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_7713335
_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, C8 N2'
_chemical_formula_sum            'C8 Cd I4 N2'
_chemical_formula_weight         744.10
_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_primary     dual
_audit_creation_date             2022-10-28
_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                   13.3771(7)
_cell_length_b                   9.7035(6)
_cell_length_c                   16.8488(12)
_cell_measurement_reflns_used    4782
_cell_measurement_temperature    273.00(10)
_cell_measurement_theta_max      30.4600
_cell_measurement_theta_min      2.4190
_cell_volume                     2187.1(2)
_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      273.00(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 1.000
_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    -34.00  36.00   0.50    2.50    --   -5.57  89.00 154.00  140
  2  \w     15.00  48.00   0.50    2.50    --    4.87  38.00 -60.00   66
  3  \w     -3.00  72.00   0.50    2.50    --    4.87  38.00-180.00  150
;
_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      -0.0021574000
_diffrn_orient_matrix_UB_12      -0.0072835000
_diffrn_orient_matrix_UB_13      -0.0418482000
_diffrn_orient_matrix_UB_21      0.0225657000
_diffrn_orient_matrix_UB_22      0.0656872000
_diffrn_orient_matrix_UB_23      -0.0044783000
_diffrn_orient_matrix_UB_31      0.0479388000
_diffrn_orient_matrix_UB_32      -0.0312571000
_diffrn_orient_matrix_UB_33      0.0002521000
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.944
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82909
_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    2.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_refine_diff_density_max         2.207
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         2044
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0794P)^2^+11.4086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1602
_reflns_number_total             2044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01574b2.cif
_cod_data_source_block           zsy_221017_1_273k_auto
_cod_database_code               7713335
_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. Restrained distances
 N2-C6
 1.49 with sigma of 0.01
 N2-C9 = N1-C1 = N1-C4
 1.49 with sigma of 0.01
 C6-C9
 2.5 with sigma of 0.01
 C4-C2
 2.5 with sigma of 0.01
 C2-C1
 2.5 with sigma of 0.01
 C9-C7
 2.5 with sigma of 0.01
 N2-C7
 1.49 with sigma of 0.01
 N1-C2
 1.49 with sigma of 0.01
 C4-C4_$1
 2.5 with sigma of 0.01
 C7-C6
 2.5 with sigma of 0.01
 C9-N2
 1.49 with sigma of 0.01
 C8-C7
 1.35 with sigma of 0.01
 N2-C8
 1.51 with sigma of 0.01
 N1-C3
 1.584 with sigma of 0.02
 C9-C8
 1.63 with sigma of 0.01
 C3-C4
 1.865 with sigma of 0.02
 C3-C2
 1.217 with sigma of 0.02
 C5-C4
 1.4 with sigma of 0.01
 N1-C5
 1.5 with sigma of 0.01
 C1-C5
 2.5 with sigma of 0.01
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C5) \\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
Uanis(N1) = Uanis(C4) = Uanis(C5) = Uanis(C2) = Uanis(C3)
4. Others
 Fixed Sof: C9(0.5) C4(0.5) C2(0.25) C7(0.5) C8(0.5) C3(0.5) C5(0.25)
;
_shelx_res_checksum              21318
_shelx_hkl_checksum              90656
_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 1.291
_oxdiff_exptl_absorpt_empirical_full_min 0.829