Tunable mechanics and energetics in structurally diverse TNPG-based metal organic networks.
Karak, Shayan; Khata, Soubhik; Ahmad, Shamim; Yadav, Abhishek Kumar; AlMasoud, Najla; Alomar, Taghrid S.; Dharavath, Srinivas; Reddy, C. Malla; Banerjee, Rahul; Chemical science 16 (2025) 21508–21517; doi:10.1039/d5sc04870b

data_1575879
_publ_section_title
;
 Tunable mechanics and energetics in structurally diverse TNPG-based metal
 organic networks.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              21508
_journal_page_last               21517
_journal_paper_doi               10.1039/d5sc04870b
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C6 K0.99 Li2 N3 O9, H2 O'
_chemical_formula_sum            'C6 H2 K0.99 Li2 N3 O10'
_chemical_formula_weight         328.684
_chemical_name_systematic        'Mixed MOF'
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-07 deposited with the CCDC.	2025-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.218(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1937(2)
_cell_length_b                   12.6249(2)
_cell_length_c                   6.7246(1)
_cell_measurement_reflns_used    5744
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.9740
_cell_measurement_theta_min      3.4230
_cell_volume                     1032.41(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9894
_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  -9.00   0.50    0.76    --  -82.50  96.00-120.00  142
  2  \w    -48.00  27.00   0.50    0.20    --  -40.58  43.00   0.00  150
  3  \w    -26.00  32.00   0.50    0.20    --  -40.58  18.00 175.00  116
  4  \w     18.00  78.00   0.50    0.20    --   40.58-104.00  60.00  120
  5  \w     33.00 109.00   0.50    0.76    --   96.67-117.00 -90.00  152
  6  \w     33.00 109.00   0.50    0.76    --   96.67-117.00-120.00  152
  7  \w     41.00 100.00   0.50    0.20    --   40.58-139.00-180.00  118
  8  \w     27.00 127.00   0.50    0.76    --   96.67 -87.00-120.00  200
  9  \w     29.00  83.00   0.50    0.76    --   96.67 -68.00 -90.00  108
 10  \w     30.00  57.00   0.50    0.76    --   96.67 -50.00 -90.00   54
 11  \w     30.00  57.00   0.50    0.76    --   96.67 -50.00-180.00   54
 12  \w     29.00  68.00   0.50    0.76    --   96.67 -59.00 -30.00   78
 13  \w     30.00  57.00   0.50    0.76    --   96.67 -50.00   0.00   54
 14  \w     30.00  57.00   0.50    0.76    --   96.67 -50.00  30.00   54
 15  \w     29.00  68.00   0.50    0.76    --   96.67 -59.00  90.00   78
 16  \w     30.00  57.00   0.50    0.76    --   96.67 -50.00 120.00   54
 17  \w     30.00  57.00   0.50    0.76    --   96.67 -50.00 -60.00   54
 18  \w     30.00  57.00   0.50    0.76    --   96.67 -50.00-150.00   54
 19  \w    -32.00  26.00   0.50    0.20    --   40.58 -18.00   7.00  116
 20  \w    -31.00  28.00   0.50    0.20    --   40.58 -21.00-120.00  118
 21  \w    -27.00  37.00   0.50    0.20    --   40.58 -32.00 150.00  128
 22  \w     99.00 161.00   0.50    0.76    --   96.67 117.00-150.00  124
 23  \w    105.00 170.00   0.50    0.76    --   96.67  96.00-120.00  130
 24  \w     70.00 165.00   0.50    0.76    --   96.67  77.00 -90.00  190
 25  \w     83.00 164.00   0.50    0.76    --   96.67  33.00-150.00  162
 26  \w     83.00 164.00   0.50    0.76    --   96.67  33.00-150.00  162
 27  \w     83.00 164.00   0.50    0.76    --   96.67  33.00-180.00  162
 28  \w     83.00 164.00   0.50    0.76    --   96.67  33.00  90.00  162
 29  \w     72.00 170.00   0.50    0.76    --   96.67  18.00 175.00  196
 30  \w     16.00 114.00   0.50    0.20    --   40.58  18.00 175.00  196
 31  \w     16.00 114.00   0.50    0.20    --   40.58  18.00 175.00  196
 32  \w   -113.00 -17.00   0.50    0.20    --  -40.58 -18.00   7.00  192
 33  \w   -109.00 -14.00   0.50    0.20    --  -40.58 -77.00-180.00  190
 34  \w   -109.00 -14.00   0.50    0.20    --  -40.58 -77.00-120.00  190
 35  \w   -109.00 -17.00   0.50    0.20    --  -40.58 -66.00 -90.00  184
 36  \w   -109.00 -14.00   0.50    0.20    --  -40.58 -77.00 -30.00  190
 37  \w   -109.00 -17.00   0.50    0.20    --  -40.58 -66.00   0.00  184
 38  \w   -109.00 -14.00   0.50    0.20    --  -40.58 -77.00  90.00  190
 39  \w   -155.00 -59.00   0.50    0.76    --  -82.50 -18.00   7.00  192
 40  \w   -155.00 -59.00   0.50    0.76    --  -82.50 -18.00   7.00  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1263510000
_diffrn_orient_matrix_UB_12      -0.0010720000
_diffrn_orient_matrix_UB_13      -0.0352501000
_diffrn_orient_matrix_UB_21      0.0095807000
_diffrn_orient_matrix_UB_22      0.0288194000
_diffrn_orient_matrix_UB_23      -0.2207678000
_diffrn_orient_matrix_UB_31      0.0037045000
_diffrn_orient_matrix_UB_32      -0.1184377000
_diffrn_orient_matrix_UB_33      -0.0531862000
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.9973
_diffrn_reflns_Laue_measured_fraction_max 0.9894
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9723
_diffrn_reflns_point_group_measured_fraction_full 0.9973
_diffrn_reflns_point_group_measured_fraction_max 0.9894
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         68.20
_diffrn_reflns_theta_min         3.63
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.119a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_description       plate
_exptl_crystal_F_000             659.971
_exptl_crystal_preparation       Metallation
_exptl_crystal_recrystallization_method Evaporation
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.7548
_refine_diff_density_min         -0.5221
_refine_diff_density_rms         0.0839
_refine_ls_d_res_high            0.8303
_refine_ls_d_res_low             12.1607
_refine_ls_goodness_of_fit_ref   1.0441
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     210
_refine_ls_number_reflns         1863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0441
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+0.6724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                1654
_reflns_number_total             1863
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5sc04870b2.cif
_cod_data_source_block           RB_SK_LiK-TNPG_auto
_cod_depositor_comments
'Adding full bibliography for 1575876--1575880.cif.'
_cod_database_code               1575879
_chemical_oxdiff_formula         'C H O N Li Na K'
_chemical_oxdiff_usercomment     LT
_olex2_refinement_description
;
1.a Rotating group:
 O1(H1b,H1a)
;
_olex2_exptl_crystal_mounting_method 1
_olex2_submission_original_sample_id RB_SK_LNKTNPG
_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 1.423
_oxdiff_exptl_absorpt_empirical_full_min 0.745