1D and 2D coordination polymers with a new rigid chelating linker: diacetylenedisalicylic acid.
Naifert, Sergei A.; Osipov, Artem A.; Efremov, Andrey N.; Rajakumar, Kanthapazham; Uchaev, Daniil A.; Zherebtsov, Dmitry A.; Belov, Kirill N.; Acta crystallographica Section B, Structural science, crystal engineering and materials 80 (2024) –; doi:10.1107/S205252062301017X

data_2312379
_publ_section_title
;
 1D and 2D coordination polymers with a new rigid chelating linker:
 diacetylenedisalicylic acid.
;
_journal_issue                   1
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_paper_doi               10.1107/S205252062301017X
_journal_volume                  80
_journal_year                    2024
_chemical_formula_moiety         'C18 H9 O6, C2 H8 N'
_chemical_formula_sum            'C20 H17 N O6'
_chemical_formula_weight         367.35
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5705(2)
_cell_length_b                   12.5736(2)
_cell_length_c                   13.5708(2)
_cell_measurement_reflns_used    8392
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      78.6050
_cell_measurement_theta_min      3.8290
_cell_volume                     1973.83(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (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      100(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     90.00 116.00   0.50    0.60    --   47.35  50.00  60.00   52
  2  \w     36.00  77.00   0.50    0.60    --   47.35  50.00  60.00   82
  3  \w    -21.00  24.00   0.50    0.60    --   47.35 -50.00 -85.00   90
  4  \w     30.00  55.00   0.50    0.60    --   47.35 -50.00 -85.00   50
  5  \w   -177.00-152.00   0.50    2.90    -- -106.00 -50.00 -85.00   50
  6  \w    100.00 175.00   0.50    2.90    --  113.25  50.00  60.00  150
  7  \w    -18.00  25.00   0.50    0.60    --  -47.35  50.00  60.00   86
  8  \w   -119.00 -38.00   0.50    0.60    --  -47.35 -50.00 -85.00  162
  9  \w    -48.00 -22.00   0.50    0.60    --  -47.35  50.00  60.00   52
 10  \w    -27.00  25.00   0.50    0.60    --   47.35 -19.00 120.00  104
 11  \w     88.00 119.00   0.50    0.60    --   47.35 125.00 -60.00   62
 12  \w   -132.00 -89.00   0.50    2.90    -- -106.00 -61.00   0.00   86
 13  \w   -176.00-148.00   0.50    2.90    -- -106.00 -61.00   0.00   56
 14  \w   -143.00 -93.00   0.50    2.90    -- -106.00 -30.00 150.00  100
 15  \w    -65.00 -33.00   0.50    2.90    -- -106.00  61.00 -90.00   64
 16  \w    -64.00 -36.00   0.50    2.90    -- -106.00  61.00-120.00   56
 17  \w   -124.00 -94.00   0.50    2.90    -- -106.00 -50.00 -85.00   60
 18  \w    -71.00 -37.00   0.50    2.90    -- -106.00  61.00  60.00   68
 19  \w   -106.00 -72.00   0.50    2.90    -- -106.00  77.00  90.00   68
 20  \w    -60.00 -35.00   0.50    2.90    -- -106.00  77.00  90.00   50
 21  \w     62.00  87.00   0.50    2.90    --  113.25 -77.00-150.00   50
 22  \w     42.00  86.00   0.50    2.90    --  113.25 -77.00 120.00   88
 23  \w     43.00  70.00   0.50    2.90    --  113.25 -61.00 150.00   54
 24  \w     42.00  69.00   0.50    2.90    --  113.25 -61.00 -90.00   54
 25  \w     42.00  67.00   0.50    2.90    --  113.25 -61.00-180.00   50
 26  \w     44.00  71.00   0.50    2.90    --  113.25 -61.00 120.00   54
 27  \w     42.00 109.00   0.50    2.90    --  113.25-125.00   0.00  134
 28  \w     44.00  69.00   0.50    2.90    --  113.25 -61.00 -30.00   50
 29  \w    101.00 175.00   0.50    2.90    --  113.25  15.00-150.00  148
 30  \w     66.00 100.00   0.50    2.90    --  113.25 -77.00 150.00   68
 31  \w     48.00 103.00   0.50    2.90    --  113.25 -94.00 -90.00  110
 32  \w     70.00  82.50   0.50    2.90    --  113.25 -94.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0413748000
_diffrn_orient_matrix_UB_12      0.0739069000
_diffrn_orient_matrix_UB_13      0.0826436000
_diffrn_orient_matrix_UB_21      -0.1261278000
_diffrn_orient_matrix_UB_22      -0.0162360000
_diffrn_orient_matrix_UB_23      -0.0355215000
_diffrn_orient_matrix_UB_31      -0.0105201000
_diffrn_orient_matrix_UB_32      -0.0963724000
_diffrn_orient_matrix_UB_33      0.0693125000
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14589
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.997
_diffrn_reflns_theta_min         4.795
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0607P)^2^+0.7745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3337
_reflns_number_total             3741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aw5081sup1.cif
_cod_data_source_block           3
_cod_database_code               2312379
_publcif_datablock.id            {3f7a9e7d-5a72-44dd-b9f0-026db28143be}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H10 O6'
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H2(0.5) H4(0.5)
3.a Secondary CH2 refined with riding coordinates:
 N7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C6(H6A), C9(H9), C10(H10), C12(H12)
3.c Tetrahedral OH refined with riding coordinates:
 O4(H4)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
3.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3), O6(H6)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82420
_shelx_hkl_checksum              33908
_shelx_fab_checksum              78997
_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 1.472
_oxdiff_exptl_absorpt_empirical_full_min 0.711
_cod_database_fobs_code 2312379