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_7713338
_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         '0.5(Cd2 I8), 2(C5 N)'
_chemical_formula_sum            'C10 Cd I4 N2'
_chemical_formula_weight         768.12
_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     direct
_audit_creation_date             2023-04-23
_audit_creation_method
;FinalCif V118 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-05-05 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                   14.196(7)
_cell_length_b                   9.791(5)
_cell_length_c                   17.224(10)
_cell_measurement_reflns_used    2280
_cell_measurement_temperature    273.00
_cell_measurement_theta_max      16.93
_cell_measurement_theta_min      2.37
_cell_volume                     2394(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1972
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.288
_diffrn_reflns_theta_min         1.859
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.057
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6593
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0942 before and 0.0704 after correction.
The Ratio of minimum to maximum transmission is 0.8847.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2309
_refine_ls_number_restraints     396
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1469P)^2^+0.4362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                880
_reflns_number_total             2309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01574b2.cif
_cod_data_source_block           mo_zsy_2_273k_0m_a
_cod_database_code               7713338
_olex2_refinement_description
;
1. Restrained distances
 N1-C2 = N1-C5 = N1-C6
 1.5 with sigma of 0.01
 N006-C9 = N006-C1
 1.5 with sigma of 0.01
 C11-C6
 1.54 with sigma of 0.01
 N006-C3
 1.5 with sigma of 0.01
 C4-C1
 1.54 with sigma of 0.01
 C11-N1
 2.5 with sigma of 0.02
 C11-C11_$1
 2.5 with sigma of 0.02
 C1-C9
 2.5 with sigma of 0.02
 C4-N006
 2.5 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 5.5A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 5.5A
3. Rigid body (RIGU) restrains
 N1, C2, C5, C6, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: I004(0.5) C4(0.5) C11(0.5) I2(0.5) I1(0.5) I4(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.676
_shelx_estimated_absorpt_t_max   0.713
_shelx_res_checksum              4270
_shelx_hkl_checksum              69271