Design and synthesis of two functional coordination polymers based on the 1,1′-bis(3-carboxybenzyl)-4,4′-bipyridinium ligand
Chen, Jiali; Fu, Yuying; Liu, Qiaoyun; Shen, Shoujie; Liu, Jinjian; CrystEngComm 26 (2024) 5518–5524; doi:10.1039/D4CE00732H

data_7249373
_publ_section_title
;
 Design and synthesis of two functional coordination polymers based on the
 1,1&#x2032;-bis(3-carboxybenzyl)-4,4&#x2032;-bipyridinium ligand
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              5518
_journal_page_last               5524
_journal_paper_doi               10.1039/D4CE00732H
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C18 H13 N O7 Zn'
_chemical_formula_sum            'C18 H13 N O7 Zn'
_chemical_formula_weight         420.66
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-08 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.246(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9146(4)
_cell_length_b                   10.0980(3)
_cell_length_c                   15.0368(4)
_cell_measurement_reflns_used    6211
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0350
_cell_measurement_theta_min      4.0290
_cell_volume                     1635.76(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.935
_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    -73.00 -22.00   1.00    5.00    --  -18.75 126.00  96.00   51
  2  \w     10.00  37.00   1.00    5.00    --   20.16-145.00-147.00   27
  3  \w     49.00  74.00   1.00    5.00    --   20.16-126.00  19.00   25
  4  \w     -2.00  32.00   1.00    5.00    --   20.16-126.00  19.00   34
  5  \w    -32.00  -6.00   1.00    5.00    --  -18.75 -38.00  60.00   26
  6  \w    -88.00 -60.00   1.00    5.00    --  -18.75 -38.00  60.00   28
  7  \w    -82.00 -57.00   1.00    5.00    --  -18.75 145.00 -96.00   25
  8  \w    -19.00  11.00   1.00    5.00    --  -18.75 -99.00-150.00   30
  9  \w      6.00  87.00   1.00    5.00    --   20.16  57.00 150.00   81
 10  \w      0.00  74.00   1.00    5.00    --   20.16-125.00  87.03   74
 11  \w    -25.00  58.00   1.00    5.00    --   20.16 -99.00 -60.00   83
 12  \w    -25.00  59.00   1.00    5.00    --   20.16 -99.00-150.00   84
 13  \w      1.00  89.00   1.00    5.00    --   20.16  38.00-120.00   88
 14  \w     28.00  89.00   1.00    5.00    --   20.16  38.00 -60.00   61
 15  \w     17.00  87.00   1.00    5.00    --   20.16  57.00  60.00   70
 16  \w     -2.00  88.00   1.00    5.00    --   20.16  77.00 -30.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0029669000
_diffrn_orient_matrix_UB_12      -0.0591621000
_diffrn_orient_matrix_UB_13      0.0256600000
_diffrn_orient_matrix_UB_21      0.0057064000
_diffrn_orient_matrix_UB_22      0.0378486000
_diffrn_orient_matrix_UB_23      0.0401962000
_diffrn_orient_matrix_UB_31      -0.0655409000
_diffrn_orient_matrix_UB_32      0.0006253000
_diffrn_orient_matrix_UB_33      -0.0030582000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34381
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.965
_diffrn_reflns_theta_min         3.219
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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    1.708
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4871
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0400P)^2^+1.9713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3118
_reflns_number_total             4871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00732h2.cif
_cod_data_source_block           exp_437_auto
_cod_depositor_comments
'Adding full bibliography for 7249372--7249373.cif.'
_cod_database_code               7249373
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N'
_shelx_estimated_absorpt_t_max   0.747
_shelx_estimated_absorpt_t_min   0.654
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-C17 = C17-O21
 1.25 with sigma of 0.02
 O6-C17 = C17-O20
 1.25 with sigma of 0.02
 O4-C14 = C14-O5
 1.25 with sigma of 0.02
 O8-C14 = C14-O9
 1.25 with sigma of 0.02
 O7-O21
 2.165 with sigma of 0.04
 O6-O20
 2.165 with sigma of 0.04
 O4-O5
 2.165 with sigma of 0.04
 O8-O9
 2.165 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C8 \\sim N1 \\sim C9 \\sim C11 \\sim C13 \\sim C12 \\sim C10 \\sim C7: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O4, C14, O5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O8, C14, O9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O20, C17, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O21, C17, O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O7)=Sof(O21)=Sof(O8)=Sof(O9)=1-FVAR(1)
 Sof(O6)=Sof(O4)=Sof(O5)=Sof(O20)=FVAR(1)
6.a Rotating group:
 O3(H3A,H3B)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
6.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C10(H10)
;
_shelx_res_checksum              77929
_shelx_hkl_checksum              90885
_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 1.096
_oxdiff_exptl_absorpt_empirical_full_min 0.869