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_7248055
_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         'C33 H22 Mn N2 O13'
_chemical_formula_sum            'C33 H22 Mn N2 O13'
_chemical_formula_weight         709.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-01
_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                96.076(3)
_cell_angle_beta                 104.603(3)
_cell_angle_gamma                111.886(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2767(4)
_cell_length_b                   11.9402(4)
_cell_length_c                   12.4311(4)
_cell_measurement_reflns_used    7560
_cell_measurement_temperature    213.00(10)
_cell_measurement_theta_max      75.9890
_cell_measurement_theta_min      4.4300
_cell_volume                     1465.30(10)
_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      213.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.926
_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     28.00 121.00   1.00    0.10    --   48.46  77.00 150.00   93
  2  \w     71.00 104.00   1.00    0.10    --   48.46 169.00 138.00   33
  3  \w     67.00 118.00   1.00    0.50    --  105.98 169.00 138.00   51
  4  \w    106.00 152.00   1.00    0.50    --  105.98 115.00  -4.00   46
  5  \w     93.00 178.00   1.00    0.50    --  105.98  15.00-180.00   85
  6  \w     33.00  75.00   1.00    0.50    --  105.98 -77.00  60.00   42
  7  \w     28.00  63.00   1.00    0.10    --   48.46-115.00 -94.00   35
  8  \w     66.00  91.00   1.00    0.10    --   48.46-115.00 -94.00   25
  9  \w     80.00 105.00   1.00    0.50    --  105.98 -77.00  60.00   25
 10  \w     66.00  91.00   1.00    0.10    --   48.46-169.00 122.00   25
 11  \w    105.00 142.00   1.00    0.50    --  105.98-169.00 122.00   37
 12  \w     87.00 112.00   1.00    0.50    --  105.98-125.00 150.00   25
 13  \w     34.00  76.00   1.00    0.50    --  105.98-125.00 150.00   42
 14  \w     36.00 112.00   1.00    0.50    --  105.98-125.00 120.00   76
 15  \w     46.00  97.00   1.00    0.50    --  105.98 -94.00 150.00   51
 16  \w     43.00 111.00   1.00    0.50    --  105.98-125.00 -30.00   68
 17  \w     66.00 108.00   1.00    0.50    --  105.98-115.00 -94.00   42
 18  \w     33.00  66.00   1.00    0.50    --  105.98 -94.00-180.00   33
 19  \w     69.00 105.00   1.00    0.50    --  105.98 -94.00-180.00   36
 20  \w    -82.00  -7.00   1.00    0.10    --  -48.46 115.00  -4.00   75
 21  \w   -114.00 -82.00   1.00    0.10    --  -48.46 169.00 138.00   32
 22  \w   -100.00 -75.00   1.00    0.50    --  -91.75 169.00 138.00   25
 23  \w    -83.00 -31.00   1.00    0.50    --  -91.75 115.00  -4.00   52
 24  \w    -84.00 -19.00   1.00    0.50    --  -91.75 125.00 -60.00   65
 25  \w    -46.00 -21.00   1.00    0.50    --  -91.75  45.00  30.00   25
 26  \w    -48.00 -22.00   1.00    0.50    --  -91.75  45.00 -30.00   26
 27  \w    -50.00 -22.00   1.00    0.50    --  -91.75  45.00 -60.00   28
 28  \w    -51.00 -21.00   1.00    0.50    --  -91.75  45.00 150.00   30
 29  \w   -162.00-136.00   1.00    0.50    --  -91.75 -15.00 150.00   26
 30  \w   -115.00 -89.00   1.00    0.50    --  -91.75 -15.00 150.00   26
 31  \w   -159.00 -69.00   1.00    0.50    --  -91.75 -77.00 -60.00   90
 32  \w   -119.00 -28.00   1.00    0.10    --  -48.46 -77.00-120.00   91
 33  \w   -160.00 -81.00   1.00    0.50    --  -91.75 -45.00 -30.00   79
 34  \w   -121.00 -84.00   1.00    0.50    --  -91.75 -94.00 120.00   37
 35  \w   -161.00-126.00   1.00    0.50    --  -91.75 -94.00 120.00   35
 36  \w   -122.00 -88.00   1.00    0.50    --  -91.75-169.00 122.00   34
 37  \w    -81.00 -46.00   1.00    0.50    --  -91.75-169.00 122.00   35
 38  \w    -87.00 -55.00   1.00    0.10    --  -48.46-169.00 122.00   32
 39  \w   -106.00 -81.00   1.00    0.50    --  -91.75-115.00 -94.00   25
;
_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      0.0338655000
_diffrn_orient_matrix_UB_12      0.0838101000
_diffrn_orient_matrix_UB_13      -0.0839463000
_diffrn_orient_matrix_UB_21      0.0636860000
_diffrn_orient_matrix_UB_22      0.1151743000
_diffrn_orient_matrix_UB_23      0.0986453000
_diffrn_orient_matrix_UB_31      0.1373929000
_diffrn_orient_matrix_UB_32      -0.0071784000
_diffrn_orient_matrix_UB_33      0.0218467000
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17701
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.190
_diffrn_reflns_theta_min         4.093
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.351
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85992
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       plate
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         5683
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0707P)^2^+1.0804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4994
_reflns_number_total             5683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01285a2.cif
_cod_data_source_block           wj_1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7248053--7248056.cif.'
_cod_original_cell_volume        1465.30(9)
_cod_database_code               7248055
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNO
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Mn1-H13A \\sim Mn1-H13B
 with sigma of 0.02
3.a Riding coordinates:
 O3(H3)
3.b Free rotating group:
 O13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6A), C7(H7), C10(H10A), C12(H12), C14(H14), C17(H17), C20(H20),
 C21(H21), C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33)
3.d Tetrahedral OH refined with riding coordinates:
 O6(H6)
3.e Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_shelx_res_checksum              61673
_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 1.390
_oxdiff_exptl_absorpt_empirical_full_min 0.783