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_7719797
_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         'C18 H16.027 O21 Rb6'
_chemical_formula_sum            'C18 H16.03 O21 Rb6'
_chemical_formula_weight         1081.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-05-12
_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                 98.107(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   4.04600(10)
_cell_length_b                   20.0693(3)
_cell_length_c                   10.4837(2)
_cell_measurement_reflns_used    10105
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      70.4480
_cell_measurement_theta_min      4.2430
_cell_volume                     842.77(3)
_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      air
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_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    -29.00  42.00   1.00    1.00    --    0.00  77.00  30.00   71
  2  \w    -19.00  68.00   1.00    1.00    --    0.00  57.00-180.00   87
  3  \w    -21.00  29.00   1.00    1.00    --    0.00 -77.00-180.00   50
  4  \w    -14.00  73.00   1.00    1.00    --   54.00 -57.00  60.00   87
  5  \w    -18.00  92.00   1.00    1.00    --   54.00 -19.00 120.00  110
  6  \w      6.00  94.00   1.00    1.00    --   54.00 -99.00  90.00   88
  7  \w    -17.00  77.00   1.00    1.00    --   54.00 -37.00-120.00   94
  8  \w    -14.00  73.00   1.00    1.00    --   54.00 -57.00 -30.00   87
  9  \w     35.00 122.00   1.00    1.00    --   54.00  57.00   0.00   87
 10  \w    -14.00  73.00   1.00    1.00    --   54.00 -57.00-120.00   87
 11  \w    104.00 178.00   1.00    1.00    --  108.00 111.00 -60.00   74
 12  \w     39.00 137.00   1.00    1.00    --  108.00 -77.00-120.00   98
 13  \w     89.00 177.00   1.00    1.00    --  108.00  50.00 -30.00   88
 14  \w     87.00 176.00   1.00    1.00    --  108.00  63.00 -90.00   89
 15  \w     40.00 129.00   1.00    1.00    --  108.00 -63.00 -60.00   89
 16  \w     37.00 109.00   1.00    1.00    --  108.00-111.00  60.00   72
 17  \w     85.00 178.00   1.00    1.00    --  108.00  37.00  30.00   93
 18  \w    103.00 177.00   1.00    1.00    --  108.00  77.00-120.00   74
 19  \w    103.00 177.00   1.00    1.00    --  108.00  77.00 -60.00   74
 20  \w     37.00 109.00   1.00    1.00    --  108.00-111.00   0.00   72
 21  \w     36.00 138.00   1.00    1.00    --  108.00 -25.00 -90.00  102
 22  \w     37.00 108.00   1.00    1.00    --  108.00-105.00 103.00   71
 23  \w     38.00 106.00   1.00    1.00    --  108.00 -91.00-120.00   68
 24  \w     36.00 138.00   1.00    1.00    --  108.00 -25.00   0.00  102
 25  \w    104.00 178.00   1.00    1.00    --  108.00 111.00-120.00   74
 26  \w     37.00 109.00   1.00    1.00    --  108.00-111.00  90.00   72
 27  \w     61.00 146.00   1.00    1.00    --  108.00 178.00   0.00   85
 28  \w     37.00 109.00   1.00    1.00    --  108.00-111.00-180.00   72
 29  \w    104.00 178.00   1.00    1.00    --  108.00 111.00 -30.00   74
 30  \w     38.00 106.00   1.00    1.00    --  108.00 -91.00 -90.00   68
 31  \w     40.00 129.00   1.00    1.00    --  108.00 -63.00  60.00   89
 32  \w     37.00 131.00   1.00    1.00    --  108.00 -37.00-120.00   94
 33  \w    -38.00  72.00   1.00    1.00    --    0.00  19.00 120.00  110
 34  \w    -68.00  19.00   1.00    1.00    --    0.00 -57.00-150.00   87
 35  \w     35.00 122.00   1.00    1.00    --   54.00  57.00-180.00   87
 36  \w     35.00 122.00   1.00    1.00    --   54.00  57.00  60.00   87
 37  \w     35.00 122.00   1.00    1.00    --   54.00  57.00 -60.00   87
 38  \w     35.00 122.00   1.00    1.00    --   54.00  57.00 150.00   87
 39  \w     35.00 122.00   1.00    1.00    --   54.00  57.00 120.00   87
 40  \w     35.00 122.00   1.00    1.00    --   54.00  57.00-120.00   87
 41  \w     87.00 176.00   1.00    1.00    --  108.00  63.00 -60.00   89
 42  \w     85.00 178.00   1.00    1.00    --  108.00  37.00 150.00   93
 43  \w     89.00 177.00   1.00    1.00    --  108.00  50.00  60.00   88
 44  \w     85.00 178.00   1.00    1.00    --  108.00  37.00-120.00   93
 45  \w     78.00 178.00   1.00    1.00    --  108.00  25.00-150.00  100
 46  \w     85.00 165.00   1.00    1.00    --  108.00  37.00 -90.00   80
 47  \w     78.00 178.00   1.00    1.00    --  108.00  25.00 120.00  100
;
_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      0.1231673000
_diffrn_orient_matrix_UB_12      -0.0669733000
_diffrn_orient_matrix_UB_13      0.0608581000
_diffrn_orient_matrix_UB_21      0.0212911000
_diffrn_orient_matrix_UB_22      0.0311318000
_diffrn_orient_matrix_UB_23      0.1352310000
_diffrn_orient_matrix_UB_31      -0.3637458000
_diffrn_orient_matrix_UB_32      -0.0208971000
_diffrn_orient_matrix_UB_33      0.0064232000
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15648
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.354
_diffrn_reflns_theta_min         4.797
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.487
_exptl_absorpt_correction_T_max  0.502
_exptl_absorpt_correction_T_min  0.333
_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    2.130
_exptl_crystal_description       plate
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 1473 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3171
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0720P)^2^+1.4296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3150
_reflns_number_total             3171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01954k2.cif
_cod_data_source_block           4_5H2O
_cod_database_code               7719797
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Rb3 O6 C9 H9'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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. Restrained distances
 Rb2-H7A \\sim Rb2-H7B
 with sigma of 0.02
 Rb1-H9A \\sim Rb1-H9B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O10 \\sim O10A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.002 within 2A
4. Rigid body (RIGU) restrains
 O10, O10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O10A)=Sof(H10A)=Sof(H10B)=1-FVAR(1)
 Sof(O10)=FVAR(1)
 Fixed Sof: O11(0.5)
6.a Free rotating group:
 O7(H7A,H7B), O9(H9A,H9B)
6.b Rotating group:
 O10A(H10A,H10B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6)
;
_shelx_res_checksum              2365
_shelx_hkl_checksum              59328
_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 3.411
_oxdiff_exptl_absorpt_empirical_full_min 0.470