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_7713332
_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(C5 H14 N)'
_chemical_formula_sum            'C10 H28 Cd I4 N2'
_chemical_formula_weight         796.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-02
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5264(2)
_cell_length_b                   14.3056(4)
_cell_length_c                   16.5364(4)
_cell_measurement_reflns_used    10720
_cell_measurement_temperature    184.99(10)
_cell_measurement_theta_max      31.0650
_cell_measurement_theta_min      2.4480
_cell_volume                     2253.59(10)
_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      184.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.838
_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   7.00   0.50    2.00    --   -6.32 -38.00  30.00  162
  2  \w    -29.00  -3.00   0.50    2.00    --    5.54 -44.00  87.00   52
  3  \w     -4.00  26.00   0.50    2.00    --    5.54 -99.00  30.00   60
  4  \w    -17.00  20.00   0.50    2.00    --    5.54 -99.00-180.00   74
;
_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      0.0388258000
_diffrn_orient_matrix_UB_12      -0.0339967000
_diffrn_orient_matrix_UB_13      -0.0217886000
_diffrn_orient_matrix_UB_21      -0.0119363000
_diffrn_orient_matrix_UB_22      0.0250370000
_diffrn_orient_matrix_UB_23      -0.0363691000
_diffrn_orient_matrix_UB_31      0.0624260000
_diffrn_orient_matrix_UB_32      0.0259475000
_diffrn_orient_matrix_UB_33      0.0065709000
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13324
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.747
_diffrn_reflns_theta_min         1.882
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.438
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56657
_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    2.347
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         5431
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0391P)^2^+1.4638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.687
_reflns_number_gt                5004
_reflns_number_total             5431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01574b2.cif
_cod_data_source_block           zsy_221007_1_185k_auto
_cod_original_cell_volume        2253.60(10)
_cod_database_code               7713332
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 N1 I1 Cd1'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.77(5)
 0.23(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-C4 = N1-C1 = N1-C2 = N1-C3 = N2-C7 = N2-C6 = N2-C9 = N2-C8
 1.49 with sigma of 0.01
 C1-C2 = C4-C3 = C6-C7 = C9-C8
 2.5 with sigma of 0.01
 C1-C4 = C2-C3 = C7-C8 = C6-C9
 2.5 with sigma of 0.01
 C5-C4 = C10-C9
 1.51 with sigma of 0.01
 C10-N2 = C5-N1
 2.53 with sigma of 0.01
4. 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
5. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
6.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C4(H4A,H4B)
6.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C10(H10A,
 H10B,H10C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              73305
_shelx_hkl_checksum              52838
_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 1.819
_oxdiff_exptl_absorpt_empirical_full_min 0.745