#------------------------------------------------------------------------------
#$Date: 2023-07-01 01:50:55 +0300 (Sat, 01 Jul 2023) $
#$Revision: 284731 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/33/7713337.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_7713337
loop_
_publ_author_name
'Zhang, Si-Yue'
'Zhang, Zhi-Cheng'
'Zhang, Tie'
'Ni, Hao-Fei'
'Zhang, Zhixu'
'Fu, Da-Wei'
'Lu, Hai-Feng'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     16.00  59.00   0.50    2.00    --   -6.32  69.00 160.00   86
  2  ω    -15.00  10.00   0.50    2.00    --    5.54 -99.00 -90.00   50
  3  ω    -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       'ω 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       â\/E?blockâ\/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/[σ²(Fo²)+(0.1191P)²+14.6383P] where P=(Fo²+2Fc²)/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 > 2σ(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'
_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 99.93
_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)
;
_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
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
Cd1 Cd 0.75172(7) 0.750000 0.39925(6) 0.0814(3) Uani 1 2 d S T P . .
I3 I 0.55978(7) 0.750000 0.38769(8) 0.1048(4) Uani 1 2 d S T P . .
I1 I 0.81728(9) 0.750000 0.54800(7) 0.1044(4) Uani 1 2 d S T P . .
I2 I 0.81821(7) 0.51708(13) 0.33401(8) 0.1630(4) Uani 1 1 d . . . . .
N2 N 0.8804(4) 0.250000 0.5812(4) 0.279(10) Uani 1 2 d DS T P . .
N1 N 0.4955(4) 0.250000 0.3552(3) 0.174(5) Uani 1 2 d DS T P . .
C3 C 0.5245(7) 0.250000 0.2728(3) 0.174(5) Uani 1 2 d DS T P . .
H3 H 0.464721 0.250000 0.245930 0.209 Uiso 1 2 calc R U P . .
C7 C 0.7773(3) 0.250000 0.5640(5) 0.279(10) Uani 1 2 d DS T P . .
H7 H 0.772562 0.249999 0.508386 0.334 Uiso 1 2 calc R U P . .
C1 C 0.4380(5) 0.1257(4) 0.3717(6) 0.174(5) Uani 1 1 d D . . . .
H1A H 0.385515 0.149554 0.402690 0.261 Uiso 1 1 calc R U . . .
H1B H 0.475690 0.061373 0.398263 0.261 Uiso 1 1 calc R U . . .
H1C H 0.416583 0.087555 0.324763 0.261 Uiso 1 1 calc DR U . . .
C6 C 0.9258(5) 0.3749(3) 0.5494(5) 0.279(10) Uani 1 1 d D . . . .
H6A H 0.881853 0.422276 0.518206 0.418 Uiso 1 1 calc R U . . .
H6B H 0.978824 0.350177 0.519314 0.418 Uiso 1 1 calc R U . . .
H6C H 0.945394 0.431601 0.590539 0.418 Uiso 1 1 calc R U . . .
C5 C 0.8953(7) 0.250000 0.6677(4) 0.279(10) Uani 1 2 d DS T P . .
H5A H 0.862799 0.325590 0.688599 0.418 Uiso 0.5 1 d R U P A -1
H5B H 0.960089 0.255640 0.680889 0.418 Uiso 0.5 1 d R U P A -1
H5C H 0.869559 0.168780 0.688069 0.418 Uiso 0.5 1 d R U P A -1
C4 C 0.5677(8) 0.3824(7) 0.2482(6) 0.172(7) Uani 1 1 d D . . . .
H4A H 0.538060 0.454707 0.274835 0.258 Uiso 1 1 calc R U . . .
H4B H 0.559314 0.393991 0.194422 0.258 Uiso 1 1 calc R U . . .
H4C H 0.633017 0.381862 0.259853 0.258 Uiso 1 1 calc R U . . .
C8 C 0.7285(9) 0.3773(9) 0.5900(12) 0.279(10) Uani 1 1 d D . . . .
H8A H 0.741101 0.392015 0.643034 0.418 Uiso 1 1 calc R U . . .
H8B H 0.662639 0.368105 0.582529 0.418 Uiso 1 1 calc R U . . .
H8C H 0.751084 0.452003 0.560998 0.418 Uiso 1 1 calc R U . . .
C2 C 0.5799(5) 0.250000 0.4065(5) 0.174(5) Uani 1 2 d DS T P . .
H2A H 0.561829 0.223150 0.456807 0.261 Uiso 0.5 1 d R U P B -1
H2B H 0.606089 0.338460 0.408207 0.261 Uiso 0.5 1 d R U P B -1
H2C H 0.625379 0.188390 0.387017 0.261 Uiso 0.5 1 d R U P B -1
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'
I I -0.4742 1.8119 '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'
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
I3 Cd1 I1 114.02(5) . . ?
I2 Cd1 I3 108.32(4) 7_575 . ?
I2 Cd1 I3 108.32(4) . . ?
I2 Cd1 I1 105.87(4) 7_575 . ?
I2 Cd1 I1 105.87(4) . . ?
I2 Cd1 I2 114.60(7) 7_575 . ?
C7 N2 C6 110.4(4) . 7_565 ?
C7 N2 C6 110.4(4) . . ?
C7 N2 C5 109.6(5) . . ?
C6 N2 C6 110.9(5) . 7_565 ?
C6 N2 C5 107.8(4) . . ?
C6 N2 C5 107.8(4) 7_565 . ?
C3 N1 C1 109.6(4) . 7_565 ?
C3 N1 C1 109.6(4) . . ?
C3 N1 C2 110.6(5) . . ?
C1 N1 C1 109.6(5) . 7_565 ?
C2 N1 C1 108.8(4) . . ?
C2 N1 C1 108.8(4) . 7_565 ?
N1 C3 H3 102.7 . . ?
N1 C3 C4 112.7(4) . 7_565 ?
N1 C3 C4 112.7(4) . . ?
C4 C3 H3 102.7 7_565 . ?
C4 C3 H3 102.7 . . ?
C4 C3 C4 120.4(9) . 7_565 ?
N2 C7 H7 105.5 . . ?
N2 C7 C8 113.0(7) . . ?
N2 C7 C8 113.0(7) . 7_565 ?
C8 C7 H7 105.5 . . ?
C8 C7 H7 105.5 7_565 . ?
C8 C7 C8 113.2(12) . 7_565 ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C5 H5A 108.1 . . ?
N2 C5 H5B 112.0 . . ?
N2 C5 H5C 108.3 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 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
Cd1 I3 2.7642(14) . ?
Cd1 I1 2.7787(16) . ?
Cd1 I2 2.7619(12) 7_575 ?
Cd1 I2 2.7619(12) . ?
N2 C7 1.511(6) . ?
N2 C6 1.514(4) . ?
N2 C6 1.514(4) 7_565 ?
N2 C5 1.536(7) . ?
N1 C3 1.506(5) . ?
N1 C1 1.518(4) . ?
N1 C1 1.518(4) 7_565 ?
N1 C2 1.511(6) . ?
C3 H3 0.9800 . ?
C3 C4 1.522(6) 7_565 ?
C3 C4 1.522(6) . ?
C7 H7 0.9800 . ?
C7 C8 1.521(6) 7_565 ?
C7 C8 1.521(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C5 H5A 0.9601 . ?
C5 H5B 0.9599 . ?
C5 H5C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C2 H2A 0.9598 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9601 . ?
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
C1 N1 C3 C4 170.0(7) . . . . ?
C1 N1 C3 C4 -49.7(9) . . . 7_565 ?
C1 N1 C3 C4 49.7(9) 7_565 . . . ?
C1 N1 C3 C4 -170.0(7) 7_565 . . 7_565 ?
C6 N2 C7 C8 176.3(10) . . . 7_565 ?
C6 N2 C7 C8 53.4(11) 7_565 . . 7_565 ?
C6 N2 C7 C8 -53.4(11) . . . . ?
C6 N2 C7 C8 -176.3(10) 7_565 . . . ?
C5 N2 C7 C8 65.1(9) . . . . ?
C5 N2 C7 C8 -65.1(9) . . . 7_565 ?
C2 N1 C3 C4 -70.2(7) . . . . ?
C2 N1 C3 C4 70.2(7) . . . 7_565 ?
