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_7719796
_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 H9 O9 Rb2'
_chemical_formula_sum            'C9 H9 O9 Rb2'
_chemical_formula_weight         432.10
_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
_audit_creation_date             2024-05-30
_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                86.986(5)
_cell_angle_beta                 83.558(4)
_cell_angle_gamma                79.522(4)
_cell_formula_units_Z            2
_cell_length_a                   3.9898(2)
_cell_length_b                   10.1336(6)
_cell_length_c                   16.8294(9)
_cell_measurement_reflns_used    3001
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.0220
_cell_measurement_theta_min      2.6230
_cell_volume                     664.50(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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    -15.00  21.00   1.00    1.00    --    0.00 -77.00  30.00   36
  2  \w    -23.00   2.00   1.00    1.00    --    0.00  77.00-180.00   25
  3  \w     -2.00  27.00   1.00    1.00    --    0.00 -77.00 -30.00   29
  4  \w     13.00  42.00   1.00    1.00    --    0.00  77.00-180.00   29
  5  \w    -21.00   4.00   1.00    1.00    --    0.00 -77.00-120.00   25
  6  \w     43.00  96.00   1.00    4.00    --   54.00  57.00-180.00   53
  7  \w    -13.00  76.00   1.00    4.00    --   54.00 -37.00-120.00   89
  8  \w     47.00 109.00   1.00    4.00    --   54.00-125.00 -30.00   62
  9  \w     28.00 124.00   1.00    4.00    --   54.00  37.00 120.00   96
 10  \w      7.00  74.00   1.00    4.00    --   54.00 -37.00 150.00   67
 11  \w     39.00 100.00   1.00    4.00    --   54.00  57.00  30.00   61
 12  \w     31.00  83.00   1.00    4.00    --   54.00 -99.00 120.00   52
 13  \w     96.00 127.00   1.00    4.00    --  108.00  63.00  30.00   31
 14  \w    130.00 175.00   1.00    4.00    --  108.00 111.00 -90.00   45
 15  \w     78.00 106.00   1.00    4.00    --  108.00 -91.00  90.00   28
 16  \w     90.00 130.00   1.00    4.00    --  108.00 -50.00  90.00   40
 17  \w     38.00 106.00   1.00    4.00    --  108.00 -37.00  30.00   68
 18  \w     44.00 133.00   1.00    4.00    --  108.00 -37.00-120.00   89
 19  \w     47.00 103.00   1.00    4.00    --  108.00-111.00 -60.00   56
 20  \w     76.00 157.00   1.00    4.00    --  108.00  25.00-120.00   81
 21  \w     38.00  93.00   1.00    4.00    --  108.00-111.00 -90.00   55
 22  \w     37.00 109.00   1.00    4.00    --  108.00-111.00  60.00   72
 23  \w     50.00  87.00   1.00    4.00    --  108.00 -91.00 -60.00   37
 24  \w    117.00 144.00   1.00    4.00    --  108.00  77.00 -30.00   27
 25  \w     82.00 115.00   1.00    4.00    --  108.00  37.00 -60.00   33
 26  \w    123.00 151.00   1.00    4.00    --  108.00  37.00 -60.00   28
 27  \w     93.00 140.00   1.00    4.00    --  108.00 178.00 -30.00   47
 28  \w    104.00 135.00   1.00    4.00    --  108.00 -77.00  90.00   31
 29  \w     56.00  82.00   1.00    4.00    --  108.00 -91.00   0.00   26
 30  \w    141.00 176.00   1.00    4.00    --  108.00  63.00  30.00   35
 31  \w    106.00 154.00   1.00    4.00    --  108.00  77.00 -60.00   48
 32  \w     81.00 134.00   1.00    4.00    --  108.00 -12.00-120.00   53
 33  \w     85.00 110.00   1.00    4.00    --  108.00-120.00-152.00   25
 34  \w     37.00  62.00   1.00    4.00    --  108.00-120.00-152.00   25
 35  \w     55.00 109.00   1.00    4.00    --  108.00-111.00   0.00   54
 36  \w     49.00 106.00   1.00    4.00    --  108.00 -63.00 -30.00   57
 37  \w     88.00 147.00   1.00    4.00    --  108.00  63.00  60.00   59
 38  \w     45.00  76.00   1.00    4.00    --  108.00 -77.00  90.00   31
 39  \w    104.00 129.00   1.00    4.00    --  108.00 -12.00  30.00   25
 40  \w    110.00 136.00   1.00    4.00    --  108.00 178.00-180.00   26
 41  \w     97.00 122.00   1.00    4.00    --  108.00 -63.00  60.00   25
 42  \w     87.00 112.00   1.00    4.00    --  108.00  50.00  60.00   25
 43  \w     42.00  95.00   1.00    4.00    --  108.00 -12.00  30.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0297751000
_diffrn_orient_matrix_UB_12      -0.1417165000
_diffrn_orient_matrix_UB_13      -0.0320915000
_diffrn_orient_matrix_UB_21      -0.0168682000
_diffrn_orient_matrix_UB_22      0.0603486000
_diffrn_orient_matrix_UB_23      -0.0857066000
_diffrn_orient_matrix_UB_31      0.3933580000
_diffrn_orient_matrix_UB_32      -0.0142400000
_diffrn_orient_matrix_UB_33      -0.0109092000
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5786
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.989
_diffrn_reflns_theta_min         2.644
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.978
_exptl_absorpt_correction_T_max  0.607
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_description       needle
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2492
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0415P)^2^+0.8521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2272
_reflns_number_total             2492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01954k2.cif
_cod_data_source_block           5_3H2O
_cod_database_code               7719796
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Li2 O4 C10 H10'
_reflns_odcompleteness_completeness 98.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O7-H7A = O7-H7B = O8-H8A = O8-H8B = O9-H9A = O9-H9B
 0.82 with sigma of 0.02
 H7A-H7B = H8A-H8B = H9A-H9B
 1.35 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C4(H4)
;
_shelx_res_checksum              26839
_shelx_hkl_checksum              25067
_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 1.893
_oxdiff_exptl_absorpt_empirical_full_min 0.447