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_1569598
_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         'C6 H16 N, C3 Cd N3 S3'
_chemical_formula_sum            'C9 H16 Cd N4 S3'
_chemical_formula_weight         388.84
_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             2023-02-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7498(7)
_cell_length_b                   9.0463(8)
_cell_length_c                   16.0214(13)
_cell_measurement_reflns_used    5722
_cell_measurement_temperature    298.45(10)
_cell_measurement_theta_max      29.2720
_cell_measurement_theta_min      2.2860
_cell_volume                     1558.0(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      air
_diffrn_ambient_temperature      298.45(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.836
_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     -8.00  17.00   0.50    0.28    --    4.71-102.00 -23.00   50
  2  \w    -17.00   8.00   0.50    0.28    --    4.71 -99.00  30.00   50
  3  \w    -78.00 -47.00   0.50    0.28    --   -5.49 -26.00  93.00   62
  4  \w    -18.00   7.00   0.50    0.28    --   -5.49 -26.00  93.00   50
  5  \w     -8.00  77.00   0.50    0.28    --    4.71  38.00  60.00  170
  6  \w    -45.00 -20.00   0.50    0.28    --   -5.49 115.00 -27.63   50
;
_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      0.0659389000
_diffrn_orient_matrix_UB_12      0.0191895000
_diffrn_orient_matrix_UB_13      -0.0220149000
_diffrn_orient_matrix_UB_21      0.0358396000
_diffrn_orient_matrix_UB_22      -0.0391910000
_diffrn_orient_matrix_UB_23      0.0010960000
_diffrn_orient_matrix_UB_31      -0.0226686000
_diffrn_orient_matrix_UB_32      -0.0074805000
_diffrn_orient_matrix_UB_33      -0.0622016000
_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  0.1100
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11416
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.921
_diffrn_reflns_theta_min         2.282
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77719
_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_colour            colorless
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             776
_refine_diff_density_max         0.697
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.0056(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         2178
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0854
_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^)+(0.1384P)^2^+6.7409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2717
_refine_ls_wR_factor_ref         0.2832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1540
_reflns_number_total             2178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02652c2.cif
_cod_data_source_block           DEDMA_Cd_298K
_cod_depositor_comments
'Adding full bibliography for 1569598--1569604.cif.'
_cod_database_code               1569598
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.89
_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
 C1-C3
 2.2 with sigma of 0.01
 C1-N1
 1.5 with sigma of 0.01
 C1-N1 \\sim C1A-N1
 with sigma of 0.02
3. Rigid bond restraints
 C1, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C1, N1, C5, C1A, C4, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3 \\sim C1 \\sim N1 \\sim C5 \\sim C1A \\sim C4 \\sim C2: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C4) = Uanis(C5) = Uanis(C3) = Uanis(C2)
Uanis(C1) = Uanis(C1A)
Uanis(N1) = Uanis(N3)
Uanis(N1) = Uanis(N2) = Uanis(N3)
5. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(1)
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5) H3A(0.5) H3B(0.5) H4A(0.5) H4B(0.5)
 H4C(0.5) H5A(0.5) H5B(0.5)
6.a Riding coordinates:
 C4(H4A,H4B,H4C)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C1A(H1AA,H1AB,H1AC)
;
_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 1.662
_oxdiff_exptl_absorpt_empirical_full_min 0.664