Targeted regulation and optimization of multifunctional phase transition materials by novel void occupancy engineering.
Wang, Zhi-Jie; Ni, Hao-Fei; Zhang, Tie; Li, Jie; Lun, Meng-Meng; Fu, Da-Wei; Zhang, Zhi-Xu; Zhang, Yi; Chemical science 14 (2023) 9041–9047; doi:10.1039/d3sc02652c

data_1569603
_publ_section_title
;
 Targeted regulation and optimization of multifunctional phase transition
 materials by novel void occupancy engineering.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              9041
_journal_page_last               9047
_journal_paper_doi               10.1039/d3sc02652c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C3 Cd N3 S3, C5 H14 N'
_chemical_formula_sum            'C8 H14 Cd N4 S3'
_chemical_formula_weight         374.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-05-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-05-24 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.634(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3109(7)
_cell_length_b                   10.7164(6)
_cell_length_c                   14.9364(11)
_cell_measurement_reflns_used    2506
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.4890
_cell_measurement_theta_min      2.3770
_cell_volume                     1490.25(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.966
_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     14.00  39.00   0.50    0.60    --   20.00  54.00 -90.00   50
  2  \w     70.00  98.00   0.50    0.60    --   20.00  54.00 -90.00   56
  3  \w    -50.00 -24.00   0.50    0.60    --   20.00  54.00   0.00   52
  4  \w    -74.00 108.00   0.50    0.60    --   20.00  54.00  60.00  364
  5  \w    -74.00  45.00   0.50    0.60    --   20.00  54.00-180.00  238
  6  \w    -74.00   5.00   0.50    0.60    --   20.00  54.00 -60.00  158
  7  \w     82.00 107.00   0.50    0.60    --   20.00  54.00 -60.00   50
  8  \w    -13.00  21.00   0.50    0.60    --   20.00  54.00 -30.00   68
  9  \w     46.00  71.00   0.50    0.60    --   20.00  54.00 -30.00   50
 10  \w     82.00 107.00   0.50    0.60    --   20.00  54.00 -30.00   50
 11  \w    -25.00   0.00   0.50    0.60    --   20.00  54.00 -90.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0693301000
_diffrn_orient_matrix_UB_12      -0.0117047000
_diffrn_orient_matrix_UB_13      -0.0173389000
_diffrn_orient_matrix_UB_21      -0.0239694000
_diffrn_orient_matrix_UB_22      0.0193871000
_diffrn_orient_matrix_UB_23      -0.0430555000
_diffrn_orient_matrix_UB_31      0.0205339000
_diffrn_orient_matrix_UB_32      0.0621789000
_diffrn_orient_matrix_UB_33      0.0101173000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13750
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.892
_diffrn_reflns_theta_min         2.339
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       rod-shaped
_exptl_crystal_F_000             744
_refine_diff_density_max         2.104
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         4142
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0784
_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^)+(0.1457P)^2^+1.8915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2333
_refine_ls_wR_factor_ref         0.2818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2193
_reflns_number_total             4142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02652c2.cif
_cod_data_source_block           TMEA_Cd_293K
_cod_depositor_comments
'Adding full bibliography for 1569598--1569604.cif.'
_cod_database_code               1569603
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C3
 1.48 with sigma of 0.01
 H1B-H4B
 2.45 with sigma of 0.01
 N1-C2 = N1-C3 = N1-C5 = N1-C4
 1.47 with sigma of 0.01
 C2-C1
 1.54 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C5) = Uanis(C4) = Uanis(N1)
4.a Riding coordinates:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              34344
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.829