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_2312380
_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         'C48 H46 N4 Na2 O16, C3 H7 N O'
_chemical_formula_sum            'C51 H53 N5 Na2 O17'
_chemical_formula_weight         1053.96
_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             2023-09-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                71.631(3)
_cell_angle_beta                 76.965(4)
_cell_angle_gamma                68.737(4)
_cell_formula_units_Z            1
_cell_length_a                   9.0522(4)
_cell_length_b                   10.7406(4)
_cell_length_c                   15.0867(5)
_cell_measurement_reflns_used    10007
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      77.2940
_cell_measurement_theta_min      3.1180
_cell_volume                     1287.01(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.946
_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    -62.00 -37.00   0.50    1.50    --  -47.35 128.00-134.00   50
  2  \w    -95.00 -69.00   0.50    1.50    --  -47.35 142.00  36.00   52
  3  \w   -118.00 -62.00   0.50    1.50    --  -47.35-142.00 -20.00  112
  4  \w   -119.00 -94.00   0.50    1.50    --  -47.35-128.00 150.00   50
  5  \w     56.00  85.00   0.50    1.50    --   47.35-128.00 150.00   58
  6  \w     61.00 105.00   0.50    1.50    --   47.35-142.00 -20.00   88
  7  \w     86.00 114.00   0.50    1.50    --   47.35 128.00-134.00   56
  8  \w     69.00 119.00   0.50    1.50    --   47.35 142.00  36.00  100
  9  \w   -119.00 -93.00   0.50    7.00    -- -106.00 142.00  36.00   52
 10  \w   -150.00 -72.00   0.50    7.00    -- -106.00-128.00 150.00  156
 11  \w   -117.00 -92.00   0.50    7.00    -- -106.00-142.00 -20.00   50
 12  \w   -113.00 -71.00   0.50    7.00    -- -106.00 128.00-134.00   84
 13  \w    105.00 131.00   0.50    7.00    --  113.25 142.00  36.00   52
 14  \w     54.00  79.00   0.50    7.00    --  113.25-128.00 150.00   50
 15  \w     78.00 150.00   0.50    7.00    --  113.25 128.00-134.00  144
 16  \w     97.00 124.00   0.50    7.00    --  113.25-142.00 -20.00   54
 17  \w    -42.00  20.00   0.50    1.50    --  -47.35  37.00-180.00  124
 18  \w    -25.00  27.00   0.50    1.50    --  -47.35  19.00  60.00  104
 19  \w    -24.00  25.00   0.50    1.50    --   47.35 -19.00  30.00   98
 20  \w     27.00 110.00   0.50    1.50    --   47.35  77.00-180.00  166
 21  \w     82.00 110.00   0.50    1.50    --   47.35 125.00 120.00   56
 22  \w   -108.00 -79.00   0.50    7.00    -- -106.00 111.00 157.63   58
 23  \w    -74.00 -37.00   0.50    7.00    -- -106.00 111.00 157.63   74
 24  \w    -71.00 -33.00   0.50    7.00    -- -106.00  61.00 -30.00   76
 25  \w    -65.00 -39.00   0.50    7.00    -- -106.00 144.00-133.80   52
 26  \w   -108.00 -38.00   0.50    7.00    -- -106.00 111.00 113.10  140
 27  \w   -126.00 -94.00   0.50    7.00    -- -106.00 144.00-133.80   64
 28  \w    -64.00 -39.00   0.50    7.00    -- -106.00  61.00  90.00   50
 29  \w   -166.00-108.00   0.50    7.00    -- -106.00 -61.00-150.00  116
 30  \w   -107.00 -40.00   0.50    7.00    -- -106.00 109.00-160.50  134
 31  \w   -106.00 -41.00   0.50    7.00    -- -106.00 125.00 -60.00  130
 32  \w    -73.00 -48.00   0.50    7.00    -- -106.00 115.00 -83.23   50
 33  \w   -175.00-130.00   0.50    7.00    -- -106.00 -30.00 150.00   90
 34  \w   -109.00 -79.00   0.50    7.00    -- -106.00 115.00 -83.23   60
 35  \w   -112.00 -33.00   0.50    7.00    -- -106.00 125.00-150.00  158
 36  \w   -166.00 -92.00   0.50    7.00    -- -106.00 -15.00  30.00  148
 37  \w     43.00  99.00   0.50    7.00    --  113.25 -94.00 150.00  112
 38  \w     42.00  70.00   0.50    7.00    --  113.25 -61.00  30.00   56
 39  \w     80.00 105.00   0.50    7.00    --  113.25 -77.00  30.00   50
 40  \w     46.00  76.00   0.50    7.00    --  113.25 -77.00  30.00   60
 41  \w    101.00 160.00   0.50    7.00    --  113.25  45.00-150.00  118
 42  \w     81.00 109.00   0.50    7.00    --  113.25-125.00  60.00   56
 43  \w     48.00  97.00   0.50    7.00    --  113.25 -77.00   0.00   98
 44  \w    136.00 162.00   0.50    7.00    --  113.25  30.00-120.00   52
 45  \w     43.00  69.00   0.50    7.00    --  113.25-125.00  60.00   52
 46  \w     63.00  89.00   0.50    7.00    --  113.25 -94.00-180.00   52
 47  \w     73.00  99.00   0.50    7.00    --  113.25 -77.00-180.00   52
 48  \w    103.00 178.00   0.50    7.00    --  113.25  30.00 150.00  150
 49  \w     47.00  93.00   0.50    7.00    --  113.25 -94.00   0.00   92
 50  \w    104.00 175.00   0.50    7.00    --  113.25  45.00-180.00  142
 51  \w     92.00 132.00   0.50    7.00    --  113.25  77.00 -60.00   80
 52  \w     42.00  67.00   0.50    7.00    --  113.25 -61.00 -30.00   50
;
_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      0.0028263000
_diffrn_orient_matrix_UB_12      0.0520336000
_diffrn_orient_matrix_UB_13      -0.1077217000
_diffrn_orient_matrix_UB_21      0.1837616000
_diffrn_orient_matrix_UB_22      -0.0429039000
_diffrn_orient_matrix_UB_23      -0.0117491000
_diffrn_orient_matrix_UB_31      0.0104547000
_diffrn_orient_matrix_UB_32      -0.1442774000
_diffrn_orient_matrix_UB_33      -0.0045862000
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18234
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.526
_diffrn_reflns_theta_min         3.111
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97134
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5345
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0640
_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^)+(0.1225P)^2^+0.7824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4679
_reflns_number_total             5345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aw5081sup1.cif
_cod_data_source_block           4
_cod_original_cell_volume        1287.01(10)
_cod_database_code               2312380
_publcif_datablock.id            {6a250d3e-cab9-48c7-a478-3a23dac8c126}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H10 O6'
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.906
_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. Restrained distances
 C28-O19
 1.22 with sigma of 0.02
 C28-N3
 1.36 with sigma of 0.02
 N3-C30
 1.45 with sigma of 0.02
 N3-C29
 1.46 with sigma of 0.02
 C28-C30
 2.46 with sigma of 0.04
 C28-C29
 2.45 with sigma of 0.04
 N3-C30 \\sim N3-C29
 with sigma of 0.02
3. Restrained planarity
 C28, O19, N3, C30, C29
 with sigma of 0.1
4. Rigid bond restraints
 C22, O17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
C28 \\sim O19 \\sim N3 \\sim C30 \\sim C29: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C30 \\sim N3 \\sim C28 \\sim C29: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
6. Rigid body (RIGU) restrains
 C28, O19, N3, C30, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: C28(0.5) H28(0.5) O19(0.5) N3(0.5) C30(0.5) H30A(0.5) H30B(0.5)
 H30C(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C2(H2), C15(H15), C16(H16A), C6(H6), C5(H5), C25(H25), C22(H22),
 C28(H28)
8.b Tetrahedral OH refined with riding coordinates:
 O14(H14)
8.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C)
8.d Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_shelx_res_checksum              79190
_shelx_hkl_checksum              93499
_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 1.401
_oxdiff_exptl_absorpt_empirical_full_min 0.812
_publcif_info_exptl_table_max_cols 5
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
'<span class="funder"><span class="fundref-name" data-id="">Aromaticheskie diatsetilenu kak osnova dlya sinteza novukh kristallicheskikh form ugleroda </span><span class="fundref-subname" data-id=""></span> (<span class="fundref-grant-group"><span class="fundref-grant-type">grant</span> No. <span class="fundref-grant-id">23-1300045</span></span>).</span>'
_cod_database_fobs_code 2312380