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_7719795
_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         'C9 H5 K2 O7'
_chemical_formula_sum            'C9 H5 K2 O7'
_chemical_formula_weight         303.33
_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   mixed
_audit_creation_date             2024-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-05-13 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.165(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.71110(10)
_cell_length_b                   18.3859(4)
_cell_length_c                   16.3390(3)
_cell_measurement_reflns_used    2121
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.1880
_cell_measurement_theta_min      3.6120
_cell_volume                     1114.61(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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     44.00  72.00   1.00    1.00    --    0.00  37.00 120.00   28
  2  \w     15.00  43.00   1.00    1.00    --    0.00  37.00 120.00   28
  3  \w    -19.00   8.00   1.00    1.00    --    0.00  37.00 120.00   27
  4  \w     11.00  38.00   1.00    5.00    --   54.00 -99.00 -60.00   27
  5  \w     42.00  72.00   1.00    5.00    --   54.00-125.00-120.00   30
  6  \w     73.00 116.00   1.00    5.00    --  108.00-111.00 -60.00   43
  7  \w     60.00  95.00   1.00    5.00    --  108.00-111.00  60.00   35
  8  \w     73.00 112.00   1.00    5.00    --  108.00-111.00  90.00   39
  9  \w     33.00  73.00   1.00    5.00    --   54.00-125.00  30.00   40
 10  \w     37.00 134.00   1.00    5.00    --  108.00 -37.00 -90.00   97
 11  \w    118.00 177.00   1.00    5.00    --  108.00  50.00   0.00   59
 12  \w    128.00 161.00   1.00    5.00    --  108.00  63.00 -90.00   33
 13  \w    100.00 130.00   1.00    5.00    --  108.00 111.00 120.00   30
 14  \w     46.00 131.00   1.00    5.00    --  108.00 -37.00  60.00   85
 15  \w     43.00 126.00   1.00    5.00    --  108.00 -63.00-180.00   83
 16  \w      0.00 113.00   1.00    5.00    --   54.00   0.00-120.00  113
;
_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      -0.0077893000
_diffrn_orient_matrix_UB_12      -0.0556734000
_diffrn_orient_matrix_UB_13      0.0703465000
_diffrn_orient_matrix_UB_21      0.0909898000
_diffrn_orient_matrix_UB_22      0.0608917000
_diffrn_orient_matrix_UB_23      0.0619119000
_diffrn_orient_matrix_UB_31      -0.4048718000
_diffrn_orient_matrix_UB_32      0.0147418000
_diffrn_orient_matrix_UB_33      0.0106690000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3969
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.988
_diffrn_reflns_theta_min         3.619
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.802
_exptl_absorpt_correction_T_max  0.536
_exptl_absorpt_correction_T_min  0.411
_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    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.485
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0829P)^2^+1.9789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1959
_reflns_number_total             2090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01954k2.cif
_cod_data_source_block           3_H2O
_cod_database_code               7719795
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'K3 O6 C9 H3'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6)
;
_shelx_res_checksum              24025
_shelx_hkl_checksum              76170
_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 2.453
_oxdiff_exptl_absorpt_empirical_full_min 0.577