Mechanochemistry Unlocking Stoichiometric Control in Alkali Metal Carboxylate Coordination Polymers
Leszczyński, Michał Krzysztof; Justyniak, Iwona; Lewinski, Janusz; Dalton Transactions  (2025) –; doi:10.1039/D5DT01954K

data_7719794
_publ_section_title
;
 Mechanochemistry Unlocking Stoichiometric Control in Alkali Metal
 Carboxylate Coordination Polymers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT01954K
_journal_year                    2025
_chemical_formula_moiety         'C36 H22 Na8 O36'
_chemical_formula_sum            'C36 H22 Na8 O36'
_chemical_formula_weight         1214.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-05-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2025-05-13 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6598(4)
_cell_length_b                   14.5235(8)
_cell_length_c                   42.4090(18)
_cell_measurement_reflns_used    7101
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      70.4290
_cell_measurement_theta_min      3.2170
_cell_volume                     4717.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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    -80.00 -38.00   1.00    7.50    --    0.00 178.00 -90.00   42
  2  \w     24.00  59.00   1.00    7.50    --    0.00  57.00-120.00   35
  3  \w    -80.00 -48.00   1.00    7.50    --    0.00 178.00   0.00   32
  4  \w     29.00 129.00   1.00   15.00    --   56.00  45.00-150.00  100
  5  \w     55.00  85.00   1.00   15.00    --   56.00 -94.00  60.00   30
  6  \w     27.00  53.00   1.00   15.00    --   56.00 -61.00-150.00   26
  7  \w    -16.00  77.00   1.00   15.00    --   56.00 -45.00 -60.00   93
  8  \w    102.00 154.00   1.00   35.00    --  112.00 -25.00  60.00   52
  9  \w     90.00 115.00   1.00   35.00    --  112.00-111.00 -30.00   25
 10  \w    143.00 169.00   1.00   35.00    --  112.00  25.00 -90.00   26
 11  \w    127.00 154.00   1.00   35.00    --  112.00  77.00 -90.00   27
 12  \w     38.00  84.00   1.00   35.00    --  112.00 -25.00  60.00   46
 13  \w     98.00 170.00   1.00   35.00    --  112.00  63.00-120.00   72
 14  \w     74.00 101.00   1.00   35.00    --  112.00 -25.00-180.00   27
 15  \w     38.00  83.00   1.00   35.00    --  112.00-111.00 -30.00   45
 16  \w    108.00 147.00   1.00   35.00    --  112.00 111.00-180.00   39
 17  \w     79.00 134.00   1.00   35.00    --  112.00 -63.00  30.00   55
 18  \w    109.00 143.00   1.00   35.00    --  112.00 -25.00-180.00   34
 19  \w    112.00 140.00   1.00   35.00    --  112.00 -67.00 144.48   28
 20  \w    101.00 126.00   1.00   35.00    --  112.00 111.00 -60.00   25
 21  \w     56.00  89.00   1.00   35.00    --  112.00 -67.00 144.48   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1178272000
_diffrn_orient_matrix_UB_12      -0.0597374000
_diffrn_orient_matrix_UB_13      0.0211650000
_diffrn_orient_matrix_UB_21      -0.0530374000
_diffrn_orient_matrix_UB_22      0.0581567000
_diffrn_orient_matrix_UB_23      0.0288559000
_diffrn_orient_matrix_UB_31      -0.1540415000
_diffrn_orient_matrix_UB_32      -0.0656126000
_diffrn_orient_matrix_UB_33      0.0062812000
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            15482
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.646
_diffrn_reflns_theta_min         2.084
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.977
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.666
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.35(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         8496
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1139P)^2^+2.3988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1683
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_full    0.891
_reflns_Friedel_fraction_max     0.862
_reflns_number_gt                7701
_reflns_number_total             8496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01954k2.cif
_cod_data_source_block           2_3H2O
_cod_database_code               7719794
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Na2 O6 C20 H20'
_reflns_odcompleteness_completeness 93.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.65(9)
 0.35(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Na3-H11A \\sim Na3-H11B
 with sigma of 0.02
 Na7-H27A \\sim Na7-H27B
 with sigma of 0.02
 Na5-H36A \\sim Na5-H36B
 with sigma of 0.02
 Na4-H18A \\sim Na4-H18B
 with sigma of 0.02
4.a Free rotating group:
 O11(H11A,H11B), O18(H18A,H18B), O27(H27A,H27B), O36(H36A,H36B)
4.b Rotating group:
 O1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C11(H11), C13(H13), C15(H15), C20(H20), C22(H22),
 C24(H24), C30(H30), C32(H32), C34(H34)
;
_shelx_res_checksum              83703
_shelx_hkl_checksum              71625
_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 3.429
_oxdiff_exptl_absorpt_empirical_full_min 0.340