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_7713337
_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(C6 H16 N)'
_chemical_formula_sum            'C12 H32 Cd I4 N2'
_chemical_formula_weight         824.39
_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
_audit_creation_date             2022-11-12
_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                   14.3623(6)
_cell_length_b                   9.9781(6)
_cell_length_c                   17.5752(8)
_cell_measurement_reflns_used    5420
_cell_measurement_temperature    272.94(10)
_cell_measurement_theta_max      30.0900
_cell_measurement_theta_min      2.3130
_cell_volume                     2518.7(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      272.94(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     16.00  59.00   0.50    2.00    --   -6.32  69.00 160.00   86
  2  \w    -15.00  10.00   0.50    2.00    --    5.54 -99.00 -90.00   50
  3  \w    -40.00  76.00   0.50    2.00    --    5.54   0.00-150.00  232
;
_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      0.0124233000
_diffrn_orient_matrix_UB_12      0.0686742000
_diffrn_orient_matrix_UB_13      0.0023653000
_diffrn_orient_matrix_UB_21      -0.0293176000
_diffrn_orient_matrix_UB_22      0.0143220000
_diffrn_orient_matrix_UB_23      -0.0314583000
_diffrn_orient_matrix_UB_31      -0.0377429000
_diffrn_orient_matrix_UB_32      0.0115021000
_diffrn_orient_matrix_UB_33      0.0251759000
_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  0.0226
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12941
_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         1.831
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54454
_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    2.174
_exptl_crystal_description       \^a\/E?block\^a\/E?
_exptl_crystal_F_000             1512
_refine_diff_density_max         1.796
_refine_diff_density_min         -1.928
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         2350
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0764
_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^)+(0.1191P)^2^+14.6383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2348
_refine_ls_wR_factor_ref         0.2480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1855
_reflns_number_total             2350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01574b2.cif
_cod_data_source_block           zsy_220930_273k_auto
_cod_database_code               7713337
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 N1 Cd1 I1'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C3 = N1-C1 = N2-C7
 1.49 with sigma of 0.01
 C7-C5
 2.5 with sigma of 0.01
 C2-C3
 2.5 with sigma of 0.01
 N2-C6
 1.49 with sigma of 0.01
 C2-C1
 2.5 with sigma of 0.01
 C7-C6
 2.5 with sigma of 0.01
 N1-C2
 1.49 with sigma of 0.01
 C1-C1_$1
 2.5 with sigma of 0.01
 C4-N1
 2.53 with sigma of 0.01
 C3-C1
 2.5 with sigma of 0.01
 H1C-H4A_$1
 2 with sigma of 0.02
 C8-C7 = C4_$1-C3
 1.52 with sigma of 0.01
 C8-C7
 1.525 with sigma of 0.01
 C4-C3
 1.523 with sigma of 0.01
 C6_$1-C7
 2.5 with sigma of 0.01
 C6-C6_$1 = C7-C5
 2.5 with sigma of 0.01
 C6-C6_$1
 2.5 with sigma of 0.01
 C5-C6
 2.5 with sigma of 0.01
 N2-C5 = N2-C6_$1 = N2-C7 = N2-C6 = N1-C1 = N1-C2 = N1-C1_$1 = N1-C3
 1.49 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(N2) = Uanis(C5) = Uanis(C7) = Uanis(C8)
Uanis(C2) = Uanis(N1) = Uanis(C3) = Uanis(C1)
4. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
5.a Riding coordinates:
 C5(H5A,H5B,H5C), C2(H2A,H2B,H2C)
5.b Ternary CH refined with riding coordinates:
 C3(H3), C7(H7)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              44001
_shelx_hkl_checksum              34257
_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 1.483
_oxdiff_exptl_absorpt_empirical_full_min 0.708