h_min              -24
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2907
_reflns_number_total             4759
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt01270g2.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        5338.6(15)
_cod_original_formula_sum        'C26.5 H16 Br3.534 Cl0.466 Co1 N1.25 O6.5'
_cod_database_code               7710716
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Shared sites
{Br1, Cl1}
{Br4, Cl4}
3. Restrained distances
 N1B-C21B = C21B-C22B = C22B-C23B = C23B-C24 = C24-C25 = C25-N1B
 1.39 with sigma of 0.01
 N1-C1C = C1C-C1D = C1D-C1E = C1E-C1A = C1A-C1B = C1B-N1
 1.39 with sigma of 0.01
 C25-Co1 \\sim Co1-C21B
 with sigma of 0.001
 C24-C1D \\sim C22B-C1A
 with sigma of 0.001
 N1B-C22B \\sim C21B-C23B \\sim C22B-C24 \\sim C23B-C25 \\sim C24-N1B \\sim
C25-C21B
 with sigma of 0.02
 N1-C1D \\sim C1C-C1E \\sim C1D-C1A \\sim C1E-C1B \\sim C1A-N1 \\sim C1B-C1C
 with sigma of 0.02
 Co1-N1B \\sim Co1-N1_$1
 with sigma of 0.01
4. Restrained planarity
 N1B, C21B, C22B, C23B, C24, C25
 with sigma of 0.1
 N1, C1C, C1D, C1E, C1A, C1B
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(Cl1)
Uanis(Br4) = Uanis(Cl4)
6. Rigid body (RIGU) restrains
 C24, C25, N1B, C21B, C22B, C23B, C1A, C1B, N1, C1C, C1D, C1E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C25, N1B, C21B, C22B, C23B, C1A, C1B, N1, C1C, C1D, C1E, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(Br1)=FVAR(1)
 Sof(Cl4)=1-FVAR(2)
 Sof(Br4)=FVAR(2)
 Fixed Sof: C24(0.5) H24(0.5) C25(0.5) H25(0.5) N1B(0.5) C21B(0.5) H21B(0.5)
 C22B(0.5) H22B(0.5) C23B(0.5) C1A(0.5) H1A(0.5) C1B(0.5) H1B(0.5) N1(0.5)
 C1C(0.5) H1C(0.5) C1D(0.5) C1E(0.5) N2(0.25) H2a(0.25) H2b(0.25)
8.a Rotating group:
 N2(H2a,H2b)
8.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C18(H18), C24(H24), C25(H25), C3(H3), C5(H5), C4(H4), C6(H6),
 C21B(H21B), C22B(H22B), C1A(H1A), C1B(H1B), C1C(H1C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 216 electrons were 
found in a volume of 520\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1.5[CH4O] per Formula Unit 
which account for 216 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'