New 3,5-bis(3,4-dicarboxyphenoxy)benzoic acid-appended Mn(ii) coordination polymers: synthesis, characterization and antibiotic photodegradation properties
Wu, Hang; Ghosh, Mithun Kumar; Wang, Guang-Li; Wang, Jun; Muddassir, Mohd.; Ghorai, Tanmay Kumar; Kushwaha, Aparna; Srivastava, Devyani; Kumar, Abhinav; CrystEngComm 26 (2024) 1453–1463; doi:10.1039/D3CE01285A

data_7248053
_publ_section_title
;
 New 3,5-bis(3,4-dicarboxyphenoxy)benzoic acid-appended Mn(ii)
 coordination polymers: synthesis, characterization and antibiotic
 photodegradation properties
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1453
_journal_page_last               1463
_journal_paper_doi               10.1039/D3CE01285A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C28 H23 Mn2 N O15'
_chemical_formula_sum            'C28 H23 Mn2 N O15'
_chemical_formula_weight         723.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-06-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2023-07-20 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.408(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1417(2)
_cell_length_b                   18.8610(3)
_cell_length_c                   16.4838(2)
_cell_measurement_reflns_used    7577
_cell_measurement_temperature    212.99(10)
_cell_measurement_theta_max      75.7060
_cell_measurement_theta_min      3.6000
_cell_volume                     3039.74(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      212.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.940
_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    105.00 130.00   1.00    0.90    --  105.98 110.00 -18.00   25
  2  \w     83.00 178.00   1.00    0.90    --  105.98  77.00  30.00   95
  3  \w     92.00 178.00   1.00    0.90    --  105.98  15.00   0.00   86
  4  \w     39.00  98.00   1.00    0.90    --  105.98 -94.00 -90.00   59
  5  \w     33.00 104.00   1.00    0.90    --  105.98-110.00-114.00   71
  6  \w     35.00 105.00   1.00    0.90    --  105.98 -77.00 -90.00   70
  7  \w     33.00  62.00   1.00    0.90    --  105.98 -61.00 150.00   29
  8  \w     76.00 103.00   1.00    0.90    --  105.98-125.00   0.00   27
  9  \w     36.00  72.00   1.00    0.90    --  105.98-125.00   0.00   36
 10  \w     42.00  68.00   1.00    0.20    --   48.46-110.00-114.00   26
 11  \w    -27.00  26.00   1.00    0.20    --  -48.46  19.00 -90.00   53
 12  \w    -48.00 -20.00   1.00    0.90    --  -91.75  45.00 120.00   28
 13  \w    -51.00 -21.00   1.00    0.90    --  -91.75  45.00 150.00   30
 14  \w    -71.00 -19.00   1.00    0.90    --  -91.75  61.00 150.00   52
 15  \w    -82.00 -32.00   1.00    0.90    --  -91.75 110.00 -18.00   50
 16  \w    -81.00  -5.00   1.00    0.20    --  -48.46 110.00 -18.00   76
 17  \w   -147.00-122.00   1.00    0.90    --  -91.75-110.00-114.00   25
 18  \w   -119.00 -73.00   1.00    0.20    --  -48.46-125.00 -30.00   46
 19  \w   -120.00 -73.00   1.00    0.20    --  -48.46-125.00  60.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1430892000
_diffrn_orient_matrix_UB_12      -0.0318816000
_diffrn_orient_matrix_UB_13      0.0374606000
_diffrn_orient_matrix_UB_21      0.0650516000
_diffrn_orient_matrix_UB_22      0.0731135000
_diffrn_orient_matrix_UB_23      -0.0052215000
_diffrn_orient_matrix_UB_31      -0.0105677000
_diffrn_orient_matrix_UB_32      0.0176467000
_diffrn_orient_matrix_UB_33      0.0893006000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19316
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.140
_diffrn_reflns_theta_min         3.637
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
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    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.071
_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     437
_refine_ls_number_reflns         5971
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0498P)^2^+3.5104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5215
_reflns_number_total             5971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01285a2.cif
_cod_data_source_block           wj_6_sq
_cod_depositor_comments
'Adding full bibliography for 7248053--7248056.cif.'
_cod_database_code               7248053
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNO
_shelx_estimated_absorpt_t_max   0.318
_shelx_estimated_absorpt_t_min   0.155
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C27-C26A = C26A-C25A = C25A-C24 = C25-C24 = C26-C25 = C27-C26
 1.48 with sigma of 0.01
3. Rigid bond restraints
 C24, N1, C27, C28, C25, C26, C26A, C25A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C24 \\sim N1 \\sim C27 \\sim C28 \\sim C25 \\sim C26 \\sim C26A \\sim C25A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Sof(H27C)=Sof(H27D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C25A)=Sof(H25C)=
 Sof(H25D)=1-FVAR(1)
 Sof(H27A)=Sof(H27B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 FVAR(1)
6.a Riding coordinates:
 O11(H11)
6.b Rotating group:
 O14(H14A,H14B), O15(H15A,H15B)
6.c Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C27(H27C,H27D), C25(H25A,H25B), C26(H26A,H26B), C26A(H26C,
 H26D), C25A(H25C,H25D)
6.d Aromatic/amide H refined with riding coordinates:
 C12(H12), C17(H17), C3(H3), C9(H9), C5(H5), C13(H13), C7(H7), C20(H20),
 C21(H21)
6.e Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44457
_shelx_fab_checksum              36366
_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 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.868