Organic cation conformational flexibility governs mechanical response in organic-inorganic hybrid materials.
Yang, Ya-Wen; Xu, Ke; Zhou, Zi-Ning; Jin, Ming-Liang; Tsunashima, Ryo; Nakamura, Takayoshi; Chai, Chao-Yang; Ye, Qiong; Chemical science  (2025) –; doi:10.1039/d5sc06333g

data_1576305
_publ_section_title
;
 Organic cation conformational flexibility governs mechanical response in
 organic-inorganic hybrid materials.
;
_journal_name_full               'Chemical science'
_journal_paper_doi               10.1039/d5sc06333g
_journal_year                    2025
_chemical_formula_moiety         'C12 H28 I6 N2 O2 Pb2'
_chemical_formula_sum            'C12 H28 I6 N2 O2 Pb2'
_chemical_formula_weight         1408.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-02-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-07-28 deposited with the CCDC.	2025-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2468(6)
_cell_length_b                   8.8197(8)
_cell_length_c                   20.448(2)
_cell_measurement_reflns_used    1602
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.7560
_cell_measurement_theta_min      2.4930
_cell_volume                     1487.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     74.00 107.00   0.50    1.50    --   20.00  54.00   0.00   66
  2  \w    -74.00  -8.00   0.50    1.50    --   20.00  54.00  90.00  132
  3  \w      8.00  73.00   0.50    1.50    --   20.00  54.00  90.00  130
  4  \w    -33.00  22.00   0.50    1.50    --   20.00  54.00  60.00  110
  5  \w    -71.00 -39.00   0.50    1.50    --   20.00  54.00 -60.00   64
  6  \w    -10.00  32.00   0.50    1.50    --   20.00  54.00 -60.00   84
  7  \w    -74.00  23.00   0.50    1.50    --   20.00  54.00   0.00  194
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0428177000
_diffrn_orient_matrix_UB_12      0.0006925000
_diffrn_orient_matrix_UB_13      -0.0300914000
_diffrn_orient_matrix_UB_21      0.0738885000
_diffrn_orient_matrix_UB_22      0.0109416000
_diffrn_orient_matrix_UB_23      -0.0170891000
_diffrn_orient_matrix_UB_31      0.0098279000
_diffrn_orient_matrix_UB_32      -0.0796843000
_diffrn_orient_matrix_UB_33      -0.0025754000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6852
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.011
_diffrn_reflns_theta_max         25.011
_diffrn_reflns_theta_min         1.992
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.541
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.295
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1399
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0543P)^2^+7.6931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                938
_reflns_number_total             1399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06333g9.cif
_cod_data_source_block           2-rac
_cod_database_code               1576305
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.273
_shelx_estimated_absorpt_t_min   0.209
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1-C1
 1.43 with sigma of 0.01
 N1-C2 = N1-C6
 1.47 with sigma of 0.01
 C1-C2 = C3-C2 = C3-C4 = C5-C4 = C5-C6
 1.54 with sigma of 0.01
 C2-O1
 2.426 with sigma of 0.02
 C1-C3 = C2-C4 = C3-C5 = C4-C6
 2.515 with sigma of 0.02
 N1-C1 = N1-C3 = N1-C5
 2.458 with sigma of 0.02
 C6-C2
 2.401 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4 \\sim C3 \\sim C2 \\sim C5 \\sim C1 \\sim N1 \\sim C6 \\sim O1: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Fixed Sof: C3(0.5) H3A(0.5) H3B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C4(0.5)
 H4A(0.5) H4B(0.5) C6(0.5) H6A(0.5) H6B(0.5) C1(0.5) H1A(0.5) H1B(0.5) C2(0.5)
 H2(0.5) N1(0.5) H1C(0.5) H1D(0.5) O1(0.5) H1(0.5)
5.a Riding coordinates:
 O1(H1)
5.b Ternary CH refined with riding coordinates:
 C2(H2)
5.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C4(H4A,H4B), C6(H6A,H6B), C1(H1A,H1B), N1(H1C,H1D)
;
_shelx_res_checksum              96030
_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 2.184
_oxdiff_exptl_absorpt_empirical_full_min 0.510