A five- and six-coordinated two-dimensional metal halide organic-inorganic phase transition material.
Chen, Hui-Ping; Wang, Zhen-Yu; Qi, Jun-Chao; Peng, Hang; Yang, Tian-En; Zhang, Xiao-Xuan; Luo, Xin-Yu; Liao, Wei-Qiang; Chemical communications (Cambridge, England) 61 (2025) 16636–16639; doi:10.1039/d5cc04326c

data_7135042
_publ_section_title
;
 A five- and six-coordinated two-dimensional metal halide
 organic-inorganic phase transition material.
;
_journal_issue                   85
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              16636
_journal_page_last               16639
_journal_paper_doi               10.1039/d5cc04326c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'Cd3 Cl7, C8 H20 N'
_chemical_formula_sum            'C8 H20 Cd3 Cl7 N'
_chemical_formula_weight         715.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-09-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-09-17 deposited with the CCDC.	2025-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                67.720(3)
_cell_angle_beta                 81.919(2)
_cell_angle_gamma                69.603(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8550(2)
_cell_length_b                   11.1928(3)
_cell_length_c                   13.5318(3)
_cell_measurement_reflns_used    8579
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      73.3920
_cell_measurement_theta_min      3.5110
_cell_volume                     1031.81(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.129a 64-bit (release 29-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_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      298.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10886
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         3.530
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    32.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.129a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.303
_exptl_crystal_description       needle
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.054
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3548
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0572
_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^)+(0.1272P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3076
_reflns_number_total             3548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04326c2.cif
_cod_data_source_block           1_298K
_cod_depositor_comments
'Adding full bibliography for 7135041--7135042.cif.'
_cod_database_code               7135042
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.077
_shelx_estimated_absorpt_t_min   0.035
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C3 = C4A-C3A = C5A-C3A = C5-C3
 1.54 with sigma of 0.01
 C4-C3 = C4A-C3A = C5-C3 = C5A-C3A
 1.54 with sigma of 0.01
 C7-C6 = C7A-C6A = C8A-C6A = C8-C6
 1.54 with sigma of 0.01
 C2A-C1A = C2-C1
 1.54 with sigma of 0.01
 C4-C3 = C4A-C3A
 1.54 with sigma of 0.01
 N1-C3 = N1-C3A
 1.48 with sigma of 0.01
 N1-C6A = N1-C6
 1.48 with sigma of 0.01
 N1-C1A = N1-C1
 1.48 with sigma of 0.01
 C2A-C1A \\sim C2-C1
 with sigma of 0.02
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 C5-C3 \\sim C5A-C3A
 with sigma of 0.02
 N1-C3A \\sim N1-C3
 with sigma of 0.02
 C7-C6 \\sim C7A-C6A
 with sigma of 0.02
 C8-C6 \\sim C8A-C6A
 with sigma of 0.02
 N1-C3 \\sim N1-C3A
 with sigma of 0.02
 N1-C6 \\sim N1-C6A
 with sigma of 0.02
 N1-C6A \\sim N1-C6
 with sigma of 0.02
 N1-C1A \\sim N1-C1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1A \\sim C2A \\sim C1 \\sim C2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C3A \\sim C4A \\sim C5A \\sim C4 \\sim C3 \\sim C5: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C6A \\sim C7A \\sim C8A \\sim C6 \\sim C8 \\sim C7: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Same fragment restrains
{C6, C7, C8} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C6A, C7A, C8A}
{C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C3A, C4A, C5A}
{C1, C2} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C1A, C2A}
5. Others
 Sof(C1A)=Sof(H1C)=Sof(H1D)=Sof(C2A)=Sof(H2D)=Sof(H2E)=Sof(H2F)=Sof(C3A)=
 Sof(H3A)=Sof(C4A)=Sof(H4D)=Sof(H4E)=Sof(H4F)=Sof(C5A)=Sof(H5D)=Sof(H5E)=
 Sof(H5F)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7D)=Sof(H7E)=Sof(H7F)=Sof(C8A)=
 Sof(H8D)=Sof(H8E)=Sof(H8F)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C6)=Sof(H6)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C3)=
 Sof(H3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=
 FVAR(1)
6.a Ternary CH refined with riding coordinates:
 N1(H1), C3A(H3A), C6A(H6A), C6(H6), C3(H3)
6.b Secondary CH2 refined with riding coordinates:
 C1A(H1C,H1D), C1(H1A,H1B)
6.c Idealised Me refined as rotating group:
 C2A(H2D,H2E,H2F), C4A(H4D,H4E,H4F), C5A(H5D,H5E,H5F), C7A(H7D,H7E,H7F),
 C8A(H8D,H8E,H8F), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C4(H4A,
 H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              2016
_olex2_submission_special_instructions 'No special instructions were received'