Methyl Regulation Triggers High-Temperature Ferroelastic Phase Transition
Zhang, Si-Yue; Zhang, Zhi-Cheng; Zhang, Tie; Ni, Hao-Fei; Zhang, Zhixu; Fu, Da-Wei; Lu, Hai-Feng; Dalton Transactions  (2023) –; doi:10.1039/D3DT01574B

data_7713333
_publ_section_title
;
 Methyl Regulation Triggers High-Temperature Ferroelastic Phase Transition
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01574B
_journal_year                    2023
_chemical_formula_moiety         'Cd I4, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 Cd I4 N2'
_chemical_formula_weight         768.29
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-04-05 deposited with the CCDC.	2023-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.115(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.3120(5)
_cell_length_b                   9.6733(3)
_cell_length_c                   33.4780(12)
_cell_measurement_reflns_used    11865
_cell_measurement_temperature    229.97(10)
_cell_measurement_theta_max      30.3930
_cell_measurement_theta_min      2.1690
_cell_volume                     4311.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      229.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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    -28.00  19.00   0.50    2.80    --    5.54 -38.00   0.00   94
  2  \w    -11.00  36.00   0.50    2.80    --    5.54 -99.00 -30.00   94
  3  \w    -23.00  10.00   0.50    2.80    --    5.54 -33.00-163.00   66
  4  \w    -65.00 -31.00   0.50    2.80    --    5.54 -38.00   0.00   68
  5  \w    -10.00  37.00   0.50    2.80    --    5.54  89.00 154.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0025328000
_diffrn_orient_matrix_UB_12      -0.0070457000
_diffrn_orient_matrix_UB_13      -0.0210754000
_diffrn_orient_matrix_UB_21      0.0227207000
_diffrn_orient_matrix_UB_22      0.0658276000
_diffrn_orient_matrix_UB_23      -0.0022495000
_diffrn_orient_matrix_UB_31      0.0481151000
_diffrn_orient_matrix_UB_32      -0.0315061000
_diffrn_orient_matrix_UB_33      -0.0000033000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            25249
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.953
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.367
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_refine_diff_density_max         4.231
_refine_diff_density_min         -2.459
_refine_diff_density_rms         0.429
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         7455
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.1477
_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^)+(0.0001P)^2^+872.7260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3453
_refine_ls_wR_factor_ref         0.3478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6461
_reflns_number_total             7455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01574b2.cif
_cod_data_source_block           zsy_221017_1_230k_auto
_cod_database_code               7713333
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 I1 Cd1 N1'
_reflns_odcompleteness_completeness 96.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C13 = N4-C16 = N1-C2 = N2-C7 = N2-C5 = N2-C8 = N3-C10
 1.49 with sigma of 0.01
 N1-C3 = N1-C1 = N1-C2 = N1-C4 = N2-C6 = N2-C7 = N2-C8 = N2-C5 = N3-C9 = N3-
 C12 = N3-C10 = N3-C11 = N4-C13 = N4-C16 = N4-C15 = N4-C14
 1.49 with sigma of 0.01
 C2-C1 = C3-C4
 2.5 with sigma of 0.01
 C9-C12
 2.5 with sigma of 0.01
 C1-C4
 2.5 with sigma of 0.01
 C1-C3
 2.5 with sigma of 0.01
 H11C-H10C
 2 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C12) \\sim
Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Riding coordinates:
 C13(H13A,H13B,H13C), C4(H4A,H4B,H4C)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C),
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C),
 C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C),
  C9(H9A,H9B,H9C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              19685
_shelx_hkl_checksum              24204
_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 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.788