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_2312378
_publ_section_title
;
 1D and 2D coordination polymers with a new rigid chelating linker:
 diacetylenedisalicylic acid.
;
_journal_coeditor_code           AW5081
_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         'C20 H14 O6'
_chemical_formula_sum            'C20 H14 O6'
_chemical_formula_weight         350.31
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-11-29 # Formatted by IUCr publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90.336(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.82699(9)
_cell_length_b                   35.3044(7)
_cell_length_c                   5.73042(13)
_cell_measurement_reflns_used    4879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.0500
_cell_measurement_theta_min      2.4930
_cell_volume                     774.22(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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     25.00  54.00   0.50    0.15    --   47.35  77.00  23.00   58
  2  \w   -175.00-135.00   0.50    0.60    -- -106.00 -77.00  13.00   80
  3  \w    -82.00 -57.00   0.50    0.60    -- -106.00  68.00 -94.00   50
  4  \w   -132.00 -95.00   0.50    0.60    -- -106.00 -77.00  13.00   74
  5  \w     42.00 104.00   0.50    0.60    --  113.25 -77.00-102.00  124
  6  \w   -118.00 -74.00   0.50    0.15    --  -47.35-125.00  60.00   88
  7  \w     85.00 113.00   0.50    0.15    --   47.35 125.00  90.00   56
  8  \w     66.00  93.00   0.50    0.15    --   47.35  77.00  23.00   54
  9  \w     90.00 116.00   0.50    0.15    --   47.35 125.00   0.00   52
 10  \w    -71.00 -34.00   0.50    0.60    -- -106.00  61.00  60.00   74
 11  \w   -129.00-102.00   0.50    0.60    -- -106.00 -68.00 131.00   54
 12  \w     42.00  67.00   0.50    0.60    --  113.25 -61.00  60.00   50
 13  \w     44.00  71.00   0.50    0.60    --  113.25 -61.00 -90.00   54
 14  \w     43.00  69.00   0.50    0.60    --  113.25 -61.00  30.00   52
 15  \w     45.00  71.00   0.50    0.60    --  113.25 -77.00-180.00   52
 16  \w     77.00 102.00   0.50    0.60    --  113.25 -77.00-180.00   50
 17  \w     43.00  68.00   0.50    0.60    --  113.25 -61.00 -60.00   50
 18  \w   -158.00 -85.00   0.50    0.60    -- -106.00 -77.00-102.00  146
 19  \w   -119.00 -72.00   0.50    0.15    --  -47.35 -37.00  90.00   94
 20  \w    -25.00   4.00   0.50    0.15    --  -47.35  19.00  30.00   58
 21  \w    -65.00 -39.00   0.50    0.15    --  -47.35 -37.00  90.00   52
 22  \w    -18.00  20.00   0.50    0.15    --   47.35 -19.00  90.00   76
 23  \w    -20.00  15.00   0.50    0.15    --   47.35 -19.00 120.00   70
 24  \w    -26.00  34.00   0.50    0.15    --   47.35 -37.00-120.00  120
 25  \w    -61.00 -36.00   0.50    0.60    -- -106.00  61.00-120.00   50
 26  \w   -173.00-117.00   0.50    0.60    -- -106.00 -45.00-150.00  112
 27  \w    -69.00 -43.00   0.50    0.60    -- -106.00  61.00 -30.00   52
 28  \w   -109.00 -83.00   0.50    0.60    -- -106.00 -94.00 150.00   52
 29  \w    -65.00 -39.00   0.50    0.60    -- -106.00 125.00 150.00   52
 30  \w   -169.00-143.00   0.50    0.60    -- -106.00 -94.00 150.00   52
 31  \w   -111.00 -70.00   0.50    0.60    -- -106.00 125.00 150.00   82
 32  \w    -60.00 -33.00   0.50    0.60    -- -106.00  61.00  30.00   54
 33  \w   -119.00 -93.00   0.50    0.60    -- -106.00 -61.00 150.00   52
 34  \w   -121.00 -94.00   0.50    0.60    -- -106.00 -15.00 150.00   54
 35  \w   -161.00-128.00   0.50    0.60    -- -106.00 -15.00 150.00   66
 36  \w    -61.00 -35.00   0.50    0.60    -- -106.00  61.00   0.00   52
 37  \w    103.00 129.00   0.50    0.60    --  113.25  61.00 -30.00   52
 38  \w     56.00  91.00   0.50    0.60    --  113.25 -94.00   0.00   70
 39  \w    140.00 171.00   0.50    0.60    --  113.25  45.00 120.00   62
 40  \w    151.00 177.00   0.50    0.60    --  113.25  77.00 -60.00   52
 41  \w     93.00 138.00   0.50    0.60    --  113.25  77.00 -60.00   90
 42  \w    108.00 133.00   0.50    0.60    --  113.25  45.00 120.00   50
 43  \w    132.00 177.00   0.50    0.60    --  113.25  45.00  90.00   90
 44  \w     44.00  57.00   0.50    0.60    --  113.25 -61.00 -60.00   26
;
_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      0.0809698000
_diffrn_orient_matrix_UB_12      -0.0320149000
_diffrn_orient_matrix_UB_13      -0.1742781000
_diffrn_orient_matrix_UB_21      0.3269977000
_diffrn_orient_matrix_UB_22      -0.0107096000
_diffrn_orient_matrix_UB_23      0.1434466000
_diffrn_orient_matrix_UB_31      -0.2204385000
_diffrn_orient_matrix_UB_32      -0.0276510000
_diffrn_orient_matrix_UB_33      0.1459932000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7056
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.967
_diffrn_reflns_theta_min         2.503
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60304
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       prism
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0786P)^2^+0.2117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1356
_reflns_number_total             1474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aw5081sup1.cif
_cod_data_source_block           1
_cod_database_code               2312378
_publcif_datablock.id            {0a6ae591-df22-4906-a91f-6b4e057d26a1}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H14 O6'
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.820
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              4083
_shelx_hkl_checksum              3411
_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 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.661
_cod_database_fobs_code 2312378