#------------------------------------------------------------------------------
#$Date: 2023-09-05 22:22:09 +0300 (Tue, 05 Sep 2023) $
#$Revision: 286072 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/95/1569598.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1569598
loop_
_publ_author_name
'Wang, Zhi-Jie'
'Ni, Hao-Fei'
'Zhang, Tie'
'Li, Jie'
'Lun, Meng-Meng'
'Fu, Da-Wei'
'Zhang, Zhi-Xu'
'Zhang, Yi'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -8.00  17.00   0.50    0.28    --    4.71-102.00 -23.00   50
  2  ω    -17.00   8.00   0.50    0.28    --    4.71 -99.00  30.00   50
  3  ω    -78.00 -47.00   0.50    0.28    --   -5.49 -26.00  93.00   62
  4  ω    -18.00   7.00   0.50    0.28    --   -5.49 -26.00  93.00   50
  5  ω     -8.00  77.00   0.50    0.28    --    4.71  38.00  60.00  170
  6  ω    -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       'ω 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.1384P)²+6.7409P] where P=(Fo²+2Fc²)/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 > 2σ(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
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2978(13) 0.9159(6) 0.6012(8) 0.131(3) Uani 0.485(12) 1 d D U P A 1
H1A H 0.299699 0.959582 0.546632 0.196 Uiso 0.485(12) 1 calc R U P A 1
H1B H 0.366278 0.952644 0.633600 0.196 Uiso 0.485(12) 1 calc R U P A 1
H1C H 0.220980 0.941099 0.628338 0.196 Uiso 0.485(12) 1 calc R U P A 1
C2 C 0.5214(12) 0.750000 0.5375(10) 0.138(3) Uani 1 2 d S TU P . .
H2A H 0.544208 0.695235 0.586520 0.207 Uiso 0.5 1 calc R U P B -1
H2B H 0.550558 0.849897 0.542588 0.207 Uiso 0.5 1 calc R U P B -1
H2C H 0.558263 0.704868 0.489279 0.207 Uiso 0.5 1 calc R U P B -1
C3 C 0.3998(10) 0.750000 0.5296(7) 0.138(3) Uani 1 2 d DS TU P A .
H3A H 0.381033 0.664408 0.495405 0.166 Uiso 0.5 1 calc R U P . .
H3B H 0.381033 0.835592 0.495405 0.166 Uiso 0.5 1 calc R U P . .
C4 C 0.0768(11) 0.750000 0.6315(11) 0.138(3) Uani 1 2 d S TU P . .
H4A H 0.003623 0.730220 0.598985 0.207 Uiso 0.5 1 d R U P C -1
H4B H 0.068933 0.844830 0.657875 0.207 Uiso 0.5 1 d R U P C -1
H4C H 0.086153 0.674960 0.673365 0.207 Uiso 0.5 1 d R U P C -1
C5 C 0.1829(11) 0.750000 0.5788(10) 0.138(3) Uani 1 2 d S TU P A .
H5A H 0.170406 0.664704 0.543051 0.166 Uiso 0.5 1 calc R U P . .
H5B H 0.170406 0.835296 0.543052 0.166 Uiso 0.5 1 calc R U P . .
N1 N 0.3077(6) 0.750000 0.5936(5) 0.0776(12) Uani 1 2 d DS TU P . .
C6 C 0.6686(5) 0.4407(7) 0.6868(4) 0.0582(14) Uani 1 1 d . . . . .
C7 C 0.2100(7) 0.250000 0.6305(5) 0.068(3) Uani 1 2 d S T P . .
Cd1 Cd 0.43767(5) 0.250000 0.77689(4) 0.0628(2) Uani 1 2 d S T P . .
N2 N 0.5709(4) 0.4247(10) 0.7115(3) 0.0776(12) Uani 1 1 d . . . . .
N3 N 0.3050(7) 0.250000 0.6666(6) 0.0776(12) Uani 1 2 d S T P . .
S1 S 0.80563(13) 0.4739(3) 0.64720(12) 0.0820(6) Uani 1 1 d . . . . .
S2 S 0.0784(2) 0.250000 0.58325(16) 0.0911(11) Uani 1 2 d S T P . .
C1A C 0.3496(18) 0.811(2) 0.6755(8) 0.131(3) Uani 0.515(12) 1 d D U P A 2
H1AA H 0.342877 0.916351 0.674800 0.196 Uiso 0.515(12) 1 calc R U P A 2
H1AB H 0.434583 0.782862 0.685153 0.196 Uiso 0.515(12) 1 calc R U P A 2
H1AC H 0.298228 0.771362 0.719239 0.196 Uiso 0.515(12) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
C2 C3 H3A 105.2 . . ?
C2 C3 H3B 105.2 . . ?
C2 C3 N1 128.5(12) . . ?
H3A C3 H3B 105.9 . . ?
N1 C3 H3A 105.2 . . ?
N1 C3 H3B 105.2 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C4 H4A 109.6 . . ?
C5 C4 H4B 109.4 . . ?
C5 C4 H4C 109.4 . . ?
C4 C5 H5A 103.9 . . ?
C4 C5 H5B 103.9 . . ?
H5A C5 H5B 105.4 . . ?
N1 C5 C4 133.5(14) . . ?
N1 C5 H5A 103.9 . . ?
N1 C5 H5B 103.9 . . ?
C1 N1 C1 167.6(11) . 7_575 ?
C3 N1 C1 96.2(5) . 7_575 ?
C3 N1 C1 96.2(5) . . ?
C3 N1 C1A 115.0(10) . 7_575 ?
C3 N1 C1A 115.0(10) . . ?
C5 N1 C1 86.8(6) . 7_575 ?
C5 N1 C1 86.8(6) . . ?
C5 N1 C3 124.0(10) . . ?
C5 N1 C1A 116.8(11) . . ?
C5 N1 C1A 116.8(11) . 7_575 ?
N2 C6 S1 175.9(7) . . ?
N3 C7 S2 178.6(8) . . ?
N2 Cd1 N2 83.4(4) 7_565 . ?
N2 Cd1 S1 90.92(19) 7_565 4_456 ?
N2 Cd1 S1 90.92(18) . 6_557 ?
N2 Cd1 S1 173.58(17) . 4_456 ?
N2 Cd1 S1 173.58(17) 7_565 6_557 ?
N2 Cd1 S2 91.59(13) . 6_657 ?
N2 Cd1 S2 91.59(13) 7_565 6_657 ?
N3 Cd1 N2 92.1(2) . . ?
N3 Cd1 N2 92.1(2) . 7_565 ?
N3 Cd1 S1 91.13(14) . 6_557 ?
N3 Cd1 S1 91.13(14) . 4_456 ?
N3 Cd1 S2 175.1(2) . 6_657 ?
S1 Cd1 S1 94.58(9) 4_456 6_557 ?
S2 Cd1 S1 85.55(5) 6_657 6_557 ?
S2 Cd1 S1 85.55(5) 6_657 4_456 ?
C6 N2 Cd1 143.0(7) . . ?
C7 N3 Cd1 158.5(7) . . ?
C6 S1 Cd1 99.1(2) . 6_657 ?
C7 S2 Cd1 95.9(3) . 6_557 ?
N1 C1A H1AA 109.5 . . ?
N1 C1A H1AB 109.5 . . ?
N1 C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 N1 1.510(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 C3 1.313(16) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 N1 1.425(12) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9601 . ?
C4 H4C 0.9598 . ?
C4 C5 1.420(18) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 N1 1.362(13) . ?
N1 C1A 1.491(13) . ?
N1 C1A 1.491(13) 7_575 ?
C6 N2 1.131(7) . ?
C6 S1 1.632(5) . ?
C7 N3 1.174(11) . ?
C7 S2 1.603(8) . ?
Cd1 N2 2.376(7) 7_565 ?
Cd1 N2 2.376(7) . ?
Cd1 N3 2.271(8) . ?
Cd1 S1 2.756(2) 4_456 ?
Cd1 S1 2.756(2) 6_557 ?
Cd1 S2 2.704(3) 6_657 ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C3 N1 C1 -89.7(6) . . . 7_575 ?
C2 C3 N1 C1 89.7(6) . . . . ?
C2 C3 N1 C5 180.000(3) . . . . ?
C2 C3 N1 C1A 23.9(9) . . . . ?
C2 C3 N1 C1A -23.9(9) . . . 7_575 ?
C4 C5 N1 C1 -84.7(6) . . . . ?
C4 C5 N1 C1 84.7(6) . . . 7_575 ?
C4 C5 N1 C3 180.000(3) . . . . ?
C4 C5 N1 C1A -24.3(9) . . . . ?
C4 C5 N1 C1A 24.3(9) . . . 7_575 ?
